An evaluation of soil sampling for 137Cs using various field-sampling volumes.

PubMed

Nyhan, J W; White, G C; Schofield, T G; Trujillo, G

1983-05-01

The sediments from a liquid effluent receiving area at the Los Alamos National Laboratory and soils from an intensive study area in the fallout pathway of Trinity were sampled for 137Cs using 25-, 500-, 2500- and 12,500-cm3 field sampling volumes. A highly replicated sampling program was used to determine mean concentrations and inventories of 137Cs at each site, as well as estimates of spatial, aliquoting, and counting variance components of the radionuclide data. The sampling methods were also analyzed as a function of soil size fractions collected in each field sampling volume and of the total cost of the program for a given variation in the radionuclide survey results. Coefficients of variation (CV) of 137Cs inventory estimates ranged from 0.063 to 0.14 for Mortandad Canyon sediments, whereas CV values for Trinity soils were observed from 0.38 to 0.57. Spatial variance components of 137Cs concentration data were usually found to be larger than either the aliquoting or counting variance estimates and were inversely related to field sampling volume at the Trinity intensive site. Subsequent optimization studies of the sampling schemes demonstrated that each aliquot should be counted once, and that only 2-4 aliquots out of as many as 30 collected need be assayed for 137Cs. The optimization studies showed that as sample costs increased to 45 man-hours of labor per sample, the variance of the mean 137Cs concentration decreased dramatically, but decreased very little with additional labor.

Microvolume protein concentration determination using the NanoDrop 2000c spectrophotometer.

PubMed

Desjardins, Philippe; Hansen, Joel B; Allen, Michael

2009-11-04

Traditional spectrophotometry requires placing samples into cuvettes or capillaries. This is often impractical due to the limited sample volumes often used for protein analysis. The Thermo Scientific NanoDrop 2000c Spectrophotometer solves this issue with an innovative sample retention system that holds microvolume samples between two measurement surfaces using the surface tension properties of liquids, enabling the quantification of samples in volumes as low as 0.5-2 microL. The elimination of cuvettes or capillaries allows real time changes in path length, which reduces the measurement time while greatly increasing the dynamic range of protein concentrations that can be measured. The need for dilutions is also eliminated, and preparations for sample quantification are relatively easy as the measurement surfaces can be simply wiped with laboratory wipe. This video article presents modifications to traditional protein concentration determination methods for quantification of microvolume amounts of protein using A280 absorbance readings or the BCA colorimetric assay.

Determination of dissolved-phase pesticides in surface water from the Yakima River basin, Washington, using the Goulden large-sample extractor and gas chromatography/mass spectrometer

USGS Publications Warehouse

Foster, Gregory D.; Gates, Paul M.; Foreman, William T.; McKenzie, Stuart W.; Rinella, Frank A.

1993-01-01

Concentrations of pesticides in the dissolved phase of surface water samples from the Yakima River basin, WA, were determined using preconcentration in the Goulden large-sample extractor (GLSE) and gas chromatography/mass spectrometry (GC/MS) analysis. Sample volumes ranging from 10 to 120 L were processed with the GLSE, and the results from the large-sample analyses were compared to those derived from 1-L continuous liquid-liquid extractions Few of the 40 target pesticides were detected in 1-L samples, whereas large-sample preconcentration in the GLSE provided detectable levels for many of the target pesticides. The number of pesticides detected in GLSE processed samples was usually directly proportional to sample volume, although the measured concentrations of the pesticides were generally lower at the larger sample volumes for the same water source. The GLSE can be used to provide lower detection levels relative to conventional liquid-liquid extraction in GC/MS analysis of pesticides in samples of surface water.

[A thermodynamic study on bovine spermatozoa by microcalorimetry after Percoll density-gradient centrifugation - experimental probe of its utility in andrology].

PubMed

Fischer, C; Scherfer-Brähler, V; Müller-Schlösser, F; Schröder-Printzen, I; Weidner, W

2007-05-01

Microcalorimetric measurements can be used for recording exothermic or endothermic summation effects of a great variety of biological processes. The aim of the present study was to examine the usefullness of the microcalorimetry method to characterise the biological activity of spermatozoa. The heat flow of bovine fresh sperm as well as cryosperm samples were measured after Percoll density-gradient centrifugation in a 4-channel microcalorimeter. Various calibration times, volumes of samples and sperm concentrations were tested and analysed. Sperm concentration was recorded by a computer-assisted, computer-aided software system method (CASA). Using a calibration time of 15 minutes, the heat signal of the fresh and cryosperm samples showed a characteristic peak after 39.5 min and 38.1 min (mean), respectively, with a significant correlation to sample volume and sperm concentration (p < 0.05). For obtaining the best results, a sample volume of 1 ml and a sperm concentration of more than 50 x 10 (6)/mL was used. With microcalorimetric measurements the biological activity of spermatozoa could be recorded for reproducible results, thus opening the way to an automatised ejaculate analysis in the future. More investigations are necessary to correlate microcalorimetric parameters with semen function.

A novel approach to the measurement of surfactant parameters in arthropod digestive juices.

PubMed

Romih, Tea; Kogej, Ksenija; Drobne, Damjana

2016-05-01

In arthropods, the determination of two important parameters of digestive juices, i.e. the total surfactant concentration and the critical micelle concentration (CMC), is challenging due to small sample volumes and low surfactant concentrations. In this work, we report a successful implementation of potentiometric titrations using the surfactant ion-selective electrode (SISE) and the pyrene fluorescence method (PFM) for the determination of the total surfactant concentration and CMC in the digestive juice of terrestrial isopod crustaceans Porcellio scaber. Pooled digestive juice extracts of four (SISE) or two (PFM) animals were used per measurement run. In both cases, digestive juice extracts in 100 μL of deionized water were sufficient for one measurement run. The total surfactant concentration of P. scaber digestive juice was determined to be 9.2 ± 3.5mM and the CMC was approximately 90 μM. Our work presents an important improvement towards easy CMC determination in small volume samples in comparison with the commonly used stalagmometric technique, where much larger sample volumes are usually needed. To date, the total surfactant concentration was not measured in the digestive juices of arthropods other than Homarus vulgaris, Astacus leptodactylus and Cancer pagurus, for which complex separation and analytical techniques were required. Our results obtained by SISE and PFM therefore present the first successful quantification of surfactants and their CMC in small volumes of arthropod digestive juice without prior separation or purification techniques. Copyright © 2016 Elsevier Ltd. All rights reserved.

“Nanofiltration” Enabled by Super-Absorbent Polymer Beads for Concentrating Microorganisms in Water Samples

NASA Astrophysics Data System (ADS)

Xie, Xing; Bahnemann, Janina; Wang, Siwen; Yang, Yang; Hoffmann, Michael R.

2016-02-01

Detection and quantification of pathogens in water is critical for the protection of human health and for drinking water safety and security. When the pathogen concentrations are low, large sample volumes (several liters) are needed to achieve reliable quantitative results. However, most microbial identification methods utilize relatively small sample volumes. As a consequence, a concentration step is often required to detect pathogens in natural waters. Herein, we introduce a novel water sample concentration method based on superabsorbent polymer (SAP) beads. When SAP beads swell with water, small molecules can be sorbed within the beads, but larger particles are excluded and, thus, concentrated in the residual non-sorbed water. To illustrate this approach, millimeter-sized poly(acrylamide-co-itaconic acid) (P(AM-co-IA)) beads are synthesized and successfully applied to concentrate water samples containing two model microorganisms: Escherichia coli and bacteriophage MS2. Experimental results indicate that the size of the water channel within water swollen P(AM-co-IA) hydrogel beads is on the order of several nanometers. The millimeter size coupled with a negative surface charge of the beads are shown to be critical in order to achieve high levels of concentration. This new concentration procedure is very fast, effective, scalable, and low-cost with no need for complex instrumentation.

"Nanofiltration" Enabled by Super-Absorbent Polymer Beads for Concentrating Microorganisms in Water Samples.

PubMed

Xie, Xing; Bahnemann, Janina; Wang, Siwen; Yang, Yang; Hoffmann, Michael R

2016-02-15

Detection and quantification of pathogens in water is critical for the protection of human health and for drinking water safety and security. When the pathogen concentrations are low, large sample volumes (several liters) are needed to achieve reliable quantitative results. However, most microbial identification methods utilize relatively small sample volumes. As a consequence, a concentration step is often required to detect pathogens in natural waters. Herein, we introduce a novel water sample concentration method based on superabsorbent polymer (SAP) beads. When SAP beads swell with water, small molecules can be sorbed within the beads, but larger particles are excluded and, thus, concentrated in the residual non-sorbed water. To illustrate this approach, millimeter-sized poly(acrylamide-co-itaconic acid) (P(AM-co-IA)) beads are synthesized and successfully applied to concentrate water samples containing two model microorganisms: Escherichia coli and bacteriophage MS2. Experimental results indicate that the size of the water channel within water swollen P(AM-co-IA) hydrogel beads is on the order of several nanometers. The millimeter size coupled with a negative surface charge of the beads are shown to be critical in order to achieve high levels of concentration. This new concentration procedure is very fast, effective, scalable, and low-cost with no need for complex instrumentation.

“Nanofiltration” Enabled by Super-Absorbent Polymer Beads for Concentrating Microorganisms in Water Samples

PubMed Central

Xie, Xing; Bahnemann, Janina; Wang, Siwen; Yang, Yang; Hoffmann, Michael R.

2016-01-01

Detection and quantification of pathogens in water is critical for the protection of human health and for drinking water safety and security. When the pathogen concentrations are low, large sample volumes (several liters) are needed to achieve reliable quantitative results. However, most microbial identification methods utilize relatively small sample volumes. As a consequence, a concentration step is often required to detect pathogens in natural waters. Herein, we introduce a novel water sample concentration method based on superabsorbent polymer (SAP) beads. When SAP beads swell with water, small molecules can be sorbed within the beads, but larger particles are excluded and, thus, concentrated in the residual non-sorbed water. To illustrate this approach, millimeter-sized poly(acrylamide-co-itaconic acid) (P(AM-co-IA)) beads are synthesized and successfully applied to concentrate water samples containing two model microorganisms: Escherichia coli and bacteriophage MS2. Experimental results indicate that the size of the water channel within water swollen P(AM-co-IA) hydrogel beads is on the order of several nanometers. The millimeter size coupled with a negative surface charge of the beads are shown to be critical in order to achieve high levels of concentration. This new concentration procedure is very fast, effective, scalable, and low-cost with no need for complex instrumentation. PMID:26876979

Rapid method for measuring rotenone in water at piscicidal concentrations

USGS Publications Warehouse

Dawson, V.K.; Harman, P.D.; Schultz, D.P.; Allen, J.L.

1983-01-01

A high-performance liquid chromatography (HPLC) procedure that is rapid, specific, and sensitive (limit of detection <0.005 mg/liter) was developed for monitoring application and degradation rates of rotenone. For analysis, a water sample is buffered to pH 5 and injected through a Sep Pak(R) C18 disposable cartridge. The cartridge adsorbs and retains the rotenone which then can be eluted quantitatively from the cartridge with a small volume of methanol. This step effectively concentrates the sample and provides sample cleanup. The methanol extract is analyzed directly by HPLC on an MCH 10 reverse-phase column; methanol: water (75:25, volume : volume) is the mobile phase and flow rate is 1.5 ml/minute. The rotenone is detected by ultraviolet spectrophotometry at a wavelength of 295 nm.

TO PURGE OR NOT TO PURGE? VOC CONCENTRATION CHANGES DURING LINE VOLUME PURGING

EPA Science Inventory

Soil vapor surveys are commonly used as a screening technique to delineate volatile organic compound (VOC) contaminant plumes and provide information for soil sampling plans. Traditionally, three purge volumes of vapor are removed before a sample is collected. One facet of this s...

Microplastic analysis in the South Funen Archipelago, Baltic Sea, implementing manta trawling and bulk sampling.

PubMed

Tamminga, Matthias; Hengstmann, Elena; Fischer, Elke Kerstin

2018-03-01

Microplastic contamination in surface waters of the South Funen Archipelago in Denmark was assessed. Therefore, ten manta trawls were conducted in June 2015. Moreover, 31 low-volume bulk samples were taken to evaluate, whether consistent results in comparison to the net-based approach can be obtained. Microplastic contamination in the South Funen Archipelago (0.07 ± 0.02 particles/m3) is slightly below values reported before. The sheltered position of the study area, low population pressure on adjacent islands and the absence of any major potential point sources were identified as major factors explaining the low concentration of microplastics. Within the Archipelago, harbors or marinas and the associated vessel traffic are the most probable sources of microplastics. The concentration of microplastics in low-volume bulk samples is not comparable to manta trawl results. This is mainly due to insufficient representativeness of the bulk sample volumes.

Tree Sampling as a Method to Assess Vapor Intrusion Potential at a Site Characterized by VOC-Contaminated Groundwater and Soil.

PubMed

Wilson, Jordan L; Limmer, Matthew A; Samaranayake, V A; Schumacher, John G; Burken, Joel G

2017-09-19

Vapor intrusion (VI) by volatile organic compounds (VOCs) in the built environment presents a threat to human health. Traditional VI assessments are often time-, cost-, and labor-intensive; whereas traditional subsurface methods sample a relatively small volume in the subsurface and are difficult to collect within and near structures. Trees could provide a similar subsurface sample where roots act as the "sampler' and are already onsite. Regression models were developed to assess the relation between PCE concentrations in over 500 tree-core samples with PCE concentrations in over 50 groundwater and 1000 soil samples collected from a tetrachloroethylene- (PCE-) contaminated Superfund site and analyzed using gas chromatography. Results indicate that in planta concentrations are significantly and positively related to PCE concentrations in groundwater samples collected at depths less than 20 m (adjusted R 2 values greater than 0.80) and in soil samples (adjusted R 2 values greater than 0.90). Results indicate that a 30 cm diameter tree characterizes soil concentrations at depths less than 6 m over an area of 700-1600 m 2 , the volume of a typical basement. These findings indicate that tree sampling may be an appropriate method to detect contamination at shallow depths at sites with VI.

Analytical evaluation of BEA zeolite for the pre-concentration of polycyclic aromatic hydrocarbons and their subsequent chromatographic analysis in water samples.

PubMed

Wilson, Walter B; Costa, Andréia A; Wang, Huiyong; Dias, José A; Dias, Sílvia C L; Campiglia, Andres D

2012-07-06

The analytical performance of BEA - a commercial zeolite - is evaluated for the pre-concentration of fifteen Environmental Protection Agency - polycyclic aromatic hydrocarbons and their subsequent HPLC analysis in tap and lake water samples. The pre-concentration factors obtained with BEA have led to a method with excellent analytical figures of merit. One milliliter aliquots were sufficient to obtain excellent precision of measurements at the parts-per-trillion concentration level with relative standard deviations varying from 4.1% (dibenzo[a,h]anthracene) to 13.4% (pyrene). The limits of detection were excellent as well and varied between 1.1 (anthracene) and 49.9 ng L(-1) (indeno[1,2,3-cd]pyrene). The recovery values of all the studied compounds meet the criterion for regulated polycyclic aromatic hydrocarbons, which mandates relative standard deviations equal or lower than 25%. The small volume of organic solvents (100 μL per sample) and amount of BEA (2 mg per sample) makes sample pre-concentration environmentally friendly and cost effective. The extraction procedure is well suited for numerous samples as the small working volume (1 mL) facilitates the implementation of simultaneous sample extraction. These are attractive features when routine monitoring of numerous samples is contemplated. Copyright © 2012 Elsevier B.V. All rights reserved.

Tree sampling as a method to assess vapor intrusion potential at a site characterized by VOC-contaminated groundwater and soil

USGS Publications Warehouse

Wilson, Jordan L.; Limmer, Matthew A.; Samaranayake, V. A.; Schumacher, John G.; Burken, Joel G.

2017-01-01

Vapor intrusion (VI) by volatile organic compounds (VOCs) in the built environment presents a threat to human health. Traditional VI assessments are often time-, cost-, and labor-intensive; whereas traditional subsurface methods sample a relatively small volume in the subsurface and are difficult to collect within and near structures. Trees could provide a similar subsurface sample where roots act as the “sampler’ and are already onsite. Regression models were developed to assess the relation between PCE concentrations in over 500 tree-core samples with PCE concentrations in over 50 groundwater and 1000 soil samples collected from a tetrachloroethylene- (PCE-) contaminated Superfund site and analyzed using gas chromatography. Results indicate that in planta concentrations are significantly and positively related to PCE concentrations in groundwater samples collected at depths less than 20 m (adjusted R2 values greater than 0.80) and in soil samples (adjusted R2 values greater than 0.90). Results indicate that a 30 cm diameter tree characterizes soil concentrations at depths less than 6 m over an area of 700–1600 m2, the volume of a typical basement. These findings indicate that tree sampling may be an appropriate method to detect contamination at shallow depths at sites with VI.

Atmospheric CO2 Records from Sites in the Main Geophysical Observatory Air Sampling Network (1983 - 1993)

DOE Data Explorer

Brounshtein, A. M. [Main Geophysical Observatory, St. Petersburg, Russia; Shaskov, A. A. [Main Geophysical Observatory, St. Petersburg, Russia; Paramonova, N. N. [Main Geophysical Observatory, St. Petersburg, Russia; Privalov, V. I. [Main Geophysical Observatory, St. Petersburg, Russia; Starodubtsev, Y. A. [Main Geophysical Observatory, St. Petersburg, Russia

1997-01-01

Air samples were collected from five sites in the Main Geophysical Observatory air sampling network to monitor the atmospheric CO2 from 1983 - 1993. Airwas collected generally four times per month in pairs of 1.5-L stainless steel electropolished flasks with one greaseless stainless steel stopcock. Sampling was performed by opening the stopcock of the flasks, which have been evacuated at the central laboratory at the Main Geophysical Observatory (MGO). The air was not dried during sample collection. Attempts were made to obtain samples when the wind speed was >5 m/s and the wind direction corresponded to the predetermined "clean air" sector. The period of record at Bering Island is too short to identify any long-term trends in atmospheric CO2 concentrations; however, the yearly mean atmospheric CO2 concentration at Bering Island rose from approximately 346 parts per million by volume (ppmv) in 1986 to 362.6 ppmv in 1993. Measurements from this station are considered indicative of maritime air masses. The period of record at Kotelny Island is too short to identify any long-term trends in atmospheric CO2 concentrations; however, the yearly mean atmospheric CO2 concentration at Kotelny Island rose from 356.08 parts per million by volume (ppmv) in 1988 to 358.8 ppmv in 1993. Because Kotelny Island is the northernmost Russian sampling site, measurements from this site serve as a useful comparison to other northern sites (e.g., Alert, Northwest Territories). In late 1989, air sampling began at the Russian site of Kyzylcha, located in the Republic of Uzbekistan. Unfortunately, the desert site at Kyzylcha has been out of operation since mid-1991 due to financial difficulties in Russia. The annual mean value of 359.02 parts per million by volume (ppmv) for 1990, the lone full year of operation, is higher than measurements from other monitoring programs at this latitude [e.g., Niwot Ridge (354.7 ppmv in 1990) and Tae-ahn Peninsula]. Station "C," an open ocean site, in the North Atlantic, east of Greenland, was established in 1968 and was operated in cooperation with NOAA's National Weather Service through 1973. The Main Geophysical Observatory collected flask samples at the site from January 1983 through October 1990. The yearly mean atmospheric CO concentration at Station "C" rose from 348.15 parts per million by volume (ppmv) in 1985 to 354.33 ppmv in 1989. The period of record at Teriberka Station is too short to identify any long-term trends in atmospheric CO2 concentrations; however, the yearly mean atmospheric CO2 concentration at Teriberka Station rose from 354.8 parts per million by volume (ppmv) in 1989 to 358.7 ppmv in 1993.

Pushing quantitation limits in micro UHPLC-MS/MS analysis of steroid hormones by sample dilution using high volume injection.

PubMed

Márta, Zoltán; Bobály, Balázs; Fekete, Jenő; Magda, Balázs; Imre, Tímea; Mészáros, Katalin Viola; Szabó, Pál Tamás

2016-09-10

Ultratrace analysis of sample components requires excellent analytical performance in terms of limits of quantitation (LoQ). Micro UHPLC coupling with sensitive tandem mass spectrometry provides state of the art solutions for such analytical problems. Decreased column volume in micro LC limits the injectable sample volume. However, if analyte concentration is extremely low, it might be necessary to inject high sample volumes. This is particularly critical for strong sample solvents and weakly retained analytes, which are often the case when preparing biological samples (protein precipitation, sample extraction, etc.). In that case, high injection volumes may cause band broadening, peak distortion or even elution in dead volume. In this study, we evaluated possibilities of high volume injection onto microbore RP-LC columns, when sample solvent is diluted. The presented micro RP-LC-MS/MS method was optimized for the analysis of steroid hormones from human plasma after protein precipitation with organic solvents. A proper sample dilution procedure helps to increase the injection volume without compromising peak shapes. Finally, due to increased injection volume, the limit of quantitation can be decreased by a factor of 2-5, depending on the analytes and the experimental conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

Quantifying viruses and bacteria in wastewater—Results, interpretation methods, and quality control

USGS Publications Warehouse

Francy, Donna S.; Stelzer, Erin A.; Bushon, Rebecca N.; Brady, Amie M.G.; Mailot, Brian E.; Spencer, Susan K.; Borchardt, Mark A.; Elber, Ashley G.; Riddell, Kimberly R.; Gellner, Terry M.

2011-01-01

Membrane bioreactors (MBR), used for wastewater treatment in Ohio and elsewhere in the United States, have pore sizes small enough to theoretically reduce concentrations of protozoa and bacteria, but not viruses. Sampling for viruses in wastewater is seldom done and not required. Instead, the bacterial indicators Escherichia coli (E. coli) and fecal coliforms are the required microbial measures of effluents for wastewater-discharge permits. Information is needed on the effectiveness of MBRs in removing human enteric viruses from wastewaters, particularly as compared to conventional wastewater treatment before and after disinfection. A total of 73 regular and 28 quality-control (QC) samples were collected at three MBR and two conventional wastewater plants in Ohio during 23 regular and 3 QC sampling trips in 2008-10. Samples were collected at various stages in the treatment processes and analyzed for bacterial indicators E. coli, fecal coliforms, and enterococci by membrane filtration; somatic and F-specific coliphage by the single agar layer (SAL) method; adenovirus, enterovirus, norovirus GI and GII, rotavirus, and hepatitis A virus by molecular methods; and viruses by cell culture. While addressing the main objective of the study-comparing removal of viruses and bacterial indicators in MBR and conventional plants-it was realized that work was needed to identify data analysis and quantification methods for interpreting enteric virus and QC data. Therefore, methods for quantifying viruses, qualifying results, and applying QC data to interpretations are described in this report. During each regular sampling trip, samples were collected (1) before conventional or MBR treatment (post-preliminary), (2) after secondary or MBR treatment (post-secondary or post-MBR), (3) after tertiary treatment (one conventional plant only), and (4) after disinfection (post-disinfection). Glass-wool fiber filtration was used to concentrate enteric viruses from large volumes, and small volume grab samples were collected for direct-plating analyses for bacterial indicators and coliphage. After filtration, the viruses were eluted from the filter and further concentrated. The final concentrated sample volume (FCSV) was used for enteric virus analysis by use of two methods-cell culture and a molecular method, polymerase chain reaction (PCR). Quantitative PCR (qPCR) for DNA viruses and quantitative reverse-transcriptase PCR (qRT-PCR) for RNA viruses were used in this study. To support data interpretations, the assay limit of detection (ALOD) was set for each virus assay and used to determine sample reporting limits (SRLs). For qPCR and qRT-PCR the ALOD was an estimated value because it was not established according to established method detection limit procedures. The SRLs were different for each sample because effective sample volumes (the volume of the original sample that was actually used in each analysis) were different for each sample. Effective sample volumes were much less than the original sample volumes because of reductions from processing steps and (or) from when dilutions were made to minimize the effects from PCR-inhibiting substances. Codes were used to further qualify the virus data and indicate the level of uncertainty associated with each measurement. Quality-control samples were used to support data interpretations. Field and laboratory blanks for bacteria, coliphage, and enteric viruses were all below detection, indicating that it was unlikely that samples were contaminated from equipment or processing procedures. The absolute value log differences (AVLDs) between concurrent replicate pairs were calculated to identify the variability associated with each measurement. For bacterial indicators and coliphage, the AVLD results indicated that concentrations <10 colony-forming units or plaque-forming units per 100 mL can differ between replicates by as much as 1 log, whereas higher concentrations can differ by as much as 0.3 log. The AVLD results for viruses indicated that differences between replicates can be as great as 1.2 log genomic copies per liter, regardless of the concentration of virus. Relatively large differences in molecular results for viruses between replicate pairs were likely due to lack of precision for samples with small effective volumes. Concentrations of E. coli, fecal coliforms, enterococci, and somatic and F-specific coliphage in post-secondary and post-tertiary samples in conventional plants were higher than those in post-MBR samples. In post-MBR and post-secondary samples, concentrations of somatic coliphage were higher than F-specific coliphage. In post-disinfection samples from two MBR plants (the third MBR plant had operational issues) and the ultraviolet conventional plant, concentrations for all bacterial indicators and coliphage were near or below detection; from the chlorine conventional plant, concentrations in post-disinfection samples were in the single or double digits. All of the plants met the National Pollutant Discharge Elimination System required effluent limits established for fecal coliforms. Norovirus GII and hepatitis A virus were not detected in any samples, and rotavirus was detected in one sample but could not be quantified. Adenovirus was found in 100 percent, enterovirus in over one-half, and norovirus GI in about one-half of post-preliminary wastewater samples. Adenovirus and enterovirus were detected throughout the treatment processes, and norovirus GI was detected less often than the other two enteric viruses. Culturable viruses were detected in post-preliminary samples and in only two post-treatment samples from the plant with operational issues.

Implementing DBS methodology for the determination of Compound A in monkey blood: GLP method validation and investigation of the impact of blood spreading on performance.

PubMed

Fan, Leimin; Lee, Jacob; Hall, Jeffrey; Tolentino, Edward J; Wu, Huaiqin; El-Shourbagy, Tawakol

2011-06-01

This article describes validation work for analysis of an Abbott investigational drug (Compound A) in monkey whole blood with dried blood spots (DBS). The impact of DBS spotting volume on analyte concentration was investigated. The quantitation range was between 30.5 and 10,200 ng/ml. Accuracy and precision of quality controls, linearity of calibration curves, matrix effect, selectivity, dilution, recovery and multiple stabilities were evaluated in the validation, and all demonstrated acceptable results. Incurred sample reanalysis was performed with 57 out of 58 samples having a percentage difference (versus the mean value) less than 20%. A linear relationship between the spotting volume and the spot area was drawn. The influence of spotting volume on concentration was discussed. All validation results met good laboratory practice acceptance requirements. Radial spreading of blood on DBS cards can be a factor in DBS concentrations at smaller spotting volumes.

Microvolume Protein Concentration Determination using the NanoDrop 2000c Spectrophotometer

PubMed Central

Desjardins, Philippe; Hansen, Joel B.; Allen, Michael

2009-01-01

Traditional spectrophotometry requires placing samples into cuvettes or capillaries. This is often impractical due to the limited sample volumes often used for protein analysis. The Thermo Scientific NanoDrop 2000c Spectrophotometer solves this issue with an innovative sample retention system that holds microvolume samples between two measurement surfaces using the surface tension properties of liquids, enabling the quantification of samples in volumes as low as 0.5-2 μL. The elimination of cuvettes or capillaries allows real time changes in path length, which reduces the measurement time while greatly increasing the dynamic range of protein concentrations that can be measured. The need for dilutions is also eliminated, and preparations for sample quantification are relatively easy as the measurement surfaces can be simply wiped with laboratory wipe. This video article presents modifications to traditional protein concentration determination methods for quantification of microvolume amounts of protein using A280 absorbance readings or the BCA colorimetric assay. PMID:19890248

Electrical Transport Ability of Nanostructured Potassium-Doped Titanium Oxide Film

NASA Astrophysics Data System (ADS)

Lee, So-Yoon; Matsuno, Ryosuke; Ishihara, Kazuhiko; Takai, Madoka

2011-02-01

Potassium-doped nanostructured titanium oxide films were fabricated using a wet corrosion process with various KOH solutions. The doped condition of potassium in TiO2 was confirmed by Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). Nanotubular were synthesized at a dopant concentration of <0.27% when the dopant concentration increased to >0.27%, these structures disappeared. To investigate the electrical properties of K-doped TiO2, pseudo metal-oxide-semiconductor field-effect transistor (MOSFET) samples were fabricated. The samples exhibited a distinct electrical behavior and p-type characteristics. The electrical behavior was governed by the volume of the dopant when the dopant concentration was <0.10% and the volume of the TiO2 phase when the dopant concentration was >0.18%.

Concentration and separation of biological organisms by ultrafiltration and dielectrophoresis

DOEpatents

Simmons, Blake A.; Hill, Vincent R.; Fintschenko, Yolanda; Cummings, Eric B.

2010-10-12

Disclosed is a method for monitoring sources of public water supply for a variety of pathogens by using a combination of ultrafiltration techniques together dielectrophoretic separation techniques. Because water-borne pathogens, whether present due to "natural" contamination or intentional introduction, would likely be present in drinking water at low concentrations when samples are collected for monitoring or outbreak investigations, an approach is needed to quickly and efficiently concentrate and separate particles such as viruses, bacteria, and parasites in large volumes of water (e.g., 100 L or more) while simultaneously reducing the sample volume to levels sufficient for detecting low concentrations of microbes (e.g., <10 mL). The technique is also designed to screen the separated microbes based on specific conductivity and size.

Model-based flow rate control for an orfice-type low-volume air sampler

USDA-ARS?s Scientific Manuscript database

The standard method of measuring air suspended particulate matter concentration per volume of air consists of continuously drawing a defined volume of air across a filter over an extended period of time, then measuring the mass of the filtered particles and dividing it by the total volume sampled ov...

40 CFR 60.446 - Test methods and procedures.

Code of Federal Regulations, 2010 CFR

2010-07-01

... the web substrate. (b) Method 25 shall be used to determine the VOC concentration, in parts per... equivalent, and each effluent gas stream emitted directly to the atmosphere. Methods 1, 2, 3, and 4 shall be... minimum sampling volume must be 0.003 dscm except that shorter sampling times or smaller volumes, when...

40 CFR 60.446 - Test methods and procedures.

Code of Federal Regulations, 2011 CFR

2011-07-01

... the web substrate. (b) Method 25 shall be used to determine the VOC concentration, in parts per... equivalent, and each effluent gas stream emitted directly to the atmosphere. Methods 1, 2, 3, and 4 shall be... minimum sampling volume must be 0.003 dscm except that shorter sampling times or smaller volumes, when...

Presence of pathogenic microorganisms in power-plant cooling waters. Final report, October 1, 1981-June 30, 1983

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tyndall, R.L.

1983-07-01

Air was sampled at the point of discharge and at short distances downwind and upwind from industrial and power-plant cooling towers. Both high-volume electrostatic and impinger type samplers were used. Concentrates of the air samples were analyzed for Legionnaires' Disease Bacteria (LDB). In some cases, the samples were also tested for the presence of free-living amoebae. The concentrations of LDB in the air samples were well below the minimal infectious dose for guinea pigs and precluded testing of the samples for infectious LDB. Results of LDB analysis were related to the meteorological conditions at the time of sampling. Generally, themore » concentrations of LDB in the air at the discharge of the cooling towers were 1 x 10/sup -6/ to 1 x 10/sup -7/ of that found in comparable volumes of tower basin water. During periods of high humidity and wind speed, LDB was detected in a few downwind samples and one upwind sample. One site with extensive construction and excavation activity had higher LDB concentrations in air samples relative to other sites. Nonpathogenic Naegleria were present in one of two air samples taken in the mist at the base of a natural-draft cooling tower.« less

Concentration and purification of HIV-1 virions by microfluidic separation of superparamagnetic nanoparticles

PubMed Central

Chen, Grace Dongqing; Alberts, Catharina Johanna

2009-01-01

The low concentration and complex sample matrix of many clinical and environmental viral samples presents a significant challenge in the development of low cost, point-of-care viral assays. To address this problem, we investigated the use of a microfluidic passive magnetic separator combined with on-chip mixer to both purify and concentrate whole particle HIV-1 virions. Virus-containing plasma samples are first mixed to allow specific binding of the viral particles with antibody-conjugated superparamagnetic nanoparticles, and several passive mixer geometries were assessed for their mixing efficiencies. The virus-nanoparticle complexes are then separated from the plasma in a novel magnetic separation chamber, where packed micron-sized ferromagnetic particles serve as high magnetic gradient concentrators for an externally applied magnetic field. Thereafter, a viral lysis buffer was flowed through the chip and the released HIV proteins were assayed off-chip. Viral protein extraction efficiencies of 62% and 45% were achieved at 10uL/min and 30uL/min throughputs respectively. More importantly, an 80-fold concentration was observed for an initial sample volume of 1mL, and a 44-fold concentration for an initial sample volume of 0.5mL. The system is broadly applicable to microscale sample preparation of any viral sample and can be used for nucleic acid extraction as well as 40–80 fold enrichment of target viruses. PMID:19954210

National Estimate of Per- and Polyfluoroalkyl Substance (PFAS) Release to U.S. Municipal Landfill Leachate.

PubMed

Lang, Johnsie R; Allred, B McKay; Field, Jennifer A; Levis, James W; Barlaz, Morton A

2017-02-21

Landfills are the final stage in the life cycle of many products containing per- and polyfluoroalkyl substances (PFASs) and their presence has been reported in landfill leachate. The concentrations of 70 PFASs in 95 samples of leachate were measured in a survey of U.S. landfills of varying climates and waste ages. National release of PFASs was estimated by coupling measured concentrations for the 19 PFASs where more than 50% of samples had quantifiable concentrations, with climate-specific estimates of annual leachate volumes. For 2013, the total volume of leachate generated in the U.S. was estimated to be 61.1 million m 3 , with 79% of this volume coming from landfills in wet climates (>75 cm/yr precipitation) that contain 47% of U.S. solid waste. The mass of measured PFASs from U.S. landfill leachate to wastewater treatment plants was estimated to be between 563 and 638 kg for 2013. In the majority of landfill leachate samples, 5:3 fluorotelomer carboxylic acid (FTCA) was dominant and variations in concentrations with waste age affected total estimated mass. There were six PFASs that demonstrated significantly higher concentrations in leachate from younger waste compared to older waste and six PFAS demonstrated significant variation with climate.

Variation in Nectar Volume and Sugar Concentration of Allium ursinum L. ssp. ucrainicum in Three Habitats

PubMed Central

Farkas, Ágnes; Molnár, Réka; Morschhauser, Tamás; Hahn, István

2012-01-01

Floral nectar volume and concentration of ramson (Allium ursinum L. ssp. ucrainicum) were investigated in three different habitats, including two types of sessile oak-hornbeam association on brown forest soil with clay illuviation and a silver lime-flowering ash rock forest association on rendzina. Daily nectar production ranged from 0.1 to 3.8 μL per flower with sugar concentrations of 25 to 50%. Mean nectar volumes and concentrations showed significant differences between freely exposed flowers and covered flowers, which had been isolated from flower visitors 24 h prior to nectar studies. Both the amount and quality of nectar were affected by microclimatic conditions and soil properties and varied between populations at different habitats. In the silver lime-flowering ash rock-forest association mean nectar volumes and concentrations were lower than in a typical sessile oak-hornbeam association on three occasions, the difference being significant in two cases. During full bloom, the date of sampling did not have a profound effect on either nectar volume or concentration. PMID:22619588

Delineation of discharge areas of two contaminant plumes by use of diffusion samplers, Johns Pond, Cape Cod, Massachusetts, 1998

USGS Publications Warehouse

Savoie, Jennifer G.; LeBlanc, D.R.; Blackwood, D.S.; McCobb, T.D.; Rendigs, R. R.; Clifford, Scott

2000-01-01

Diffusion samplers were installed in the bottom of Johns Pond, Cape Cod, Massachusetts, to confirm that volatile organic compounds from the Storm Drain-5 (SD-5) plume emanating from the Massachusetts Military Reservation (MMR) were discharging into the pond. An array of 134 vapor-diffusion samplers was buried by divers about 0.5 feet below the pond bottom in the presumed discharge area of the SD-5 plume and left in place for about 2 weeks to equilibrate. Two areas of high concentrations of volatile organic compounds (VOCs) were identified. Samples from the first area contained trichloroethene (TCE) and tetrachloroethene with concentrations in vapor as high as 890 and 667 parts per billion by volume, respectively. This discharge area is about 1,000 feet wide, extends from 100 to 350 feet offshore, and is interpreted to be the discharge area of the SD-5 plume. Samples from the second area were located closer to shore than the discharge area of the SD-5 plume and contained unexpectedly high vapor concentrations of TCE (more than 40,000 parts per billion by volume). Ground-water samples collected with a drive-point sampler near the second area had aqueous TCE concentrations as high as 1,100 micrograms per liter. Subsequently, a more closely spaced array of 110 vapor-diffusion samplers was installed to map the area of elevated TCE concentrations . The discharge area detected with the samplers is about 75 feet wide and extends from about 25 to 200 feet offshore . TCE vapor concentrations in this area were as high as 42,800 parts per billion by volume. TCE concentrations in micrograms per liter in water-diffusion samples from 15 selected sites in the two discharge areas were about 35 times lower than the TCE concentrations in parts per billion by volume in corresponding vapor-diffusion samples. The difference in values is due to the volatile nature of TCE and the different units of measure. TCE was detected in diffusion samplers set in the pond water column above the plume discharge areas, but the TCE concentrations were 20 to 30 times lower than the corresponding levels in diffusion samplers buried in the pond bottom.

Method for concentration and separation of biological organisms by ultrafiltration and dielectrophoresis

DOEpatents

Simmons, Blake A.; Hill, Vincent R.; Fintschenko, Yolanda; Cummings, Eric B.

2012-09-04

Disclosed is a method for monitoring sources of public water supply for a variety of pathogens by using a combination of ultrafiltration techniques together dielectrophoretic separation techniques. Because water-borne pathogens, whether present due to "natural" contamination or intentional introduction, would likely be present in drinking water at low concentrations when samples are collected for monitoring or outbreak investigations, an approach is needed to quickly and efficiently concentrate and separate particles such as viruses, bacteria, and parasites in large volumes of water (e.g., 100 L or more) while simultaneously reducing the sample volume to levels sufficient for detecting low concentrations of microbes (e.g., <10 mL). The technique is also designed to screen the separated microbes based on specific conductivity and size.

Impact of phase ratio, polydimethylsiloxane volume and size, and sampling temperature and time on headspace sorptive extraction recovery of some volatile compounds in the essential oil field.

PubMed

Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Rubiolo, Patrizia; Sgorbini, Barbara; Sandra, Pat

2005-04-15

This study evaluates concentration capability of headspace sorptive extraction (HSSE) and the influence of sampling conditions on HSSE recovery of an analyte. A standard mixture in water of six high-to-medium volatility analytes (isobutyl methyl ketone, 3-hexanol, isoamyl acetate, 1,8-cineole, linalool and carvone) was used to sample the headspace by HSSE with stir bars coated with different polydimethylsiloxane (PDMS) volumes (20, 40, 55 and 110 microL, respectively), headspace vial volumes (8, 21.2, 40, 250 and 1000 mL), sampling temperatures (25, 50 and 75 degrees C) and sampling times (30, 60 and 120 min, and 4, 8 and 16 h). The concentration factors (CFs) of HSSE versus static headspace (S-HS) were also determined. Analytes sampled by the PDMS stir bars were recovered by thermal desorption (TDS) and analysed by capillary GC-MS. This study demonstrates how analyte recovery depends on its physico-chemical characteristics and affinity for PDMS (octanol-water partition coefficients), sampling temperatures (50 degrees C) and times (60 min), the volumes of headspace (40 mL) and of PDMS (in particular, for high volatility analytes). HSSE is also shown to be very effective for trace analysis. The HSSE CFs calculated versus S-HS with a 1000 mL headspace volumes at 25 degrees C during 4 h sampling ranged between 10(3) and 10(4) times for all analytes investigated while the limits of quantitation determined under the same conditions were in the nmol/L range.

Enhancing concentration and mass sensitivities for liquid chromatography trace analysis of clopyralid in drinking water.

PubMed

Gu, Binghe; Meldrum, Brian; McCabe, Terry; Phillips, Scott

2012-01-01

A theoretical treatment was developed and validated that relates analyte concentration and mass sensitivities to injection volume, retention factor, particle diameter, column length, column inner diameter and detection wavelength in liquid chromatography, and sample volume and extracted volume in solid-phase extraction (SPE). The principles were applied to improve sensitivity for trace analysis of clopyralid in drinking water. It was demonstrated that a concentration limit of detection of 0.02 ppb (μg/L) for clopyralid could be achieved with the use of simple UV detection and 100 mL of a spiked drinking water sample. This enabled reliable quantitation of clopyralid at the targeted 0.1 ppb level. Using a buffered solution as the elution solvent (potassium acetate buffer, pH 4.5, containing 10% of methanol) in the SPE procedures was found superior to using 100% methanol, as it provided better extraction recovery (70-90%) and precision (5% for a concentration at 0.1 ppb level). In addition, the eluted sample was in a weaker solvent than the mobile phase, permitting the direct injection of the extracted sample, which enabled a faster cycle time of the overall analysis. Excluding the preparation of calibration standards, the analysis of a single sample, including acidification, extraction, elution and LC run, could be completed in 1 h. The method was used successfully for the determination of clopyralid in over 200 clopyralid monoethanolamine-fortified drinking water samples, which were treated with various water treatment resins. Copyright © 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim.

Personal exposure to aerosolized red tide toxins (brevetoxins).

PubMed

Cheng, Yung Sung; Zhou, Yue; Naar, Jerome; Irvin, C Mitch; Su, Wei-Chung; Fleming, Lora E; Kirkpatrick, Barbara; Pierce, Richard H; Backer, Lorraine C; Baden, Daniel G

2010-06-01

Florida red tides occur annually in the Gulf of Mexico from blooms of the marine dinoflagellate, Karenia brevis, which produces highly potent natural polyether toxins, brevetoxins. Several epidemiologic studies have demonstrated that human exposure to red tide aerosol could result in increased respiratory symptoms. Environmental monitoring of aerosolized brevetoxins was performed using a high-volume sampler taken hourly at fixed locations on Siesta Beach, Florida. Personal exposure was monitored using personal air samplers and taking nasal swab samples from the subjects who were instructed to spend 1 hr on Sarasota Beach during two sampling periods of an active Florida red tide event in March 2005, and in May 2008 when there was no red tide. Results showed that the aerosolized brevetoxins from the personal sampler were in modest agreement with the environmental concentration taken from a high-volume sampler. Analysis of nasal swab samples for brevetoxins demonstrated 68% positive samples in the March 2005 sampling period when air concentrations of brevetoxins were between 50 to 120 ng/m(3) measured with the high-volume sampler. No swab samples showed detectable levels of brevetoxins in the May 2008 study, when all personal samples were below the limit of detection. However, there were no statistical correlations between the amounts of brevetoxins detected in the swab samples with either the environmental or personal concentration. Results showed that the personal sample might provide an estimate of individual exposure level. Nasal swab samples showed that brevetoxins indeed were inhaled and deposited in the nasal passage during the March 2005 red tide event.

Probability density function of non-reactive solute concentration in heterogeneous porous formations.

PubMed

Bellin, Alberto; Tonina, Daniele

2007-10-30

Available models of solute transport in heterogeneous formations lack in providing complete characterization of the predicted concentration. This is a serious drawback especially in risk analysis where confidence intervals and probability of exceeding threshold values are required. Our contribution to fill this gap of knowledge is a probability distribution model for the local concentration of conservative tracers migrating in heterogeneous aquifers. Our model accounts for dilution, mechanical mixing within the sampling volume and spreading due to formation heterogeneity. It is developed by modeling local concentration dynamics with an Ito Stochastic Differential Equation (SDE) that under the hypothesis of statistical stationarity leads to the Beta probability distribution function (pdf) for the solute concentration. This model shows large flexibility in capturing the smoothing effect of the sampling volume and the associated reduction of the probability of exceeding large concentrations. Furthermore, it is fully characterized by the first two moments of the solute concentration, and these are the same pieces of information required for standard geostatistical techniques employing Normal or Log-Normal distributions. Additionally, we show that in the absence of pore-scale dispersion and for point concentrations the pdf model converges to the binary distribution of [Dagan, G., 1982. Stochastic modeling of groundwater flow by unconditional and conditional probabilities, 2, The solute transport. Water Resour. Res. 18 (4), 835-848.], while it approaches the Normal distribution for sampling volumes much larger than the characteristic scale of the aquifer heterogeneity. Furthermore, we demonstrate that the same model with the spatial moments replacing the statistical moments can be applied to estimate the proportion of the plume volume where solute concentrations are above or below critical thresholds. Application of this model to point and vertically averaged bromide concentrations from the first Cape Cod tracer test and to a set of numerical simulations confirms the above findings and for the first time it shows the superiority of the Beta model to both Normal and Log-Normal models in interpreting field data. Furthermore, we show that assuming a-priori that local concentrations are normally or log-normally distributed may result in a severe underestimate of the probability of exceeding large concentrations.

Automated agar plate streaker: a linear plater on Society for Biomolecular Sciences standard plates.

PubMed

King, Gregory W; Kath, Gary S; Siciliano, Sal; Simpson, Neal; Masurekar, Prakash; Sigmund, Jan; Polishook, Jon; Skwish, Stephen; Bills, Gerald; Genilloud, Olga; Peláez, Fernando; Martín, Jesus; Dufresne, Claude

2006-09-01

Several protocols for bacterial isolation and techniques for aerobic plate counting rely on the use of a spiral plater to deposit concentration gradients of microbial suspensions onto a circular agar plate to isolate colony growth. The advantage of applying a gradient of concentrations across the agar surface is that the original microbiological sample can be applied at a single concentration rather than as multiple serial dilutions. The spiral plater gradually dilutes the sample across a compact area and therefore saves time preparing dilutions and multiple agar plates. Commercial spiral platers are not automated and require manual sample loading. Dispensing of the sample volume and rate of gradients are often very limited in range. Furthermore, the spiral sample application cannot be used with rectangular microplates. Another limitation of commercial spiral platers is that they are useful only for dilute, filtered suspensions and cannot plate suspensions of coarse organic particles therefore precluding the use of many kinds of microorganism-containing substrata. An automated agar plate spreader capable of processing 99 rectangular microplates in unattended mode is described. This novel instrument is capable of dispensing discrete volumes of sample in a linear pattern. It can be programmed to dispense a sample suspense at a uniform application rate or across a decreasing concentration gradient.

Evaluation of needle trap micro-extraction and automatic alveolar sampling for point-of-care breath analysis.

PubMed

Trefz, Phillip; Rösner, Lisa; Hein, Dietmar; Schubert, Jochen K; Miekisch, Wolfram

2013-04-01

Needle trap devices (NTDs) have shown many advantages such as improved detection limits, reduced sampling time and volume, improved stability, and reproducibility if compared with other techniques used in breath analysis such as solid-phase extraction and solid-phase micro-extraction. Effects of sampling flow (2-30 ml/min) and volume (10-100 ml) were investigated in dry gas standards containing hydrocarbons, aldehydes, and aromatic compounds and in humid breath samples. NTDs contained (single-bed) polymer packing and (triple-bed) combinations of divinylbenzene/Carbopack X/Carboxen 1000. Substances were desorbed from the NTDs by means of thermal expansion and analyzed by gas chromatography-mass spectrometry. An automated CO2-controlled sampling device for direct alveolar sampling at the point-of-care was developed and tested in pilot experiments. Adsorption efficiency for small volatile organic compounds decreased and breakthrough increased when sampling was done with polymer needles from a water-saturated matrix (breath) instead from dry gas. Humidity did not affect analysis with triple-bed NTDs. These NTDs showed only small dependencies on sampling flow and low breakthrough from 1-5 %. The new sampling device was able to control crucial parameters such as sampling flow and volume. With triple-bed NTDs, substance amounts increased linearly with increasing sample volume when alveolar breath was pre-concentrated automatically. When compared with manual sampling, automatic sampling showed comparable or better results. Thorough control of sampling and adequate choice of adsorption material is mandatory for application of needle trap micro-extraction in vivo. The new CO2-controlled sampling device allows direct alveolar sampling at the point-of-care without the need of any additional sampling, storage, or pre-concentration steps.

Potential for formation of disinfection by-products from storage of chlorinated surface water in the Basalt aquifer near Fallon, Nevada

USGS Publications Warehouse

Fram, Miranda S.; Maurer, Douglas K.; Lico, Michael S.

2005-01-01

Increased pumpage from a basalt aquifer near Fallon, Nevada, has caused its water levels to decline and has induced changes in the quality of water pumped from the basalt. The aquifer is the sole source of water for municipal supply to the city of Fallon, the Naval Air Station Fallon, and the Fallon Paiute-Shoshone Tribe. These changes may be mitigated by storage of surface water in the basalt for subsequent use. Because chlorination of the surface water may be required for storage, the U.S. Geological Survey, in cooperation with the Fallon Paiute-Shoshone Tribe, made laboratory tests using laboratory carbon-organic-free water, surface-water, ground-water, and basaltic-rock samples to determine the potential for formation of disinfection by-products. Experiments with water samples only (no rock and no chlorine) indicated no change in dissolved-organic-carbon (DOC) concentrations over a 20-day reaction period; whereas, all experiments using rock, water, and no chlorine indicated an increase in DOC concentrations. The greatest increase in DOC concentrations for all three water samples occurred in experiments with the rock samples from outcrops on Rattlesnake Hill. Experiments with water only and chlorine yielded a total trihalomethane (THM) concentration of 97.4 ?g/L for the ground-water sample and 347 ?g/L for the surface-water sample. Experiments with mixtures of water, rocks, and chlorine indicated that reactions with the rock consumed chlorine and released significant amounts of organic carbon from the rock, increasing the DOC concentration in the water. The organic carbon in the rocks likely is associated with the secondary clay minerals that line vesicles and fractures in the rocks. THM concentrations were greatest, from 335 to 909 ?g/L, for surface water equilibrated with rock samples from Rattlesnake Hill. However, the concentration of chlorine required to produce these high THM concentrations ranged from 18 to 84 mg/L. The results of the experiments suggest that the amount of organic carbon released from the rocks during successive cycles of recharge, storage, and recovery of chlorinated surface water may be relatively small. The chlorine demand of the rocks is so large that all of the free chlorine in the entire volume of recharged water likely would be consumed by only a very small volume of the aquifer surrounding an injection well, or beneath an infiltration bed. The majority of the volume of the aquifer filled by the stored water likely would never come in contact with free chlorine, and the increases in concentration of DOC observed in these experiments likely would occur in a very small volume of the stored water. For this reason, increases in concentration of THMs for the entire volume of water stored also likely would be considerably less than those measured in these experiments. To test this hypothesis, additional laboratory experiments using varying levels of chlorination, varying lengths of reaction periods, and repeated cycles of chlorination would be useful. A field experiment made at a small scale in an isolated part of the basalt aquifer would aid in the design of an operational system.

Initial susceptibility and viscosity properties of low concentration ɛ-Fe3 N based magnetic fluid

NASA Astrophysics Data System (ADS)

Huang, Wei; Wu, Jianmin; Guo, Wei; Li, Rong; Cui, Liya

2007-03-01

In this paper, the initial susceptibility of ɛ-Fe3N magnetic fluid at volume concentrations in the range Φ = 0.0 ˜ 0.0446 are measured. Compared with the experimental initial susceptibility, the Langevin, Weiss and Onsager susceptibility were calculated using the data obtained from the low concentration ɛ-Fe3N magnetic fluid samples. The viscosity of the ɛ-Fe3N magnetic fluid at the same concentrations is measured. The result shows that, the initial susceptibility of the low concentration ɛ-Fe3N magnetic fluid is proportional to the concentration. A linear relationship between relative viscosity and the volume fraction is observed when the concentration Φ < 0.02.

Problems associated with using filtration to define dissolved trace element concentrations in natural water samples

USGS Publications Warehouse

Horowitz, A.J.; Lum, K.R.; Garbarino, J.R.; Hall, G.E.M.; Lemieux, C.; Demas, C.R.

1996-01-01

Field and laboratory experiments indicate that a number of factors associated with filtration other than just pore size (e.g., diameter, manufacturer, volume of sample processed, amount of suspended sediment in the sample) can produce significant variations in the 'dissolved' concentrations of such elements as Fe, Al, Cu, Zn, Pb, Co, and Ni. The bulk of these variations result from the inclusion/exclusion of colloidally associated trace elements in the filtrate, although dilution and sorption/desorption from filters also may be factors. Thus, dissolved trace element concentrations quantitated by analyzing filtrates generated by processing whole water through similar pore-sized filters may not be equal or comparable. As such, simple filtration of unspecified volumes of natural water through unspecified 0.45-??m membrane filters may no longer represent an acceptable operational definition for a number of dissolved chemical constituents.

Improved sensitivity of the urine CAA lateral-flow assay for diagnosing active Schistosoma infections by using larger sample volumes.

PubMed

Corstjens, Paul L A M; Nyakundi, Ruth K; de Dood, Claudia J; Kariuki, Thomas M; Ochola, Elizabeth A; Karanja, Diana M S; Mwinzi, Pauline N M; van Dam, Govert J

2015-04-22

Accurate determination of Schistosoma infection rates in low endemic regions to examine progress towards interruption of transmission and elimination requires highly sensitive diagnostic tools. An existing lateral flow (LF) based test demonstrating ongoing infections through detection of worm circulating anodic antigen (CAA), was improved for sensitivity through implementation of a protocol allowing increased sample input. Urine is the preferred sample as collection is non-invasive and sample volume is generally not a restriction. Centrifugal filtration devices provided a method to concentrate supernatant of urine samples extracted with trichloroacetic acid (TCA). For field trials a practical sample volume of 2 mL urine allowed detection of CAA down to 0.3 pg/mL. The method was evaluated on a set of urine samples (n = 113) from an S. mansoni endemic region (Kisumu, Kenya) and compared to stool microscopy (Kato Katz, KK). In this analysis true positivity was defined as a sample with either a positive KK or UCAA test. Implementation of the concentration method increased clinical sensitivity (Sn) from 44 to 98% when moving from the standard 10 μL (UCAA10 assay) to 2000 μL (UCAA2000 assay) urine sample input. Sn for KK varied between 23 and 35% for a duplicate KK (single stool, two slides) to 52% for a six-fold KK (three consecutive day stools, two slides). The UCAA2000 assay indicated 47 positive samples with CAA concentration above 0.3 pg/mL. The six-fold KK detected 25 egg positives; 1 sample with 2 eggs detected in the 6-fold KK was not identified with the UCAA2000 assay. Larger sample input increased Sn of the UCAA assay to a level indicating 'true' infection. Only a single 2 mL urine sample is needed, but analysing larger sample volumes could still increase test accuracy. The UCAA2000 test is an appropriate candidate for accurate identification of all infected individuals in low-endemic regions. Assay materials do not require refrigeration and collected urine samples may be stored and transported to central test laboratories without the need to be frozen.

Systems and methods for the detection of low-level harmful substances in a large volume of fluid

DOE Office of Scientific and Technical Information (OSTI.GOV)

Carpenter, Michael V.; Roybal, Lyle G.; Lindquist, Alan

A method and device for the detection of low-level harmful substances in a large volume of fluid comprising using a concentrator system to produce a retentate and analyzing the retentate for the presence of at least one harmful substance. The concentrator system performs a method comprising pumping at least 10 liters of fluid from a sample source through a filter. While pumping, the concentrator system diverts retentate from the filter into a container. The concentrator system also recirculates at least part of the retentate in the container again through the filter. The concentrator system controls the speed of the pumpmore » with a control system thereby maintaining a fluid pressure less than 25 psi during the pumping of the fluid; monitors the quantity of retentate within the container with a control system, and maintains a reduced volume level of retentate and a target volume of retentate.« less

High performance concentration method for viruses in drinking water.

PubMed

Kunze, Andreas; Pei, Lu; Elsässer, Dennis; Niessner, Reinhard; Seidel, Michael

2015-09-15

According to the risk assessment of the WHO, highly infectious pathogenic viruses like rotaviruses should not be present in large-volume drinking water samples of up to 90 m(3). On the other hand, quantification methods for viruses are only operable in small volumes, and presently no concentration procedure for processing such large volumes has been reported. Therefore, the aim of this study was to demonstrate a procedure for processing viruses in-line of a drinking water pipeline by ultrafiltration (UF) and consecutive further concentration by monolithic filtration (MF) and centrifugal ultrafiltration (CeUF) of viruses to a final 1-mL sample. For testing this concept, the model virus bacteriophage MS2 was spiked continuously in UF instrumentation. Tap water was processed in volumes between 32.4 m(3) (22 h) and 97.7 m(3) (72 h) continuously either in dead-end (DE) or cross-flow (CF) mode. Best results were found by DE-UF over 22 h. The concentration of MS2 was increased from 4.2×10(4) GU/mL (genomic units per milliliter) to 3.2×10(10) GU/mL and from 71 PFU/mL to 2×10(8) PFU/mL as determined by qRT-PCR and plaque assay, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

Using large volume samplers for the monitoring of particle bound micro pollutants in rivers

NASA Astrophysics Data System (ADS)

Kittlaus, Steffen; Fuchs, Stephan

2015-04-01

The requirements of the WFD as well as substance emission modelling at the river basin scale require stable monitoring data for micro pollutants. The monitoring concepts applied by the local authorities as well as by many scientists use single sampling techniques. Samples from water bodies are usually taken in volumes of about one litre and depending on predetermined time steps or through discharge thresholds. For predominantly particle bound micro pollutants the small sample size of about one litre results in a very small amount of suspended particles. To measure micro pollutant concentrations in these samples is demanding and results in a high uncertainty of the measured concentrations, if the concentration is above the detection limit in the first place. In many monitoring programs most of the measured values were below the detection limit. This results in a high uncertainty if river loads were calculated from these data sets. The authors propose a different approach to gain stable concentration values for particle bound micro pollutants from river monitoring: A mixed sample of about 1000 L was pumped in a tank with a dirty-water pump. The sampling usually is done discharge dependant by using a gauge signal as input for the control unit. After the discharge event is over or the tank is fully filled, the suspended solids settle in the tank for 2 days. After this time a clear separation of water and solids can be shown. A sample (1 L) from the water phase and the total mass of the settled solids (about 10 L) are taken to the laboratory for analysis. While the micro pollutants can't hardly be detected in the water phase, the signal from the sediment is high above the detection limit, thus certain and very stable. From the pollutant concentration in the solid phase and the total tank volume the initial pollutant concentration in the sample can be calculated. If the concentration in the water phase is detectable, it can be used to correct the total load. This relatively low cost approach (less costs for analysis because of small sample number) allows to quantify the pollutant load, to derive dissolved-solid partition coefficients and to quantify the pollutant load in different particle size classes.

Model-based monitoring of stormwater runoff quality.

PubMed

Birch, Heidi; Vezzaro, Luca; Mikkelsen, Peter Steen

2013-01-01

Monitoring of micropollutants (MP) in stormwater is essential to evaluate the impacts of stormwater on the receiving aquatic environment. The aim of this study was to investigate how different strategies for monitoring of stormwater quality (combining a model with field sampling) affect the information obtained about MP discharged from the monitored system. A dynamic stormwater quality model was calibrated using MP data collected by automatic volume-proportional sampling and passive sampling in a storm drainage system on the outskirts of Copenhagen (Denmark) and a 10-year rain series was used to find annual average (AA) and maximum event mean concentrations. Use of this model reduced the uncertainty of predicted AA concentrations compared to a simple stochastic method based solely on data. The predicted AA concentration, obtained by using passive sampler measurements (1 month installation) for calibration of the model, resulted in the same predicted level but with narrower model prediction bounds than by using volume-proportional samples for calibration. This shows that passive sampling allows for a better exploitation of the resources allocated for stormwater quality monitoring.

10 CFR 74.45 - Measurements and measurement control.

Code of Federal Regulations, 2013 CFR

2013-01-01

... measurements, obtaining samples, and performing laboratory analyses for element concentration and isotope... of random error behavior. On a predetermined schedule, the program shall include, as appropriate: (i) Replicate analyses of individual samples; (ii) Analysis of replicate process samples; (iii) Replicate volume...

10 CFR 74.45 - Measurements and measurement control.

Code of Federal Regulations, 2014 CFR

2014-01-01

... measurements, obtaining samples, and performing laboratory analyses for element concentration and isotope... of random error behavior. On a predetermined schedule, the program shall include, as appropriate: (i) Replicate analyses of individual samples; (ii) Analysis of replicate process samples; (iii) Replicate volume...

10 CFR 74.45 - Measurements and measurement control.

Code of Federal Regulations, 2012 CFR

2012-01-01

... measurements, obtaining samples, and performing laboratory analyses for element concentration and isotope... of random error behavior. On a predetermined schedule, the program shall include, as appropriate: (i) Replicate analyses of individual samples; (ii) Analysis of replicate process samples; (iii) Replicate volume...

Atmospheric CO2 Records from Sites in the Umweltbundesamt (UBA) Air Sampling Network (1972 - 1997)

DOE Data Explorer

Fricke, W. [Umweltbundesamt, Offenbach/Main, Germany; Wallasch, M. [Umweltbundesamt, Offenbach/Main, Germany; Uhse, Karin [Umweltbundesamt, Offenbach/Main, Germany; Schmidt, Martina [University of Heidelberg, Heidelberg, Germany; Levin, Ingeborg [University of Heidelberg, Heidelberg, Germany

1998-01-01

Air samples for the purpose of monitoring atmospheric CO2 were collected from five sites in the UBA air sampling network. Annual atmospheric CO2 concentrations at Brotjacklriegel rose from 331.63 parts per million by volume (ppmv) in 1972 to 353.12 ppmv in 1988. Because of the site's forest location, the monthly atmospheric CO2 record from Brotjacklriegel exhibits very large seasonal amplitude. This amplitude reached almost 40 ppmv in 1985. Minimum mixing ratios are recorded at Brotjacklriegel during July-September; maximum values, during November-March. CO2 concentrations at Deuselbach rose from 340.82 parts per million by volume (ppmv) in 1972 to 363.76 ppmv in 1989. The monthly atmospheric CO2 record from Deuselbach is influenced by local agricultural activities and photosynthetic depletion but does not exhibit the large seasonal amplitude observed at other UBA monitoring sites. Minimum monthly atmospheric CO2 mixing ratios at Deuselbach are typically observed in August but may appear as early as June. Maximum values are seen in the record for November-March. Atmospheric CO2 concentrations at Schauinsland rose from ~328 parts per million by volume (ppmv) in 1972 to ~365 ppmv in 1997. This represents a growth rate of approximately 1.5 ppmv per year. The Schauinsland site is considered the least contaminated of the UBA sites. CO2 concentrations at Waldhof rose from 346.82 parts per million by volume (ppmv) in 1972 to 372.09 ppmv in 1993. The Waldhof site is subject to pollution sources; consequently, the monthly atmospheric CO2 record exhibits a large seasonal amplitude. Atmospheric CO2 concentrations at Westerland rose from ~329 parts per million by volume (ppmv) in 1973 to ~364 ppmv in 1997. The atmospheric CO2 record from Westerland shows a seasonal pattern similar to other UBA sites; minimum values are recorded during July-September; maximum mixing ratios during November-March.

AUTOMATED DEAD-END ULTRAFILTRATION FOR ENHANCED SURVEILLANCE OF LEGIONELLA 2 PNEUMOPHILA AND LEGIONELLA SPP. IN COOLING TOWER WATERS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brigmon, R.; Leskinen, S.; Kearns, E.

2011-10-10

Detection of Legionella pneumophila in cooling towers and domestic hot water systems involves concentration by centrifugation or membrane filtration prior to inoculation onto growth media or analysis using techniques such as PCR or immunoassays. The Portable Multi-use Automated Concentration System (PMACS) was designed for concentrating microorganisms from large volumes of water in the field and was assessed for enhancing surveillance of L. pneumophila at the Savannah River Site, SC. PMACS samples (100 L; n = 28) were collected from six towers between August 2010 and April 2011 with grab samples (500 ml; n = 56) being collected before and aftermore » each PMACS sample. All samples were analyzed for the presence of L. pneumophila by direct fluorescence immunoassay (DFA) using FITC-labeled monoclonal antibodies targeting serogroups 1, 2, 4 and 6. QPCR was utilized for detection of Legionella spp. in the same samples. Counts of L. pneumophila from DFA and of Legionella spp. from qPCR were normalized to cells/L tower water. Concentrations were similar between grab and PMACS samples collected throughout the study by DFA analysis (P = 0.4461; repeated measures ANOVA). The same trend was observed with qPCR. However, PMACS concentration proved advantageous over membrane filtration by providing larger volume, more representative samples of the cooling tower environment, which led to reduced variability among sampling events and increasing the probability of detection of low level targets. These data highlight the utility of the PMACS for enhanced surveillance of L. pneumophila by providing improved sampling of the cooling tower environment.« less

Sampling and physical characterization of diesel exhaust aerosols. SAE Paper 770720

DOE Office of Scientific and Technical Information (OSTI.GOV)

Verrant, J.A.; Kittelson, D.A.

Diesel exhaust aerosols are highly dynamic and therefore, difficult to sample without introducing falsification. This paper describes a study of these aerosols using a rapid dilution sampling system and an electrical aerosol analyzer. An Onan single cylinder indirect injection engine was used as an exhaust source. The sampler diluted the exhaust with clean air in ratios of 400:1 to 600:1 in order to prevent sample falsification by condensation and coagulation. The electrical aerosol analyzer was used to determine particle size and concentration. Volume concentration in the exhaust ranged from 2000 to 50,000 ..mu.. m/sup 3/ cm/sup -3/ which correspond tomore » mass loadings of 2.0 to 50 mg m/sup -3/ (assuming a density of 1 gm cm/sup -3/). Volume geometric mean diameters ranged from 0.12 to 0.19 ..mu..m. Evaporation and coagulation effects on diesel aerosols were observed by aging in a Teflon holding bag. A simple evaporation model was fit to the decrease of aerosol volume concentration with time. The fit revealed that the aerosols evaporated as if they were composed of normal paraffins in the 350 to 500 molecular weight range. Although the sample dilution system used in this study may alter the sample somewhat, it is probably analogous to what happens at the tailpipe of a vehicle. Measurements taken on a test track in the exhaust plume of a Peugeot 504 diesel showed aerosol size distributions very similar to those measured in our laboratory studies.« less

Concentration determination of nucleic acids and proteins using the micro-volume BioSpec-nano-spectrophotometer.

PubMed

Sukumaran, Suja

2011-02-17

Nucleic acid quantitation procedures have advanced significantly in the last three decades. More and more, molecular biologists require consistent small-volume analysis of nucleic acid samples for their experiments. The BioSpec-nano provides a potential solution to the problems of inaccurate, non-reproducible results, inherent in current DNA quantitation methods, via specialized optics and a sensitive PDA detector. The BioSpec-nano also has automated functionality such that mounting, measurement, and cleaning are done by the instrument, thereby eliminating tedious, repetitive, and inconsistent placement of the fiber optic element and manual cleaning. In this study, data is presented on the quantification of DNA and protein, as well as on measurement reproducibility and accuracy. Automated sample contact and rapid scanning allows measurement in three seconds, resulting in excellent throughput. Data analysis is carried out using the built-in features of the software. The formula used for calculating DNA concentration is: Sample Concentration = DF · (OD260-OD320)· NACF (1) Where DF = sample dilution factor and NACF = nucleic acid concentration factor. The Nucleic Acid concentration factor is set in accordance with the analyte selected. Protein concentration results can be expressed as μg/mL or as moles/L by entering e280 and molecular weight values respectively. When residue values for Tyr, Trp and Cysteine (S-S bond) are entered in the e280Calc tab, the extinction coefficient values are calculated as e280 = 5500 x (Trp residues) + 1490 x (Tyr residues) + 125 x (cysteine S-S bond). The e280 value is used by the software for concentration calculation. In addition to concentration determination of nucleic acids and protein, the BioSpec-nano can be used as an ultra micro-volume spectrophotometer for many other analytes or as a standard spectrophotometer using 5 mm pathlength cells.

Concentration Determination of Nucleic Acids and Proteins Using the Micro-volume Bio-spec Nano Spectrophotometer

PubMed Central

Sukumaran, Suja

2011-01-01

Nucleic Acid quantitation procedures have advanced significantly in the last three decades. More and more, molecular biologists require consistent small-volume analysis of nucleic acid samples for their experiments. The BioSpec-nano provides a potential solution to the problems of inaccurate, non-reproducible results, inherent in current DNA quantitation methods, via specialized optics and a sensitive PDA detector. The BioSpec-nano also has automated functionality such that mounting, measurement, and cleaning are done by the instrument, thereby eliminating tedious, repetitive, and inconsistent placement of the fiber optic element and manual cleaning. In this study, data is presented on the quantification of DNA and protein, as well as on measurement reproducibility and accuracy. Automated sample contact and rapid scanning allows measurement in three seconds, resulting in excellent throughput. Data analysis is carried out using the built-in features of the software. The formula used for calculating DNA concentration is: Sample Concentration = DF · (OD260-OD320)· NACF (1) Where DF = sample dilution factor and NACF = nucleic acid concentration factor. The Nucleic Acid concentration factor is set in accordance with the analyte selected1. Protein concentration results can be expressed as μg/ mL or as moles/L by entering e280 and molecular weight values respectively. When residue values for Tyr, Trp and Cysteine (S-S bond) are entered in the e280Calc tab, the extinction coefficient values are calculated as e280 = 5500 x (Trp residues) + 1490 x (Tyr residues) + 125 x (cysteine S-S bond). The e280 value is used by the software for concentration calculation. In addition to concentration determination of nucleic acids and protein, the BioSpec-nano can be used as an ultra micro-volume spectrophotometer for many other analytes or as a standard spectrophotometer using 5 mm pathlength cells. PMID:21372788

A rapid, highly sensitive and culture-free detection of pathogens from blood by positive enrichment.

PubMed

Vutukuru, Manjula Ramya; Sharma, Divya Khandige; Ragavendar, M S; Schmolke, Susanne; Huang, Yiwei; Gumbrecht, Walter; Mitra, Nivedita

2016-12-01

Molecular diagnostics is a promising alternative to culture based methods for the detection of bloodstream infections, notably due to its overall lower turnaround time when starting directly from patient samples. Whole blood is usually the starting diagnostic sample in suspected bloodstream infections. The detection of low concentrations of pathogens in blood using a molecular assay necessitates a fairly high starting volume of blood sample in the range of 5-10mL. This large volume of blood sample has a substantial accompanying human genomic content that interferes with pathogen detection. In this study, we have established a workflow using magnetic beads coated with Apolipoprotein H that makes it possible to concentrate pathogens from a 5.0mL whole blood sample, thereby enriching pathogens from whole blood background and also reducing the sample volume to ~200μL or less. We have also demonstrated that this method of enrichment allows detection of 1CFU/mL of Escherichia coli, Enterococcus gallinarum and Candida tropicalis from 5mL blood using quantitative PCR; a detection limit that is not possible in unenriched samples. The enrichment method demonstrated here took 30min to complete and can be easily integrated with various downstream molecular and microbiological techniques. Copyright © 2016 Elsevier B.V. All rights reserved.

Investigation of a systematic offset in the measurement of organic carbon with a semicontinuous analyzer.

PubMed

Offenberg, John H; Lewandowski, Michael; Edney, Edward O; Kleindienst, Tadeusz E; Jaoui, Mohammed

2007-05-01

Organic carbon (OC) was measured semicontinuously in laboratory experiments of steady-state secondary organic aerosol formed by hydrocarbon + nitrogen oxide irradiations. Examination of the mass of carbon measured on the filter for various sample volumes reveals a systematic offset that is not observed when performing an instrumental blank. These findings suggest that simple subtraction of instrumental blanks determined as the standard analysis without sample collection (i.e., by cycling the pump and valves yet filtering zero liters of air followed by routine chemical analysis) from measured concentrations may be inadequate. This may be especially true for samples collected through the filtration of small air volumes wherein the influence of the systematic offset is greatest. All of the experiments show that filtering a larger volume of air minimizes the influence of contributions from the systematic offset. Application of these results to measurements of ambient concentrations of carbonaceous aerosol suggests a need for collection of sufficient carbon mass to minimize the relative influence of the offset signal.

Effect of masticatory stimulation on the quantity and quality of saliva and the salivary metabolomic profile.

PubMed

Okuma, Nobuyuki; Saita, Makiko; Hoshi, Noriyuki; Soga, Tomoyoshi; Tomita, Masaru; Sugimoto, Masahiro; Kimoto, Katsuhiko

2017-01-01

This study characterized the changes in quality and quantity of saliva, and changes in the salivary metabolomic profile, to understand the effects of masticatory stimulation. Stimulated and unstimulated saliva samples were collected from 55 subjects and salivary hydrophilic metabolites were comprehensively quantified using capillary electrophoresis-time-of-flight mass spectrometry. In total, 137 metabolites were identified and quantified. The concentrations of 44 metabolites in stimulated saliva were significantly higher than those in unstimulated saliva. Pathway analysis identified the upregulation of the urea cycle and synthesis and degradation pathways of glycine, serine, cysteine and threonine in stimulated saliva. A principal component analysis revealed that the effect of masticatory stimulation on salivary metabolomic profiles was less dependent on sample population sex, age, and smoking. The concentrations of only 1 metabolite in unstimulated saliva, and of 3 metabolites stimulated saliva, showed significant correlation with salivary secretion volume, indicating that the salivary metabolomic profile and salivary secretion volume were independent factors. Masticatory stimulation affected not only salivary secretion volume, but also metabolite concentration patterns. A low correlation between the secretion volume and these patterns supports the conclusion that the salivary metabolomic profile may be a new indicator to characterize masticatory stimulation.

MACRO- MICRO-PURGE SOIL GAS SAMPLING METHODS FOR THE COLLECTION OF CONTAMINANT VAPORS

EPA Science Inventory

Purging influence on soil gas concentrations for volatile organic compounds (VOCs), as affected by sampling tube inner diameter and sampling depth (i.e., dead-space purge volume), was evaluated at different field sites. A macro-purge sampling system consisted of a standard hollo...

Development of a solid-phase extraction system modified for preconcentration of emerging contaminants in large sample volumes from rivers of the lagoon system in the city of Rio de Janeiro, Brazil.

PubMed

Lopes, Vitor Sergio Almeida; Riente, Roselene Ribeiro; da Silva, Alexsandro Araújo; Torquilho, Delma Falcão; Carreira, Renato da Silva; Marques, Mônica Regina da Costa

2016-09-15

A single method modified for monitoring of emerging contaminants in river water was developed for large sample volumes. Water samples from rivers of the lagoon system in the city of Rio de Janeiro (Brazil) were analyzed by the SPE-HPLC-MS-TOF analytical method. Acetaminophen was detected in four rivers in the concentration range of 0.09μgL(-1) to 0.14μgL(-1). Salicylic acid was also found in the four rivers in the concentration range of 1.65μgL(-1) to 4.81μgL(-1). Bisphenol-A was detected in all rivers in the concentration range of 1.37μgL(-1) to 39.86μgL(-1). Diclofenac was found in only one river, with concentration of 0.22μgL(-1). The levels of emerging organic pollutants in the water samples of the Jacarepaguá hydrographical basin are significant. The compounds are not routinely monitored and present potential risks to environmental health. Copyright © 2016 Elsevier Ltd. All rights reserved.

Evaluating performance of stormwater sampling approaches using a dynamic watershed model.

PubMed

Ackerman, Drew; Stein, Eric D; Ritter, Kerry J

2011-09-01

Accurate quantification of stormwater pollutant levels is essential for estimating overall contaminant discharge to receiving waters. Numerous sampling approaches exist that attempt to balance accuracy against the costs associated with the sampling method. This study employs a novel and practical approach of evaluating the accuracy of different stormwater monitoring methodologies using stormflows and constituent concentrations produced by a fully validated continuous simulation watershed model. A major advantage of using a watershed model to simulate pollutant concentrations is that a large number of storms representing a broad range of conditions can be applied in testing the various sampling approaches. Seventy-eight distinct methodologies were evaluated by "virtual samplings" of 166 simulated storms of varying size, intensity and duration, representing 14 years of storms in Ballona Creek near Los Angeles, California. The 78 methods can be grouped into four general strategies: volume-paced compositing, time-paced compositing, pollutograph sampling, and microsampling. The performances of each sampling strategy was evaluated by comparing the (1) median relative error between the virtually sampled and the true modeled event mean concentration (EMC) of each storm (accuracy), (2) median absolute deviation about the median or "MAD" of the relative error or (precision), and (3) the percentage of storms where sampling methods were within 10% of the true EMC (combined measures of accuracy and precision). Finally, costs associated with site setup, sampling, and laboratory analysis were estimated for each method. Pollutograph sampling consistently outperformed the other three methods both in terms of accuracy and precision, but was the most costly method evaluated. Time-paced sampling consistently underestimated while volume-paced sampling over estimated the storm EMCs. Microsampling performance approached that of pollutograph sampling at a substantial cost savings. The most efficient method for routine stormwater monitoring in terms of a balance between performance and cost was volume-paced microsampling, with variable sample pacing to ensure that the entirety of the storm was captured. Pollutograph sampling is recommended if the data are to be used for detailed analysis of runoff dynamics.

Surface sampling concentration and reaction probe with controller to adjust sampling position

DOEpatents

Van Berkel, Gary J.; ElNaggar, Mariam S.

2016-07-19

A method of analyzing a chemical composition of a specimen is described. The method can include providing a probe comprising an outer capillary tube and an inner capillary tube disposed co-axially within the outer capillary tube, where the inner and outer capillary tubes define a solvent capillary and a sampling capillary in fluid communication with one another at a distal end of the probe; contacting a target site on a surface of a specimen with a solvent in fluid communication with the probe; maintaining a plug volume proximate a solvent-specimen interface, wherein the plug volume is in fluid communication with the probe; draining plug sampling fluid from the plug volume through the sampling capillary; and analyzing a chemical composition of the plug sampling fluid with an analytical instrument. A system for performing the method is also described.

Sexual steroids in serum and prostatic tissue of human non-cancerous prostate (STERPROSER trial).

PubMed

Neuzillet, Yann; Raynaud, Jean-Pierre; Radulescu, Camélia; Fiet, Jean; Giton, Franck; Dreyfus, Jean-François; Ghoneim, Tarek P; Lebret, Thierry; Botto, Henry

2017-11-01

The specific involvement of the sex steroids in the growth of the prostatic tissue remains unclear. Sex steroid concentrations in plasma and in fresh surgical samples of benign central prostate were correlated to prostate volume. Monocentric prospective study performed between September 2014 and January 2017. Age, obesity parameters, and both serum and intraprostatic concentrations of sex steroids were collected complying with the latest Endocrine Society guidelines and the steroids assessed by GC/MS. Statistical calculations were adjusted for age and body mass index (BMI). Thirty-two patients, equally divided between normal- and high-volume prostate groups, were included in the analysis. High-volume prostate patients were older, heavier and had higher BMI. Comparison adjusted for age and BMI showed higher DHT concentrations in high-volume prostate. Both normal- and high-volume prostate tissues concentrate sex steroids in a similar way. Comparison of enzymatic activity surrogate marker ratios within tissue highlighted similar TT/E1 and TT/E2 ratios, and higher DHT/E1 ratio and lower DHT/PSA ratio in the high-volume prostates. STERPROSER trial provides evidence for higher DHT concentration in highvolume prostates, that could reflect either higher 5-alpha reductase expression or lower expression of downstream metabolizing enzymes such as 3a-hydoxysteroid dehydrogenase. © 2017 Wiley Periodicals, Inc.

A proposal to standardize reporting units for fecal immunochemical tests for hemoglobin.

PubMed

Fraser, Callum G; Allison, James E; Halloran, Stephen P; Young, Graeme P

2012-06-06

Fecal immunochemical tests for hemoglobin are replacing traditional guaiac fecal occult blood tests in population screening programs for many reasons. However, the many available fecal immunochemical test devices use a range of sampling methods, differ with regard to hemoglobin stability, and report hemoglobin concentrations in different ways. The methods for sampling, the mass of feces collected, and the volume and characteristics of the buffer used in the sampling device also vary among fecal immunochemical tests, making comparisons of test performance characteristics difficult. Fecal immunochemical test results may be expressed as the hemoglobin concentration in the sampling device buffer and, sometimes, albeit rarely, as the hemoglobin concentration per mass of feces. The current lack of consistency in units for reporting hemoglobin concentration is particularly problematic because apparently similar hemoglobin concentrations obtained with different devices can lead to very different clinical interpretations. Consistent adoption of an internationally accepted method for reporting results would facilitate comparisons of outcomes from these tests. We propose a simple strategy for reporting fecal hemoglobin concentration that will facilitate the comparison of results between fecal immunochemical test devices and across clinical studies. Such reporting is readily achieved by defining the mass of feces sampled and the volume of sample buffer (with confidence intervals) and expressing results as micrograms of hemoglobin per gram of feces. We propose that manufacturers of fecal immunochemical tests provide this information and that the authors of research articles, guidelines, and policy articles, as well as pathology services and regulatory bodies, adopt this metric when reporting fecal immunochemical test results.

Quality of wet deposition in the Grand Calumet River watershed, northwestern Indiana, June 30, 1992-August 31, 1993

USGS Publications Warehouse

Willoughby, T.C.

1995-01-01

Northwestern Indiana is one of the most heavily industrialized and largest steel-producing areas in the United States. High temperature processes, such as fossil-fuel combustion and steel production, release contaminants to the atmosphere that may result in wet deposition being a major contributor to major ion and trace-metal loadings in north- western Indiana and Lake Michigan. A wet-deposition collection site was established at the Gary (Indiana) Regional Airport in June 1992 to monitor the chemical quality of wet deposition. Weekly samples were collected at this site from June 30, 1992, through August 31, 1993, and were analyzed for pH, specific conductance, and selected major ions and trace metals. Forty-eight samples collected during the study were of sufficient volumes for some of the determinations to be performed. Median constituent concentrations were determined for samples collected during warm weather and cold weather (November 1 through March 31). Median concentrations were substituted for missing values from samples with insufficient volumes for analysis of all the constituents of interest. Constituent concentrations were converted to weekly loadings. Two values were calculated to provide a range for the weekly loading for samples with measured concentrations of constituents less than the method reporting limit. The minimum weekly loading was computed by substituting zero for the constituent concentration; the maximum weekly loading was computed by substituting the method reporting limit for the concentration. If all of the sample concentrations measured were greater than the method reporting limit, an annual loading value was computed. The annual loadings could be used to assist in estimating the contribution of wet deposition to the total annual constituent loadings in the Grand Calumet River in northwestern Indiana.

Uncertainties in stormwater runoff data collection from a small urban catchment, Southeast China.

PubMed

Huang, Jinliang; Tu, Zhenshun; Du, Pengfei; Lin, Jie; Li, Qingsheng

2010-01-01

Monitoring data are often used to identify stormwater runoff characteristics and in stormwater runoff modelling without consideration of their inherent uncertainties. Integrated with discrete sample analysis and error propagation analysis, this study attempted to quantify the uncertainties of discrete chemical oxygen demand (COD), total suspended solids (TSS) concentration, stormwater flowrate, stormwater event volumes, COD event mean concentration (EMC), and COD event loads in terms of flow measurement, sample collection, storage and laboratory analysis. The results showed that the uncertainties due to sample collection, storage and laboratory analysis of COD from stormwater runoff are 13.99%, 19.48% and 12.28%. Meanwhile, flow measurement uncertainty was 12.82%, and the sample collection uncertainty of TSS from stormwater runoff was 31.63%. Based on the law of propagation of uncertainties, the uncertainties regarding event flow volume, COD EMC and COD event loads were quantified as 7.03%, 10.26% and 18.47%.

NP-PAH Interaction Dataset

EPA Pesticide Factsheets

Dataset presents concentrations of organic pollutants, such as polyaromatic hydrocarbon compounds, in water samples. Water samples of known volume and concentration were allowed to equilibrate with known mass of nanoparticles. The mixture was then ultracentrifuged and sampled for analysis. This dataset is associated with the following publication:Sahle-Demessie, E., A. Zhao, C. Han, B. Hann, and H. Grecsek. Interaction of engineered nanomaterials with hydrophobic organic pollutants.. Journal of Nanotechnology. Hindawi Publishing Corporation, New York, NY, USA, 27(28): 284003, (2016).

Liquid Metering Centrifuge Sticks (LMCS): A Centrifugal Approach to Metering Known Sample Volumes for Colorimetric Solid Phase Extraction (C-SPE)

NASA Technical Reports Server (NTRS)

Gazda, Daniel B.; Schultz, John R.; Clarke, Mark S.

2007-01-01

Phase separation is one of the most significant obstacles encountered during the development of analytical methods for water quality monitoring in spacecraft environments. Removing air bubbles from water samples prior to analysis is a routine task on earth; however, in the absence of gravity, this routine task becomes extremely difficult. This paper details the development and initial ground testing of liquid metering centrifuge sticks (LMCS), devices designed to collect and meter a known volume of bubble-free water in microgravity. The LMCS uses centrifugal force to eliminate entrapped air and reproducibly meter liquid sample volumes for analysis with Colorimetric Solid Phase Extraction (C-SPE). C-SPE is a sorption-spectrophotometric platform that is being developed as a potential spacecraft water quality monitoring system. C-SPE utilizes solid phase extraction membranes impregnated with analyte-specific colorimetric reagents to concentrate and complex target analytes in spacecraft water samples. The mass of analyte extracted from the water sample is determined using diffuse reflectance (DR) data collected from the membrane surface and an analyte-specific calibration curve. The analyte concentration can then be calculated from the mass of extracted analyte and the volume of the sample analyzed. Previous flight experiments conducted in microgravity conditions aboard the NASA KC-135 aircraft demonstrated that the inability to collect and meter a known volume of water using a syringe was a limiting factor in the accuracy of C-SPE measurements. Herein, results obtained from ground based C-SPE experiments using ionic silver as a test analyte and either the LMCS or syringes for sample metering are compared to evaluate the performance of the LMCS. These results indicate very good agreement between the two sample metering methods and clearly illustrate the potential of utilizing centrifugal forces to achieve phase separation and metering of water samples in microgravity.

A comparison of recovery of virus from wastewaters by beef extract-Celite, ferric chloride, and filter concentration procedures.

PubMed

Dahling, D R; Wright, B A

1988-12-01

An improved concentration method using sample volumes as large as 1500 ml has been developed to monitor for viruses in wastewaters. Non-precipitating dry beef extract powder is added to wastewater samples to give a 3% concentration and mixed until dissolved. This is followed by the addition of Celite as a virus adsorbent. By manipulating pH, viruses are eluted from the Celite in small volumes of phosphate buffer. This procedure was further tested without the aid of the Celite additives using a precipitating beef extract powder and substituting FeCl3 as an alternate reagent for the Celite. Comparison testing was also made with the currently recommended cartridge and disc filter procedures. In all cases, the non-precipitating beef extract-Celite method gave higher recovery rates in highly polluted waters.

Surface sampling concentration and reaction probe

DOEpatents

Van Berkel, Gary J; Elnaggar, Mariam S

2013-07-16

A method of analyzing a chemical composition of a specimen is described. The method can include providing a probe comprising an outer capillary tube and an inner capillary tube disposed co-axially within the outer capillary tube, where the inner and outer capillary tubes define a solvent capillary and a sampling capillary in fluid communication with one another at a distal end of the probe; contacting a target site on a surface of a specimen with a solvent in fluid communication with the probe; maintaining a plug volume proximate a solvent-specimen interface, wherein the plug volume is in fluid communication with the probe; draining plug sampling fluid from the plug volume through the sampling capillary; and analyzing a chemical composition of the plug sampling fluid with an analytical instrument. A system for performing the method is also described.

Factors associated with ruminal pH at herd level.

PubMed

Geishauser, T; Linhart, N; Neidl, A; Reimann, A

2012-08-01

The objective of this study was to evaluate factors associated with ruminal pH at herd level. Four hundred and thirty-two cows of a Thuringian dairy herd were sampled before claw trimming using a rumen fluid scoop. Volume and pH of the rumen sample were measured, and lactation number, percentage of concentrates in the ration, days in milk (DIM), time of day, and daily milk yield were recorded. Rumen sampling was successful in 99.8% of the cows. The average sample volume was 25 mL. Rumen sample pH decreased with increasing percentage of concentrates in the ration. Ruminal pH decreased from calving to 77 DIM, and grew subsequently to 330 DIM. During the day, rumen pH followed a sinus curve, with maxima in the morning (0915 h) and afternoon (1533 h), and a minimum around noon (1227 h). Ruminal pH decreased with increasing daily milk yield. Lactation number interacted with daily milk yield on rumen pH. The percentage of concentrates in the ration, DIM, time of day, and daily milk yield were significant factors affecting ruminal pH at the herd level. Copyright © 2012 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Drug Loading Capacity of Environmentally Sensitive Polymeric Microgels

NASA Astrophysics Data System (ADS)

McDonough, Ryan; Streletzky, Kiril; Bayachou, Mekki; Peiris, Pubudu

2009-10-01

Microgel nanoparticles consisting of cross-linked polymer hydroxypropyl cellulose chains have a temperature dependent volume phase transition, prompting the use of microgels for controlled drug transport. Drug particles aggregate in the slightly hydrophobic interior of microgels. Microgels are stored in equilibrium until the critical temperature (Tv) is reached and the volume phase transition limits available space, thus expelling the drugs. Our study was designed to test this property of microgels using amperometric electrochemical methods. A critical assumption was that small molecules inside microgels would not interact via diffusion with the electrode surface and thus total current would be decreased across the electrodes in a microgel sample. A room temperature (Troom) flow amperometric measurement comparing microgel/tylenol solution with control tylenol samples yielded about 20% tylenol concentration reduction of the microgel sample. Results from the steady state electrochemical experiment confirm the presence of about 20% tylenol concentration drop of the microgel sample compared to control sample at Troom. Using the steady-state experiment with a cyclic temperature ramp from Troom to beyond Tv showed that the tylenol concentration change between the temperature extremes was greater for the microgel solution than for the control solution.

An Ultra-Sensitive Method for the Analysis of Perfluorinated ...

EPA Pesticide Factsheets

In epidemiological research, it has become increasingly important to assess subjects' exposure to different classes of chemicals in multiple environmental media. It is a common practice to aliquot limited volumes of samples into smaller quantities for specific trace level chemical analysis. A novel method was developed for the determination of 14 perfluorinated alkyl acids (PFAAs) in small volumes (10 mL) of drinking water using off-line solid phase extraction (SPE) pre-treatment followed by on-line pre-concentration on WAX column before analysis on column-switching high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). In general, large volumes (100 - 1000 mL) have been used for the analysis of PFAAs in drinking water. The current method requires approximately 10 mL of drinking water concentrated by using an SPE cartridge and eluted with methanol. A large volume injection of the extract was introduced on to a column-switching HPLC-MS/MS using a mix-mode SPE column for the trace level analysis of PFAAs in water. The recoveries for most of the analytes in the fortified laboratory blanks ranged from 73±14% to 128±5%. The lowest concentration minimum reporting levels (LCMRL) for the 14 PFAAs ranged from 0.59 to 3.4 ng/L. The optimized method was applied to a pilot-scale analysis of a subset of drinking water samples from an epidemiological study. These samples were collected directly from the taps in the households of Ohio and Nor

Simultaneous extraction and quantification of lamotrigine, phenobarbital, and phenytoin in human plasma and urine samples using solidified floating organic drop microextraction and high-performance liquid chromatography.

PubMed

Asadi, Mohammad; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Abbasi, Bijan

2015-07-01

A novel and simple method based on solidified floating organic drop microextraction followed by high-performance liquid chromatography with ultraviolet detection has been developed for simultaneous preconcentration and determination of phenobarbital, lamotrigine, and phenytoin in human plasma and urine samples. Factors affecting microextraction efficiency such as the type and volume of the extraction solvent, sample pH, extraction time, stirring rate, extraction temperature, ionic strength, and sample volume were optimized. Under the optimum conditions (i.e. extraction solvent, 1-undecanol (40 μL); sample pH, 8.0; temperature, 25°C; stirring rate, 500 rpm; sample volume, 7 mL; potassium chloride concentration, 5% and extraction time, 50 min), the limits of detection for phenobarbital, lamotrigine, and phenytoin were 1.0, 0.1, and 0.3 μg/L, respectively. Also, the calibration curves for phenobarbital, lamotrigine, and phenytoin were linear in the concentration range of 2.0-300.0, 0.3-200.0, and 1.0-200.0 μg/L, respectively. The relative standard deviations for six replicate extractions and determinations of phenobarbital, lamotrigine, and phenytoin at 50 μg/L level were less than 4.6%. The method was successfully applied to determine phenobarbital, lamotrigine, and phenytoin in plasma and urine samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extraction of citral oil from lemongrass (Cymbopogon Citratus) by steam-water distillation technique

NASA Astrophysics Data System (ADS)

Alam, P. N.; Husin, H.; Asnawi, T. M.; Adisalamun

2018-04-01

In Indonesia, production of citral oil from lemon grass (Cymbopogon Cytratus) is done by a traditional technique whereby a low yield results. To improve the yield, an appropriate extraction technology is required. In this research, a steam-water distillation technique was applied to extract the essential oil from the lemongrass. The effects of sample particle size and bed volume on yield and quality of citral oil produced were investigated. The drying and refining time of 2 hours were used as fixed variables. This research results that minimum citral oil yield of 0.53% was obtained on sample particle size of 3 cm and bed volume of 80%, whereas the maximum yield of 1.95% on sample particle size of 15 cm and bed volume of 40%. The lowest specific gravity of 0.80 and the highest specific gravity of 0.905 were obtained on sample particle size of 8 cm with bed volume of 80% and particle size of 12 cm with bed volume of 70%, respectively. The lowest refractive index of 1.480 and the highest refractive index of 1.495 were obtained on sample particle size of 8 cm with bed volume of 70% and sample particle size of 15 cm with bed volume of 40%, respectively. The solubility of the produced citral oil in alcohol was 70% in ratio of 1:1, and the citral oil concentration obtained was around 79%.

A simple bubbling system for measuring radon (222Rn) gas concentrations in water samples based on the high solubility of radon in olive oil.

PubMed

Al-Azmi, D; Snopek, B; Sayed, A M; Domanski, T

2004-01-01

Based on the different levels of solubility of radon gas in organic solvents and water, a bubbling system has been developed to transfer radon gas, dissolving naturally in water samples, to an organic solvent, i.e. olive oil, which is known to be a good solvent of radon gas. The system features the application of a fixed volume of bubbling air by introducing a fixed volume of water into a flask mounted above the system, to displace an identical volume of air from an air cylinder. Thus a gravitational flow of water is provided without the need for pumping. Then, the flushing air (radon-enriched air) is directed through a vial containing olive oil, to achieve deposition of the radon gas by another bubbling process. Following this, the vial (containing olive oil) is measured by direct use of gamma ray spectrometry, without the need of any chemical or physical processing of the samples. Using a standard solution of 226Ra/222Rn, a lowest measurable concentration (LMC) of radon in water samples of 9.4 Bq L(-1) has been achieved (below the maximum contaminant level of 11 Bq L(-1)).

Direct analysis of δ13C and concentration of dissolved organic carbon (DOC) in environmental samples by TOC-IRMS

NASA Astrophysics Data System (ADS)

Kirkels, Frédérique; Cerli, Chiara; Federherr, Eugen; Kalbitz, Karsten

2014-05-01

Dissolved organic carbon (DOC) plays an important role in carbon cycling in terrestrial and aquatic systems. Stable isotope analysis (delta 13C) of DOC could provide valuable insights in its origin, fluxes and environmental fate. Precise and routine analysis of delta 13C and DOC concentration are therefore highly desirable. A promising, new system has been developed for this purpose, linking a high-temperature combustion TOC analyzer trough an interface with a continuous flow isotope ratio mass spectrometer (Elementar group, Hanau, Germany). This TOC-IRMS system enables simultaneous stable isotope (bulk delta 13C) and concentration analysis of DOC, with high oxidation efficiency by high-temperature combustion for complex mixtures as natural DOC. To give delta 13C analysis by TOC-IRMS the necessary impulse for broad-scale application, we present a detailed evaluation of its analytical performance for realistic and challenging conditions inclusive low DOC concentrations and environmental samples. High precision (standard deviation, SD predominantly < 0.15 permil) and accuracy (R2 = 0.9997, i.e. comparison TOC-IRMS and conventional EA-IRMS) were achieved by TOC-IRMS for a broad diversity of DOC solutions. This precision is comparable or even slightly better than that typically reported for EA-IRMS systems, and improves previous techniques for δ13C analysis of DOC. Simultaneously, very good precision was obtained for DOC concentration measurements. Assessment of natural abundance and slightly 13C enriched DOC, a wide range of concentrations (0.2-150 mgC/L) and injection volumes (0.05-3 ml), demonstrated good analytical performance with negligible memory effects, no concentration/volume effects and a wide linearity. Low DOC concentrations (< 2 mgC/L), were correctly analyzed without any pre-concentration. Moreover, TOC-IRMS was successfully applied to analyze DOC from diverse terrestrial, freshwater and marine environments (SD < 0.23 permil). In summary, the TOC-IRMS performs fast and reliable analysis of DOC concentration and δ13C in aqueous samples, without any pre-concentration/freeze-drying. Flexible usage is highlighted by automated, online analysis, a variable injection volume, high throughput and no extensive maintenance. Sample analysis is simple, using small aliquots and with minimal sample preparation. Further investigations should focus on complex, saline matrices and very low DOC concentrations, to achieve a potential lower limit of 0.2 mgC/L. High-resolution, routine delta 13C analysis of DOC by TOC-IRMS offers opportunities for wide-scale application in terrestrial, freshwater and marine research to elucidate the role of DOC in biogeochemical processes and ecosystem functioning.

DICARBOXYLIC ACID CONCENTRATION TRENDS AND SAMPLING ARTIFACTS

EPA Science Inventory

Dicarboxylic acids associated with airborne particulate matter were measured during a summer period in Philadelphia that included multiple air pollution episodes. Samples were collected for two ten hour periods each day using a high volume sampler with two quartz fiber filters in...

Sediment studies in the Assabet River, central Massachusetts, 2003

USGS Publications Warehouse

Zimmerman, Marc J.; Sorenson, Jason R.

2005-01-01

From its headwaters in Westborough, Massachusetts, to its confluence with the Sudbury River, the 53-kilometer-long Assabet River passes through a series of small towns and mixed land-use areas. Along the way, wastewater-treatment plants release nutrient-rich effluents that contribute to the eutrophic state of this waterway. This condition is most obvious where the river is impounded by a series of dams that have sequestered large amounts of sediment and support rooted and floating macrophytes and epiphytic algae. The water in parts of these impoundments may also have low concentrations of dissolved oxygen, another symptom of eutrophication. All of the impoundments had relatively shallow maximum water depths, which ranged from approximately 2.4 to 3.4 meters, and all had extensive shallow areas. Sediment volumes estimated for the six impoundments ranged from approximately 380 cubic meters in the Aluminum City impoundment to 580,000 cubic meters in the Ben Smith impoundment. The other impoundments had sediment volumes of 120,000 cubic meters (Powdermill), 67,000 cubic meters (Gleasondale), 55,000 cubic meters (Hudson), and 42,000 cubic meters (Allen Street). The principal objective of this study was the determination of sediment volume, extent, and chemistry, in particular, the characterization of toxic inorganic and organic chemicals in the sediments. To determine the bulk-sediment chemical-constituent concentrations, more than one hundred sediment cores were collected in pairs from the six impoundments. One core from each pair was sampled for inorganic constituents and the other for organic constituents. Most of the cores analyzed for inorganics were sectioned to provide information on the vertical distribution of analytes; a subset of the cores analyzed for organics was also sectioned. Approximately 200 samples were analyzed for inorganic constituents and 100 for organics; more than 10 percent were quality-control replicate or blank samples. Maximum bulk-sediment phosphorus concentrations in surface samples from the impoundments increased along a downstream gradient, with the exception of samples from the last impoundment, where the concentrations decreased. In addition, the highest phosphorus concentrations were generally in the surface samples; this finding may prove helpful if surface dredging is selected as a means to control phosphorus release from sediments. There is no known relation, however, between bulk-sediment concentration of phosphorus and the concentrations of phosphorus available to biota. Potentially toxic metals, including arsenic, cadmium, chromium, copper, nickel, lead, and zinc were frequently measured at concentrations that exceeded U.S. Environmental Protection Agency sediment-quality guidelines for the protection of aquatic life and that occasionally exceeded Massachusetts Department of Environmental Protection guidelines governing landfill disposal (reuse). Due to the effects of matrix interference and sample dilution on laboratory analyses, neither pesticides nor volatile organic compounds were detected at any sites. However, samples collected in other studies from nearby streams indicated the possibility that pesticides might have been detected in the impoundments if not for these analytical problems. Although polychlorinated biphenyl concentrations, as individual Aroclors, generally exceeded published U.S. Environmental Protection Agency guideline concentrations for potential effects on aquatic life, the U.S. Environmental Protection Agency guideline concentrations for human contact or the Massachusetts guidelines for landfill reuse were rarely exceeded. Concentrations of polycyclic aromatic hydrocarbons, both individually and total, frequently were greater than guideline concentrations. Concentrations of total extractable petroleum hydrocarbons did not exceed Massachusetts guideline concentrations in any samples. When the sediment analytes from surface samples are considered togethe

Physical-chemical characterization of the textile dye Azo Ab52 degradation by corona plasma

NASA Astrophysics Data System (ADS)

Gómez, A.; Torres-Arenas, A. J.; Vergara-Sánchez, J.; Torres, C.; Reyes, P. G.; Martínez, H.; Saldarriaga-Noreña, Hugo

2017-10-01

This work characterizes the degradation of the textile dye azo Acid Black 52 by measuring several physical and chemical parameters. A corona plasma was created at atmospheric pressure and applied on the liquid-air interface of water samples containing the dye. 1.0 mM of ferrous sulfate (FeSO4) was added to 1.0 mM dye solution, for a total volume of 250 mL. For each treatment, a number of parameters were quantified. These were voltage, current, temperature, loss of volume, pH, electrical conductivity, concentration, optical mission spectra, chemical oxygen demand (COD), total organic carbon (TOC), and the removal ratio. Because of the increase in the sample temperature, the volume lost by evaporation was explored. The results show that the efficiency of the dye degradation by plasma is a function of treatment time. Moreover, the reactive concentration of FeSO4 and the exposition time of the plasma were varied at a constant volume, leading to the determination of the concentrations and optimal times. Considering the degradation and removal parameters, at the maximum treated time of 80 min, it found that COD was of 96.36%, TOC of 93.93%, and the removal ratio of 97.47%.

Challenges in Development of Sperm Repositories for Biomedical Fishes: Quality Control in Small-Bodied Species.

PubMed

Torres, Leticia; Liu, Yue; Guitreau, Amy; Yang, Huiping; Tiersch, Terrence R

2017-12-01

Quality control (QC) is essential for reproducible and efficient functioning of germplasm repositories. However, many biomedical fish models present significant QC challenges due to small body sizes (<5 cm) and miniscule sperm volumes (<5 μL). Using minimal volumes of sperm, we used Zebrafish to evaluate common QC endpoints as surrogates for fertilization success along sequential steps of cryopreservation. First, concentrations of calibration bead suspensions were evaluated with a Makler ® counting chamber by using different sample volumes and mixing methods. For sperm analysis, samples were initially diluted at a 1:30 ratio with Hanks' balanced salt solution (HBSS). Motility was evaluated by using different ratios of sperm and activation medium, and membrane integrity was analyzed with flow cytometry at different concentrations. Concentration and sperm motility could be confidently estimated by using volumes as small as 1 μL, whereas membrane integrity required a minimum of 2 μL (at 1 × 10 6 cells/mL). Thus, <5 μL of sperm suspension (after dilution to 30-150 μL with HBSS) was required to evaluate sperm quality by using three endpoints. Sperm quality assessment using a combination of complementary endpoints enhances QC efforts during cryopreservation, increasing reliability and reproducibility, and reducing waste of time and resources.

Effect of masticatory stimulation on the quantity and quality of saliva and the salivary metabolomic profile

PubMed Central

Hoshi, Noriyuki; Soga, Tomoyoshi; Tomita, Masaru; Sugimoto, Masahiro; Kimoto, Katsuhiko

2017-01-01

Background This study characterized the changes in quality and quantity of saliva, and changes in the salivary metabolomic profile, to understand the effects of masticatory stimulation. Methods Stimulated and unstimulated saliva samples were collected from 55 subjects and salivary hydrophilic metabolites were comprehensively quantified using capillary electrophoresis-time-of-flight mass spectrometry. Results In total, 137 metabolites were identified and quantified. The concentrations of 44 metabolites in stimulated saliva were significantly higher than those in unstimulated saliva. Pathway analysis identified the upregulation of the urea cycle and synthesis and degradation pathways of glycine, serine, cysteine and threonine in stimulated saliva. A principal component analysis revealed that the effect of masticatory stimulation on salivary metabolomic profiles was less dependent on sample population sex, age, and smoking. The concentrations of only 1 metabolite in unstimulated saliva, and of 3 metabolites stimulated saliva, showed significant correlation with salivary secretion volume, indicating that the salivary metabolomic profile and salivary secretion volume were independent factors. Conclusions Masticatory stimulation affected not only salivary secretion volume, but also metabolite concentration patterns. A low correlation between the secretion volume and these patterns supports the conclusion that the salivary metabolomic profile may be a new indicator to characterize masticatory stimulation. PMID:28813487

Accumulation of polycyclic aromatic hydrocarbons by Neocalanus copepods in Port Valdez, Alaska.

PubMed

Carls, Mark G; Short, Jeffrey W; Payne, James

2006-11-01

Sampling zooplankton is a useful strategy for observing trace hydrocarbon concentrations in water because samples represent an integrated average over a considerable effective sampling volume and are more representative of the sampled environment than discretely collected water samples. We demonstrate this method in Port Valdez, Alaska, an approximately 100 km(2) basin that receives about 0.5-2.4 kg of polynuclear aromatic hydrocarbons (PAH) per day. Total PAH (TPAH) concentrations (0.61-1.31 microg/g dry weight), composition, and spatial distributions in a lipid-rich copepod, Neocalanus were consistent with the discharge as the source of contamination. Although Neocalanus acquire PAH from water or suspended particulate matter, total PAH concentrations in these compartments were at or below method detection limits, demonstrating plankton can amplify trace concentrations to detectable levels useful for study.

Ethylene monitoring and control system

NASA Technical Reports Server (NTRS)

Nelson, Bruce N. (Inventor); Kanc, James A. (Inventor); Richard, II, Roy V. (Inventor)

2000-01-01

A system that can accurately monitor and control low concentrations of ethylene gas includes a test chamber configured to receive sample gas potentially containing an ethylene concentration and ozone, a detector configured to receive light produced during a reaction between the ethylene and ozone and to produce signals related thereto, and a computer connected to the detector to process the signals to determine therefrom a value of the concentration of ethylene in the sample gas. The supply for the system can include a four way valve configured to receive pressurized gas at one input and a test chamber. A piston is journaled in the test chamber with a drive end disposed in a drive chamber and a reaction end defining with walls of the test chamber a variable volume reaction chamber. The drive end of the piston is pneumatically connected to two ports of the four way valve to provide motive force to the piston. A manifold is connected to the variable volume reaction chamber, and is configured to receive sample gasses from at least one of a plurality of ports connectable to degreening rooms and to supply the sample gas to the reactive chamber for reaction with ozone. The apparatus can be used to monitor and control the ethylene concentration in multiple degreening rooms.

Ethylene monitoring and control system

NASA Technical Reports Server (NTRS)

Nelson, Bruce N. (Inventor); Kane, James A. (Inventor); Richard, II, Roy V. (Inventor)

2001-01-01

A system that can accurately monitor and control low concentrations of ethylene gas includes a test chamber configured to receive sample gas potentially containing an ethylene concentration and ozone, a detector configured to receive light produced during a reaction between the ethylene and ozone and to produce signals related thereto, and a computer connected to the detector to process the signals to determine therefrom a value of the concentration of ethylene in the sample gas. The supply for the system can include a four way valve configured to receive pressurized gas at one input and a test chamber. A piston is journaled in the test chamber with a drive end disposed in a drive chamber and a reaction end defining with walls of the test chamber a variable volume reaction chamber. The drive end of the piston is pneumatically connected to two ports of the four way valve to provide motive force to the piston. A manifold is connected to the variable volume reaction chamber, and is configured to receive sample gasses from at least one of a plurality of ports connectable to degreening rooms and to supply the sample gas to the reactive chamber for reaction with ozone. The apparatus can be used to monitor and control the ethylene concentration in multiple degreening rooms.

Perilymph composition in scala tympani of the cochlea: influence of cerebrospinal fluid.

PubMed

Hara, A; Salt, A N; Thalmann, R

1989-11-01

A commonly used technique to obtain cochlear perilymph for analysis has been the aspiration of samples through the round window membrane. The present study has investigated the influence of the volume withdrawn on sample composition in the guinea pig. Samples of less than 200 nl in volume taken through the round window showed relatively high glycine content, comparable to the level found in samples taken from scala vestibuli. If larger volumes are withdrawn, lower glycine levels are observed. This is consistent with cerebrospinal fluid (having a low glycine content) being drawn into scala tympani through the cochlear aqueduct and contaminating the sample. The existence of a concentration difference for glycine between scala tympani perilymph and cerebrospinal fluid suggests the physiologic communication across the cochlear aqueduct is relatively small in this species. The observation of considerable exchange between cerebrospinal fluid and perilymph, as reported in some studies, is more likely to be an artifact of the experimental procedures, rather than of physiologic significance. Alternative sampling procedures have been evaluated which allow larger volumes of uncontaminated scala tympani perilymph to be collected.

Comparison of the solid-phase extraction efficiency of a bounded and an included cyclodextrin-silica microporous composite for polycyclic aromatic hydrocarbons determination in water samples.

PubMed

Mauri-Aucejo, Adela; Amorós, Pedro; Moragues, Alaina; Guillem, Carmen; Belenguer-Sapiña, Carolina

2016-08-15

Solid-phase extraction is one of the most important techniques for sample purification and concentration. A wide variety of solid phases have been used for sample preparation over time. In this work, the efficiency of a new kind of solid-phase extraction adsorbent, which is a microporous material made from modified cyclodextrin bounded to a silica network, is evaluated through an analytical method which combines solid-phase extraction with high-performance liquid chromatography to determine polycyclic aromatic hydrocarbons in water samples. Several parameters that affected the analytes recovery, such as the amount of solid phase, the nature and volume of the eluent or the sample volume and concentration influence have been evaluated. The experimental results indicate that the material possesses adsorption ability to the tested polycyclic aromatic hydrocarbons. Under the optimum conditions, the quantification limits of the method were in the range of 0.09-2.4μgL(-1) and fine linear correlations between peak height and concentration were found around 1.3-70μgL(-1). The method has good repeatability and reproducibility, with coefficients of variation under 8%. Due to the concentration results, this material may represent an alternative for trace analysis of polycyclic aromatic hydrocarbons in water trough solid-phase extraction. Copyright © 2016 Elsevier B.V. All rights reserved.

Quantification of protein concentration using UV absorbance and Coomassie dyes.

PubMed

Noble, James E

2014-01-01

The measurement of a solubilized protein concentration in solution is an important assay in biochemistry research and development labs for applications ranging from enzymatic studies to providing data for biopharmaceutical lot release. Spectrophotometric protein quantification assays are methods that use UV and visible spectroscopy to rapidly determine the concentration of protein, relative to a standard, or using an assigned extinction coefficient. Where multiple samples need measurement, and/or the sample volume and concentration is limited, preparations of the Coomassie dye commonly known as the Bradford assay can be used. © 2014 Elsevier Inc. All rights reserved.

Evacuated blood-collection tubes for haematological tests - a quality evaluation prior to their intended use for specimen collection.

PubMed

Gros, Nataša

2013-05-01

An inappropriate anticoagulant concentration in a blood sample can cause cell shrinkage and affect the haematocrit and mean corpuscular volume (MCV). In evacuated blood-collection tubes there are two parameters affecting the quality of the product: the anticoagulant amount introduced into the tube during its production and the internal under-pressure at the instant of the blood-specimen collection affecting the draw-volume. No testing procedures that would give an insight into the anticoagulant concentration that can be expected for blood samples after specimen collection have been available up until now. The methodology suggested here combines the draw-volume test performed with deionised water using a laboratory made measuring device, and a conductivity measurement. The corrections taking into account the air pressure and ambient temperature provide an insight into the anticoagulant concentration that can be expected for blood samples. Results presented in the form of a nomogram facilitate the routine use of the suggested methodology. Our 338-day study confirmed significant differences and variations in the quality and the anticoagulant concentrations of the K₃EDTA and K2EDTA tubes of different producers and identified different examples of non-compliance with the norms during the shelf life of the tubes. The quality evaluation of the evacuated blood-collection tubes prior to their intended use as suggested here can, in everyday laboratory practice, ensure that the tubes are used only if, and only until, their quality is adequate.

Genotyping for DQA1 and PM loci in urine using PCR-based amplification: effects of sample volume, storage temperature, preservatives, and aging on DNA extraction and typing.

PubMed

Vu, N T; Chaturvedi, A K; Canfield, D V

1999-05-31

Urine is often the sample of choice for drug screening in aviation/general forensic toxicology and in workplace drug testing. In some instances, the origin of the submitted samples may be challenged because of the medicolegal and socioeconomic consequences of a positive drug test. Methods for individualization of biological samples have reached a new boundary with the application of the polymerase chain reaction (PCR) in DNA profiling, but a successful characterization of the urine specimens depends on the quantity and quality of DNA present in the samples. Therefore, the present study investigated the influence of storage conditions, sample volume, concentration modes, extraction procedures, and chemical preservations on the quantity of DNA recovered, as well as the success rate of PCR-based genotyping for DQA1 and PM loci in urine. Urine specimens from male and female volunteers were divided and stored at various temperatures for up to 30 days. The results suggested that sample purification by dialfiltration, using 3000-100,000 molecular weight cut-off filters, did not enhance DNA recovery and typing rate as compared with simple centrifugation procedures. Extraction of urinary DNA by the organic method and by the resin method gave comparable typing results. Larger sample volume yielded a higher amount of DNA, but the typing rates were not affected for sample volumes between 1 and 5 ml. The quantifiable amounts of DNA present were found to be greater in female (14-200 ng/ml) than in male (4-60 ng/ml) samples and decreased with the elapsed time under both room temperature (RT) and frozen storage. Typing of the male samples also demonstrated that RT storage samples produced significantly higher success rates than that of frozen samples, while there was only marginal difference in the DNA typing rates among the conditions tested using female samples. Successful assignment of DQA1 + PM genotype was achieved for all samples of fresh urine, independent of gender, starting sample volume, or concentration method. Preservation by 0.25% sodium azide was acceptable for sample storage at 4 degrees C during a period of 30 days. For longer storage duration, freezing at -70 degrees C may be more appropriate. Thus, the applicability of the DQA1 + PM typing was clearly demonstrated for individualization of urine samples.

Reinforcement of acrylic resins for provisional fixed restorations. Part III: effects of addition of titania and zirconia mixtures on some mechanical and physical properties.

PubMed

Panyayong, W; Oshida, Y; Andres, C J; Barco, T M; Brown, D T; Hovijitra, S

2002-01-01

Acrylic resins have been used in many different applications in dentistry, especially in the fabrication of provisional fixed partial dentures. Ideally, a provisional crown and bridge material should be easy to handle and should protect teeth against physical, chemical, and thermal injuries. Some of the problems associated with this use are related to the material's poor mechanical properties. It has been demonstrated that acrylic resin can be strengthened through the addition of structural component of different size distributed in the acrylic matrix, thus forming a composite structure. The purpose of this study was to investigate the addition effects of mixtures of titania (titanium dioxide, TiO(2)) powder and zirconia (zirconium dioxide, ZrO(2)) powder being incorporated with pre-polymerized beads mixed in monomer liquid, on some mechanical and physical properties of PMMA resin. The pre-polymerized powder poly(methyl methacrylate) resin was admixed with titania and zirconia powder. A mixing ratio was controlled by volume % of 0, 1.0, 2.0, and 3.0 (samples with 0 v/o served as control groups). For using mixture of titania and zirconia, total amount of the mixture was controlled by volume % of 1.0, 2.0, and 3.0, in which titania and zirconia were mixed at the ratio 1 :1, 1 :2 and 2 :1. Prior to mechanical tests, all rectangular-shaped samples (25 mm x 2 mm x 5 mm) were stored in 37 degrees C distilled water for 7 days after polishing all six sides of samples. Samples were then subjected to the three-point bending flexion test to evaluate the bending strength as well as the modulus of elasticity. Weight gain and exothermic reaction survey were investigated as well. All data were collected and analyzed with one-way analysis of variance (ANOVA) and Sidak method (p=0.05). It was found that the addition of particles generally decreased the water absorbed by the composite system. Only 1 percent by volume concentration of 1 :1 ratio and 2 percent by volume concentration of 1 :2 and 2 :1 ratios had significantly higher strength than control group. There was significantly higher toughness (in terms of energy-to-break) for 1 percent by volume concentration of 1 :1 ratio and 2 percent by volume concentration of 2 :1 ratio than control group. There was no significant difference between control group and all percent by volume combinations in modulus of elasticity. In addition, there was no significant variations of exothermic reaction.

Monitoring well utility in a heterogeneous DNAPL source zone area: Insights from proximal multilevel sampler wells and sampling capture-zone modelling

NASA Astrophysics Data System (ADS)

McMillan, Lindsay A.; Rivett, Michael O.; Wealthall, Gary P.; Zeeb, Peter; Dumble, Peter

2018-03-01

Groundwater-quality assessment at contaminated sites often involves the use of short-screen (1.5 to 3 m) monitoring wells. However, even over these intervals considerable variation may occur in contaminant concentrations in groundwater adjacent to the well screen. This is especially true in heterogeneous dense non-aqueous phase liquid (DNAPL) source zones, where cm-scale contamination variability may call into question the effectiveness of monitoring wells to deliver representative data. The utility of monitoring wells in such settings is evaluated by reference to high-resolution multilevel sampler (MLS) wells located proximally to short-screen wells, together with sampling capture-zone modelling to explore controls upon well sample provenance and sensitivity to monitoring protocols. Field data are analysed from the highly instrumented SABRE research site that contained an old trichloroethene source zone within a shallow alluvial aquifer at a UK industrial facility. With increased purging, monitoring-well samples tend to a flow-weighted average concentration but may exhibit sensitivity to the implemented protocol and degree of purging. Formation heterogeneity adjacent to the well-screen particularly, alongside pump-intake position and water level, influence this sensitivity. Purging of low volumes is vulnerable to poor reproducibility arising from concentration variability predicted over the initial 1 to 2 screen volumes purged. Marked heterogeneity may also result in limited long-term sample concentration stabilization. Development of bespoke monitoring protocols, that consider screen volumes purged, alongside water-quality indicator parameter stabilization, is recommended to validate and reduce uncertainty when interpreting monitoring-well data within source zone areas. Generalised recommendations on monitoring well based protocols are also developed. A key monitoring well utility is their proportionately greater sample draw from permeable horizons constituting a significant contaminant flux pathway and hence representative fraction of source mass flux. Acquisition of complementary, high-resolution, site monitoring data, however, vitally underpins optimal interpretation of monitoring-well datasets and appropriate advancement of a site conceptual model and remedial implementation.

Direct measurement of surface carbon concentrations. [in lunar soil

NASA Technical Reports Server (NTRS)

Filleux, C.; Tombrello, T. A.; Burnett, D. S.

1977-01-01

Measurements of surface concentrations of carbon in lunar soils and soil breccias provide information on the origin of carbon in the regolith. The reaction C-12 (d, p sub zero) is used to measure 'surface' and 'volume' concentrations in lunar samples. This method has a depth resolution of 1 micron, which permits only a 'surface' and a 'volume' component to be measured. Three of four Apollo 16 double drive tube samples show a surface carbon concentration of about 8 by 10 to the 14th power/sq cm, whereas the fourth sample gave 4 by 10 to the 14th power/sq cm. It can be convincingly shown that the measured concentration does not originate from fluorocarbon or hydrocarbon contaminants. Surface adsorbed layers of CO or CO2 are removed by a sputter cleaning procedure using a 2-MeV F beam. It is shown that the residual C concentration of 8 by 10 to the 14th power/sq cm cannot be further reduced by increased F fluence, and it is therefore concluded that it is truly lunar. If one assumes that the measured surface C concentration is a steady-state concentration determined only by a balance between solar-wind implantation and sputtering, a sputter erosion rate of 0.1 A/yr is obtained. However, it would be more profitable to use an independently derived sputter erosion rate to test the hypothesis of a solar-wind origin of the surface carbon.

Concentration methods for high-resolution THz spectroscopy of nucleic-acid biomolecules and crystals

NASA Astrophysics Data System (ADS)

Brown, E. R.; Zhang, W.; Mendoza, E. A.; Kuznetsova, Y.; Brueck, S. R. J.; Rahman, M.; Norton, M. L.

2012-03-01

Biomolecules can exhibit low-lying vibrational modes in the THz region which are detectable in transmission given a strong molecular dipole moment and optical depth, and a spectrometer of adequate sensitivity. The nucleic acids are particularly interesting because of applications such as label-free gene assay, bio-agent detection, etc. However for nucleic acids, sample preparation and THz coupling are of paramount importance because of the strong absorption by liquid water and the small concentration of molecules present in physiological solutions. Concentration methods become necessary to make the THz vibrational modes detectable, either by concentrating the nucleic-acid sample itself in a small volume but large area, or by concentrating the THz radiation down to the volume of the sample. This paper summarizes one type of the first method: nanofluidic channel arrays for biological nucleic acids; and two types of the second method: (1) a circular-waveguide pinhole, and (2) a circular-waveguide, conical-horn coupling structure, both for DNA crystals. The first method has been demonstrated on a very short artificial nucleic acid [small-interfering (si) RNA (17-to-25 bp)] and a much longer, biological molecule [Lambda-phage DNA (48.5 kbp)]. The second method has been demonstrated on small (~100 micron) single crystals of DNA grown by the sitting-drop method.

Optimization of Evans blue quantitation in limited rat tissue samples

PubMed Central

Wang, Hwai-Lee; Lai, Ted Weita

2014-01-01

Evans blue dye (EBD) is an inert tracer that measures plasma volume in human subjects and vascular permeability in animal models. Quantitation of EBD can be difficult when dye concentration in the sample is limited, such as when extravasated dye is measured in the blood-brain barrier (BBB) intact brain. The procedure described here used a very small volume (30 µl) per sample replicate, which enabled high-throughput measurements of the EBD concentration based on a standard 96-well plate reader. First, ethanol ensured a consistent optic path length in each well and substantially enhanced the sensitivity of EBD fluorescence spectroscopy. Second, trichloroacetic acid (TCA) removed false-positive EBD measurements as a result of biological solutes and partially extracted EBD into the supernatant. Moreover, a 1:2 volume ratio of 50% TCA ([TCA final] = 33.3%) optimally extracted EBD from the rat plasma protein-EBD complex in vitro and in vivo, and 1:2 and 1:3 weight-volume ratios of 50% TCA optimally extracted extravasated EBD from the rat brain and liver, respectively, in vivo. This procedure is particularly useful in the detection of EBD extravasation into the BBB-intact brain, but it can also be applied to detect dye extravasation into tissues where vascular permeability is less limiting. PMID:25300427

Validated low-volume aldosterone immunoassay tailored to GCLP-compliant investigations in small sample volumes.

PubMed

Schaefer, J; Burckhardt, B B; Tins, J; Bartel, A; Laeer, S

2017-12-01

Heart failure is well investigated in adults, but data in children is lacking. To overcome this shortage of reliable data, appropriate bioanalytical assays are required. Development and validation of a bioanalytical assay for the determination of aldosterone concentrations in small sample volumes applicable to clinical studies under Good Clinical Laboratory Practice. An immunoassay was developed based on a commercially available enzyme-linked immunosorbent assay and validated according to current bioanalytical guidelines of the EMA and FDA. The assay (range 31.3-1000 pg/mL [86.9-2775 pmol/L]) is characterized by a between-run accuracy from - 3.8% to - 0.8% and a between-run imprecision ranging from 4.9% to 8.9% (coefficient of variation). For within-run accuracy, the relative error was between - 11.1% and + 9.0%, while within-run imprecision ranged from 1.2% to 11.8% (CV). For parallelism and dilutional linearity, the relative error of back-calculated concentrations varied from - 14.1% to + 8.4% and from - 7.4% to + 10.5%, respectively. The immunoassay is compliant with the bioanalytical guidelines of the EMA and FDA and allows accurate and precise aldosterone determinations. As the assay can run low-volume samples, it is especially valuable for pediatric investigations.

Optimization of Evans blue quantitation in limited rat tissue samples

NASA Astrophysics Data System (ADS)

Wang, Hwai-Lee; Lai, Ted Weita

2014-10-01

Evans blue dye (EBD) is an inert tracer that measures plasma volume in human subjects and vascular permeability in animal models. Quantitation of EBD can be difficult when dye concentration in the sample is limited, such as when extravasated dye is measured in the blood-brain barrier (BBB) intact brain. The procedure described here used a very small volume (30 µl) per sample replicate, which enabled high-throughput measurements of the EBD concentration based on a standard 96-well plate reader. First, ethanol ensured a consistent optic path length in each well and substantially enhanced the sensitivity of EBD fluorescence spectroscopy. Second, trichloroacetic acid (TCA) removed false-positive EBD measurements as a result of biological solutes and partially extracted EBD into the supernatant. Moreover, a 1:2 volume ratio of 50% TCA ([TCA final] = 33.3%) optimally extracted EBD from the rat plasma protein-EBD complex in vitro and in vivo, and 1:2 and 1:3 weight-volume ratios of 50% TCA optimally extracted extravasated EBD from the rat brain and liver, respectively, in vivo. This procedure is particularly useful in the detection of EBD extravasation into the BBB-intact brain, but it can also be applied to detect dye extravasation into tissues where vascular permeability is less limiting.

Accurate mass replacement method for the sediment concentration measurement with a constant volume container

NASA Astrophysics Data System (ADS)

Ban, Yunyun; Chen, Tianqin; Yan, Jun; Lei, Tingwu

2017-04-01

The measurement of sediment concentration in water is of great importance in soil erosion research and soil and water loss monitoring systems. The traditional weighing method has long been the foundation of all the other measuring methods and instrument calibration. The development of a new method to replace the traditional oven-drying method is of interest in research and practice for the quick and efficient measurement of sediment concentration, especially field measurements. A new method is advanced in this study for accurately measuring the sediment concentration based on the accurate measurement of the mass of the sediment-water mixture in the confined constant volume container (CVC). A sediment-laden water sample is put into the CVC to determine its mass before the CVC is filled with water and weighed again for the total mass of the water and sediments in the container. The known volume of the CVC, the mass of sediment-laden water, and sediment particle density are used to calculate the mass of water, which is replaced by sediments, therefore sediment concentration of the sample is calculated. The influence of water temperature was corrected by measuring water density to determine the temperature of water before measurements were conducted. The CVC was used to eliminate the surface tension effect so as to obtain the accurate volume of water and sediment mixture. Experimental results showed that the method was capable of measuring the sediment concentration from 0.5 up to 1200 kg m-3. A good liner relationship existed between the designed and measured sediment concentrations with all the coefficients of determination greater than 0.999 and the averaged relative error less than 0.2%. All of these seem to indicate that the new method is capable of measuring a full range of sediment concentration above 0.5 kg m-3 to replace the traditional oven-drying method as a standard method for evaluating and calibrating other methods.

Isolation of 236U and 239,240Pu from seawater samples and its determination by Accelerator Mass Spectrometry.

PubMed

López-Lora, Mercedes; Chamizo, Elena; Villa-Alfageme, María; Hurtado-Bermúdez, Santiago; Casacuberta, Núria; García-León, Manuel

2018-02-01

In this work we present and evaluate a radiochemical procedure optimised for the analysis of 236 U and 239,240 Pu in seawater samples by Accelerator Mass Spectrometry (AMS). The method is based on Fe(OH) 3 co-precipitation of actinides and uses TEVA® and UTEVA® extraction chromatography resins in a simplified way for the final U and Pu purification. In order to improve the performance of the method, the radiochemical yields are analysed in 1 to 10L seawater volumes using alpha spectrometry (AS) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Robust 80% plutonium recoveries are obtained; however, it is found that Fe(III) concentration in the precipitation solution and sample volume are the two critical and correlated parameters influencing the initial uranium extraction through Fe(OH) 3 co-precipitation. Therefore, we propose an expression that optimises the sample volume and Fe(III) amounts according to both the 236 U and 239,240 Pu concentrations in the samples and the performance parameters of the AMS facility. The method is validated for the current setup of the 1MV AMS system (CNA, Sevilla, Spain), where He gas is used as a stripper, by analysing a set of intercomparison seawater samples, together with the Laboratory of Ion Beam Physics (ETH, Zürich, Switzerland). Copyright © 2017 Elsevier B.V. All rights reserved.

An ultra-sensitive method for the analysis of perfluorinated alkyl acids in drinking water using a column switching high-performance liquid chromatography tandem mass spectrometry.

PubMed

Dasu, Kavitha; Nakayama, Shoji F; Yoshikane, Mitsuha; Mills, Marc A; Wright, J Michael; Ehrlich, Shelley

2017-04-21

In epidemiological research, it has become increasingly important to assess subjects' exposure to different classes of chemicals in multiple environmental media. It is a common practice to aliquot limited volumes of samples into smaller quantities for specific trace level chemical analyses. A novel method was developed for the determination of 14 perfluorinated alkyl acids (PFAAs) in small volumes (10mL) of drinking water using off-line solid phase extraction (SPE) pre-treatment followed by on-line pre-concentration on a WAX column before analysis on column-switching high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). In general, large volumes (100-1000mL) have been used for the analysis of PFAAs in drinking water. The current method requires approximately 10mL of drinking water concentrated by using an SPE cartridge and eluted with methanol. A large volume injection of the extract was introduced on to a column-switching HPLC-MS/MS using a mix-mode SPE column for the trace level analysis of PFAAs in water. The recoveries for most of the analytes in the fortified laboratory blanks ranged from 73±14% to 128±5%. The lowest concentration minimum reporting levels (LCMRL) for the 14 PFAAs ranged from 0.59 to 3.4ng/L. The optimized method was applied to a pilot-scale analysis of a subset of drinking water samples from an epidemiological study. These samples were collected directly from the taps in the households of Ohio and Northern Kentucky, United States and the sources of drinking water samples are both surface water and ground water, and supplied by different water distribution facilities. Only five PFAAs, perfluoro-1-butanesulfonic acid (PFBS), perfluoro-1- -hexanesulfonic acid (PFHxS), perfluoro-1-octanesulfonic acid (PFOS), perfluoro-n-heptanoic acid (PFHpA) and perfluoro-n-octanoic acid (PFOA) are detected above the LCMRL values. The median concentrations of these five PFAAs detected in the samples was ≤4.1ng/L with PFOS at 7.6ng/L and PFOA at 10ng/L. Concentrations of perfluoro-1-decanesulfonic acid, PFDS and other perfluoroalkyl carboxylic acids were below the LCMRL values. Copyright © 2017 Elsevier B.V. All rights reserved.

Simple hollow fiber renewal liquid membrane extraction method for pre-concentration of Cd(II) in environmental samples and detection by flame atomic absorption spectrometry.

PubMed

Carletto, Jeferson Schneider; Luciano, Raquel Medeiros; Bedendo, Gizelle Cristina; Carasek, Eduardo

2009-04-06

A hollow fiber renewal liquid membrane (HFRLM) extraction method to determine cadmium (II) in water samples using Flame Atomic Absorption Spectrometry (FAAS) was developed. Ammonium O,O-diethyl dithiophosphate (DDTP) was used to complex cadmium (II) in an acid medium to obtain a neutral hydrophobic complex (ML(2)). The organic solvent introduced to the sample extracts this complex from the aqueous solution and carries it over the poly(dimethylsiloxane) (PDMS) membrane, that had their walls previously filled with the same organic solvent. The organic solvent is solubilized inside the PDMS membrane, leading to a homogeneous phase. The complex strips the lumen of the membrane where, at higher pH, the complex Cd-DDTP is broken down and cadmium (II) is released into the stripping phase. EDTA was used to complex the cadmium (II), helping to trap the analyte in the stripping phase. A multivariate procedure was used to optimize the studied variables. The optimized variables were: sample (donor phase) pH 3.25, DDTP concentration 0.05% (m/v), stripping (acceptor phase) pH 8.75, EDTA concentration 1.5x10(-2) mol L(-1), extraction temperature 40 degrees C, extraction time 40 min, a solvent mixture N-butyl acetate and hexane (60/40%, v/v) with a volume of 100 microL, and addition of ammonium sulfate to saturate the sample. The sample volume used was 20 mL and the stripping volume was 165 microL. The analyte enrichment factor was 120, limit of detection (LOD) 1.3 microg L(-1), relative standard deviation (RSD) 5.5% and the working linear range 2-30 microg L(-1).

[Relationship between atmospheric particles and rain water chemistry character].

PubMed

Huo, Ming-Qun; Sun, Qian; Xie, Peng; Bai, Yu-Hua; Liu, Zhao-Rong; Li, Ji-Long; Lu, Si-Hua

2009-11-01

Rain and atmospheric particle samples were collected in the rural area of Taian and Shenzhen in 2007, respectively. Rain sampling was carried out during the precipitation process and several samples were got from the beginning of one precipitation to the end. The chemical character changes during precipitation and the changes of concentration of particles before and after rain were studied in this research to understand the contribution of particles on the rain chemical character and the rain-out effect for particles. The volume-weighted mean pH of rainwater in Taian was 5.97 and the total concentration of ions was 1 187.96 microeq x L(-1). The mass concentration of PM10 in Taian was 131.76 microg/m3 and that of PM2.5 was 103.84 microg/m3. The volume-weighted mean pH of rainwater in Shenzhen was 4.72 and the total concentration of ions was 175.89 microeq x L(-1). The mass concentration of PM10 in Shenzhen was 56.66 microg/m3 and that of PM2.5 was 41.52 microg/m3. During precipitation process pH and ion concentration of rain decrease and it is shown the neutralizing effect happens. The difference between rainwater of Taian and Shenzhen is due to cloud water acidity, atmospheric particles character and atmospheric acid-basic gases concentration. The clean-up effect of Na+ and Ca2+ by rain is high and which of NH4+ and NO3- is low. The clean-up effect for mass concentration, ions concentration and element concentration of particles by rain are significant.

Reconfirmation of frit 803 based on the January 2016 sludge batch 9 reprojection

DOE Office of Scientific and Technical Information (OSTI.GOV)

Johnson, F.; Edwards, T.

2016-02-10

On January 11, 2016, Savannah River Remediation (SRR) provided the Savannah River National Laboratory (SRNL) with a Sludge Batch 9 (SB9) reprojection that was developed from the analyzed composition of a Tank 51 sample. This sample was collected after field washing had been completed in Tank 51 to support the alternate reductant task. Based on this reprojection, Frit 803 is still a viable option for the processing of SB9 under sludge-only operations and coupled (Actinide Removal Process (ARP) product with and without monosodium titanate (MST)) operations. The maximum projected volumes of ARP product that can be transferred from the Precipitatemore » Reactor Feed Tank (PRFT) per Sludge Receipt and Adjustment Tank (SRAT) batch and the resulting Na 2O concentrations in the SRAT for coupled operations were determined. The Na 2O concentrations in the SRAT resulting from the maximum projected ARP product transfer volumes are consistent with those from the previous assessments that were based on the August 2015 projections. Regardless of the presence or absence of MST in the ARP product, the contribution of Na 2O to the resulting glass will be similar at the same waste loading (WL). These projected volumes of ARP product are not anticipated to be an issue for SB9. The actual transfer volumes from the PRFT to the SRAT are determined based upon the analyzed Na 2O concentrations in the PRFT samples, which has resulted in larger transfer volumes than those allowed by the projections for Sludge Batch 8 (SB8). An operating window of 32-40% WL around the nominal WL of 36% is achievable for both sludge-only and coupled operations; however, each of the glass systems studied does become limited by waste form affecting constraints (durability) at higher volumes of ARP product and WLs of 41-42%.« less

Preparation of immunoglobulin Y from egg yolk using ammonium sulfate precipitation and ion exchange chromatography.

PubMed

Ko, K Y; Ahn, D U

2007-02-01

The objective of this study was to develop an economical, simple, and large-scale separation method for IgY from egg yolk. Egg yolk diluted with 9 volumes of cold water was centrifuged after adjusting the pH to 5.0. The supernatant was added with 0.01% charcoal or 0.01% carrageenan and centrifuged at 2,800 x g for 30 min. The supernatant was filtered through a Whatman no. 1 filter paper and then the filtrate was concentrated to 20% original volume using ultrafiltration. The concentrated solution was further purified using either cation exchange chromatography or ammonium sulfate precipitation. For the cation exchange chromatography method, the concentrated sample was loaded onto a column equilibrated with 20 mM citrate-phosphate buffer at pH 4.8 and eluted with 200 mM citrate-phosphate buffer at pH 6.4. For the ammonium sulfate precipitation method, the concentrated sample was twice precipitated with 40% ammonium sulfate solution at pH 9.0. The yield and purity of IgY were determined by ELISA and electrophoresis. The yield of IgY from the cation exchange chromatography method was 30 to 40%, whereas that of the ammonium sulfate precipitation was 70 to 80%. The purity of IgY from the ammonium sulfate method was higher than that of the cation exchange chromatography. The cation exchange chromatography could handle only a small amount of samples, whereas the ammonium sulfate precipitation could handle a large volume of samples. This suggests that ammonium sulfate precipitation was a more efficient and useful purification method than cation exchange chromatography for the large-scale preparation of IgY from egg yolk.

Modified electrokinetic sample injection method in chromatography and electrophoresis analysis

DOEpatents

Davidson, J. Courtney; Balch, Joseph W.

2001-01-01

A sample injection method for horizontal configured multiple chromatography or electrophoresis units, each containing a number of separation/analysis channels, that enables efficient introduction of analyte samples. This method for loading when taken in conjunction with horizontal microchannels allows much reduced sample volumes and a means of sample stacking to greatly reduce the concentration of the sample. This reduction in the amount of sample can lead to great cost savings in sample preparation, particularly in massively parallel applications such as DNA sequencing. The essence of this method is in preparation of the input of the separation channel, the physical sample introduction, and subsequent removal of excess material. By this method, sample volumes of 100 nanoliter to 2 microliters have been used successfully, compared to the typical 5 microliters of sample required by the prior separation/analysis method.

Rheological and Magnetorheological Behaviour of Some Magnetic Fluids on Polar and Nonpolar Carrier Liquids

NASA Astrophysics Data System (ADS)

Bălău, Oana; Bica, Doina; Koneracka, Martina; Kopčansky, Peter; Susan-Resiga, Daniela; Vékás, Ladislau

Rheological and magnetorheological behaviour of monolayer and double layer sterically stabilized magnetic fluids, with transformer oil (UTR), diloctilsebacate (DOS), heptanol (Hept), pentanol (Pent) and water (W) as carrier liquids, were investigated. The data for volumic concentration dependence of dynamic viscosity of high colloidal stability UTR, DOS, Hept and Pent samples are particularly well fitted by the formulas given by Vand (1948) and Chow (1994). The Chow type dependence proved its universal character as the viscosity data for dilution series of various magnetic fluids are well fitted by the same curve, regardless the nonpolar or polar charcater of the sample. The magnetorheological effect measured for low and medium concentration water based magnetic fluids is much higher, due to agglomerate formation process, than the corresponding values obtained for the well stabilized UTR, DOS, Hept and Pent samples, even at very high volumic fraction of magnetic nanoparticles.

Positron annihilation and X-ray diffraction studies on tin oxide thin films

NASA Astrophysics Data System (ADS)

Prabakar, K.; Abhaya, S.; Krishnan, R.; Kalavathi, S.; Dash, S.; Jayapandian, J.; Amarendra, G.

2009-04-01

Positron annihilation spectroscopy along with glancing incidence X-ray diffraction have been used to investigate tin oxide thin films grown on Si by pulsed laser deposition. The films were prepared at room temperature and at 670 K under oxygen partial pressure. As-grown samples are amorphous and are found to contain large concentration of open volume sites (vacancy defects). Post-deposition annealing of as-grown samples at 970 K is found to drastically reduce the number of open volume sites and the film becomes crystalline. However, film grown under elevated temperature and under partial pressure of oxygen is found to exhibit a lower S-parameter, indicating lower defect concentration. Based on the analysis of experimental positron annihilation results, the defect-sensitive S-parameter and the overlayer thickness of tin oxide thin films are deduced. S- W correlation plots exhibit distinct positron trapping defect states in three samples.

Quality of stormwater runoff discharged from Massachusetts highways, 2005-07

USGS Publications Warehouse

Smith, Kirk P.; Granato, Gregory E.

2010-01-01

The U.S. Geological Survey (USGS), in cooperation with U.S. Department of Transportation Federal Highway Administration and the Massachusetts Department of Transportation, conducted a field study from September 2005 through September 2007 to characterize the quality of highway runoff for a wide range of constituents. The highways studied had annual average daily traffic (AADT) volumes from about 3,000 to more than 190,000 vehicles per day. Highway-monitoring stations were installed at 12 locations in Massachusetts on 8 highways. The 12 monitoring stations were subdivided into 4 primary, 4 secondary, and 4 test stations. Each site contained a 100-percent impervious drainage area that included two or more catch basins sharing a common outflow pipe. Paired primary and secondary stations were located within a few miles of each other on a limited-access section of the same highway. Most of the data were collected at the primary and secondary stations, which were located on four principal highways (Route 119, Route 2, Interstate 495, and Interstate 95). The secondary stations were operated simultaneously with the primary stations for at least a year. Data from the four test stations (Route 8, Interstate 195, Interstate 190, and Interstate 93) were used to determine the transferability of the data collected from the principal highways to other highways characterized by different construction techniques, land use, and geography. Automatic-monitoring techniques were used to collect composite samples of highway runoff and make continuous measurements of several physical characteristics. Flowweighted samples of highway runoff were collected automatically during approximately 140 rain and mixed rain, sleet, and snowstorms. These samples were analyzed for physical characteristics and concentrations of 6 dissolved major ions, total nutrients, 8 total-recoverable metals, suspended sediment, and 85 semivolatile organic compounds (SVOCs), which include priority polyaromatic hydrocarbons (PAHs), phthalate esters, and other anthropogenic or naturally occurring organic compounds. The distribution of particle size of suspended sediment also was determined for composite samples of highway runoff. Samples of highway runoff were collected year round and under various dry antecedent conditions throughout the 2-year sampling period. In addition to samples of highway runoff, supplemental samples also were collected of sediment in highway runoff, background soils, berm materials, maintenance sands, deicing compounds, and vegetation matter. These additional samples were collected near or on the highways to support data analysis. There were few statistically significant differences between populations of constituent concentrations in samples from the primary and secondary stations on the same principal highways (Mann-Whitney test, 95-percent confidence level). Similarly, there were few statistically significant differences between populations of constituent concentrations for the four principal highways (data from the paired primary and secondary stations for each principal highway) and populations for test stations with similar AADT volumes. Exceptions to this include several total-recoverable metals for stations on Route 2 and Interstate 195 (highways with moderate AADT volumes), and for stations on Interstate 95 and Interstate 93 (highways with high AADT volumes). Supplemental data collected during this study indicate that many of these differences may be explained by the quantity, as well as the quality, of the sediment in samples of highway runoff. Nonparametric statistical methods also were used to test for differences between populations of sample constituent concentrations among the four principal highways that differed mainly in traffic volume. These results indicate that there were few statistically significant differences (Mann-Whitney test, 95-percent confidence level) for populations of concentrations of most total-recoverable metals

40 CFR 60.285a - Test methods and procedures.

Code of Federal Regulations, 2014 CFR

2014-07-01

... performance test. (b) The owner or operator must determine compliance with the filterable particulate matter... used to determine the filterable particulate matter concentration. The sampling time and sample volume... repeat performance tests for filterable particulate matter at intervals no longer than 5 years following...

High-throughput, automated extraction of DNA and RNA from clinical samples using TruTip technology on common liquid handling robots.

PubMed

Holmberg, Rebecca C; Gindlesperger, Alissa; Stokes, Tinsley; Brady, Dane; Thakore, Nitu; Belgrader, Philip; Cooney, Christopher G; Chandler, Darrell P

2013-06-11

TruTip is a simple nucleic acid extraction technology whereby a porous, monolithic binding matrix is inserted into a pipette tip. The geometry of the monolith can be adapted for specific pipette tips ranging in volume from 1.0 to 5.0 ml. The large porosity of the monolith enables viscous or complex samples to readily pass through it with minimal fluidic backpressure. Bi-directional flow maximizes residence time between the monolith and sample, and enables large sample volumes to be processed within a single TruTip. The fundamental steps, irrespective of sample volume or TruTip geometry, include cell lysis, nucleic acid binding to the inner pores of the TruTip monolith, washing away unbound sample components and lysis buffers, and eluting purified and concentrated nucleic acids into an appropriate buffer. The attributes and adaptability of TruTip are demonstrated in three automated clinical sample processing protocols using an Eppendorf epMotion 5070, Hamilton STAR and STARplus liquid handling robots, including RNA isolation from nasopharyngeal aspirate, genomic DNA isolation from whole blood, and fetal DNA extraction and enrichment from large volumes of maternal plasma (respectively).

Fused silica capillaries with two segments of different internal diameters and inner surface roughnesses prepared by etching with supercritical water and used for volume coupling electrophoresis.

PubMed

Horká, Marie; Karásek, Pavel; Roth, Michal; Šlais, Karel

2017-05-01

In this work, single-piece fused silica capillaries with two different internal diameter segments featuring different inner surface roughness were prepared by new etching technology with supercritical water and used for volume coupling electrophoresis. The concept of separation and online pre-concentration of analytes in high conductivity matrix is based on the online large-volume sample pre-concentration by the combination of transient isotachophoretic stacking and sweeping of charged proteins in micellar electrokinetic chromatography using non-ionogenic surfactant. The modified surface roughness step helped to the significant narrowing of the zones of examined analytes. The sweeping and separating steps were accomplished simultaneously by the use of phosphate buffer (pH 7) containing ethanol, non-ionogenic surfactant Brij 35, and polyethylene glycol (PEG 10000) after sample injection. Sample solution of a large volume (maximum 3.7 μL) dissolved in physiological saline solution was injected into the wider end of capillary with inlet inner diameter from 150, 185 or 218 μm. The calibration plots were linear (R 2 ∼ 0.9993) over a 0.060-1 μg/mL range for the proteins used, albumin and cytochrome c. The peak area RSDs from at least 20 independent measuremens were below 3.2%. This online pre-concentration technique produced a more than 196-fold increase in sensitivity, and it can be applied for detection of, e.g. the presence of albumin in urine (0.060 μg/mL). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Integrated chemical/biochemical sample collection, pre-concentration, and analysis on a digital microfluidic lab-on-a-chip platform

NASA Astrophysics Data System (ADS)

Fair, Richard B.; Khlystov, A.; Srinivasan, Vijay; Pamula, Vamsee K.; Weaver, Kathryn N.

2004-12-01

An ideal on-site chemical/biochemical analysis system must be inexpensive, sensitive, fully automated and integrated, reliable, and compatible with a broad range of samples. The advent of digital microfluidic lab-on-a-chip (LoC) technology offers such a detection system due to the advantages in portability, reduction of the volumes of the sample and reagents, faster analysis times, increased automation, low power consumption, compatibility with mass manufacturing, and high throughput. We describe progress towards integrating sample collection onto a digital microfluidic LoC that is a component of a cascade impactor device. The sample collection is performed by impacting airborne particles directly onto the surface of the chip. After the collection phase, the surface of the chip is washed with a micro-droplet of solvent. The droplet will be digitally directed across the impaction surface, dissolving sample constituents. Because of the very small droplet volume used for extraction of the sample from a wide colection area, the resulting solution is realatively concentrated and the analytes can be detected after a very short sampling time (1 min) due to such pre-concentration. After the washing phase, the droplet is mixed with specific reagents that produce colored reaction products. The concentration of the analyte is quantitatively determined by measuring absorption at target wavelengths using a simple light emitting diode and photodiode setup. Specific applications include automatic measurements of major inorganic ions in aerosols, such as sulfate, nitrate and ammonium, with a time resolution of 1 min and a detection limit of 30 nm/m3. We have already demonstrated the detection and quantification of nitroaromatic explosives without integrating the sample collection. Other applications being developed include airborne bioagent detection.

Using the fundamentals of adsorption to understand peak distortion due to strong solvent effect in hydrophilic interaction chromatography.

PubMed

Gritti, Fabrice; Sehajpal, Jyotsna; Fairchild, Jacob

2017-03-17

The peak distortion observed in hydrophilic interaction chromatography (HILIC) may be caused by the sample diluent to mobile phase mismatch. The United States Pharmacopeia (USP) method for organic impurities in cetirizine HCl tablets calls for such a mismatch, having a higher concentration of strong solvent in the sample diluent than in the mobile phase. A significant peak deformation is reported for cetirizine (a second-generation antihistamine) when it is purified on a Ethylene Bridged Hybrid (BEH) HILIC column (4.6mm×100mm, 2.5μm particles) using an acetonitrile-water eluent mixture and a sample diluent containing 7% and 9% water (in volume), respectively. The mechanism and physical origin of such peak distortion are related to (1) the diluent-to-eluent excess of water that propagates along the column at a velocity similar to that of the analyte, (2) the significant drop of the Henry's constant of the analyte upon increasing water concentration in the eluent, (3) the sample volume injected, and (4) to the pre-column sample dilution factor that depends on the characteristics of the LC instrument used. This proposed mechanism is validated from the calculation of the concentration profiles of cetirizine and water by using the equilibrium-dispersive (ED) model of chromatography. The observed distortion of cetirizine peaks is successfully predicted from the measurement of (1) the excess adsorption isotherm of water from acetonitrile onto the BEH HILIC adsorbent, (2) the retention factor of cetirizine as a function of the volume fraction (7, 8, and 9%) of water in the mobile phase, and (3) of the pre-column sample dispersion related to the instrument used (HPLC or UHPLC). The results of the calculations enables the user to anticipate the impacts of the diluent-to-eluent mismatch in water content, the injection volume, the analyte retention under infinite dilution, and of the pre-column sample dispersion on the amplitude of peak distortion in HILIC. Appropriate and permitted alterations of the USP method are then suggested based on a sound physico-chemical approach. Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of environmental levels of aromatic hydrocarbons in gasoline service stations by gas chromatography.

PubMed

Periago, J F; Zambudio, A; Prado, C

1997-08-22

The volume of gasoline sold in refuelling operations and the ambient temperature, can increase significantly the environmental levels of aromatic hydrocarbon vapours and subsequently, the occupational risk of gasoline service station attendants, specially in the case of benzene. We have evaluated the occupational exposure to aromatic hydrocarbons by means of personal-breathing-zone samples of gasoline vapours in a service station attendant population. This evaluation was carried out using diffusive samplers, in two periods at quite different temperatures (March and July). A significant relationship between the volume of gasoline sold during the shift and the ambient concentration of benzene, toluene, and xylenes was found for each worker sampled. Furthermore a significant difference was found between the time-weighted average concentration of aromatic compounds measured in March, with ambient temperatures of 14-15 degrees C and July, with temperatures of 28-30 degrees C. In addition, 20% of the population sampled in the last period were exposed to a time-weighted average concentration of benzene above the proposed Threshold Limit Value of 960 micrograms/m(3) of the American Conference of Governmental Industrial Hygienists (ACGIH).

Method of high-precision microsampled blood and plasma mass densitometry

NASA Technical Reports Server (NTRS)

Hinghofer-Szalkay, H.

1986-01-01

The reliability of the mechanical oscillator technique for blood and plasma density measurements on samples of volumes less than 0.1 ml is examined, and a precision of 0.001 g/l is found if plasma-isodensic heparin solution and siliconized densitometers are employed. Sources of measurement errors in the density determinations include storage of plasma samples, inhomogeneity of blood samples, and density reading before adequate temperature equilibration. In tests of plasma sample storage, the best reproducibility was obtained with samples kept at 4 C. Linear correlations were found between plasma density and plasma protein concentration, blood density and blood hemoglobin concentration, and erythrocyte density and MCHC.

Electrolyte and plasma changes after ingestion of pickle juice, water, and a common carbohydrate-electrolyte solution.

PubMed

Miller, Kevin C; Mack, Gary; Knight, Kenneth L

2009-01-01

Health care professionals advocate that athletes who are susceptible to exercise-associated muscle cramps (EAMCs) should moderately increase their fluid and electrolyte intake by drinking sport drinks. Some clinicians have also claimed drinking small volumes of pickle juice effectively relieves acute EAMCs, often alleviating them within 35 seconds. Others fear ingesting pickle juice will enhance dehydration-induced hypertonicity, thereby prolonging dehydration. To determine if ingesting small quantities of pickle juice, a carbohydrate-electrolyte (CHO-e) drink, or water increases plasma electrolytes or other selected plasma variables. Crossover study. Exercise physiology laboratory. Nine euhydrated, healthy men (age = 25 +/- 2 years, height = 179.4 +/- 7.2 cm, mass = 86.3 +/- 15.9 kg) completed the study. Resting blood samples were collected preingestion (-0.5 minutes); immediately postingestion (0 minutes); and at 1, 5, 10, 15, 20, 25, 30, 45, and 60 minutes postingestion of 1 mL/kg body mass of pickle juice, CHO-e drink, or tap water. Plasma sodium concentration, plasma magnesium concentration, plasma calcium concentration, plasma potassium concentration, plasma osmolality, and changes in plasma volume were analyzed. Urine specific gravity, osmolality, and volume were also measured to characterize hydration status. Mean fluid intake was 86.3 +/- 16.7 mL. Plasma sodium concentration, plasma magnesium concentration, plasma calcium concentration, plasma osmolality, and plasma volume did not change during the 60 minutes after ingestion of each fluid (P >or= .05). Water ingestion slightly decreased plasma potassium concentration at 60 minutes (0.21 +/- 0.14 mg/dL [0.21 +/- 0.14 mmol/L]; P

Installation Restoration Program (IRP). Aircraft Parking Apron Area. Volume 1. 152nd Reconnaissance Group, Nevada Air National Guard, Reno-Cannon International Airport, Reno, Nevada

DTIC Science & Technology

1994-06-01

Loeltz, 1964, Evaluation of Hydroeeology and Hydrochemistry of the Truckee Meadow Area. Washoe County. Nevada. U. S. Geological Survey, Water I Supply...was detected in water samples collected from all monitoring wells. A concentration of I 0.055 ppm for the water sample collected from monitoring well...MWO8 during the first round of sampling (MW08-(1)), exceeded the federal drinking water standard of 0.05 ppm. The I background concentration for lead

Distribution of selected volatile organic compounds determined with water-to-vapor diffusion samplers at the interface between ground water and surface water, Centredale Manor site, North Providence, Rhode Island, September 1999

USGS Publications Warehouse

Church, Peter E.; Lyford, Forest P.; Clifford, Scott

2000-01-01

Volatile organic compounds are present in soils and ground water at the Centredale Manor Superfund Site in North Providence, Rhode Island. In September 1999, water-to-vapor diffusion samplers were placed in the bottom sediments of waterways adjacent to the site to identify possible contaminated ground-water discharge areas. The approximate12-acre site is a narrow stretch of land between the eastern bank of the Woonasquatucket River, downstream from the U.S. Route 44 bridge and a former mill raceway. The samplers were placed along a 2,250-foot reach of the Woonasquatucket River, in the former mill raceway several hundred feet to the east and parallel to the river, and in a cross channel between the river and former mill raceway. Volatile organic compounds were detected in 84 of the 104 water-to-vapor diffusion samplers retrieved. Trichloroethylene and tetrachloro-ethylene were the principal volatile organic compounds detected. The highest vapor concentrations measured for these two chemicals were from diffusion samplers located along an approximate 100-foot reach of the Woonasquatucket River about 500 feet downstream of the bridge; here trichloroethylene and tetrachloroethylene vapor concentrations ranged from about 2,000 to 180,000 and 1,600 to 1,400,000 parts per billion by volume, respectively. Upstream and downstream from this reach and along the former mill raceway, trichloroethylene and tetrachloroethylene vapor concentrations from the diffusion samples were generally less than 100 parts per billion by volume. Along the lower reaches of the river and mill raceway, however, and in the cross channel, vapor concentrations of trichloroethylene exceeded 100 parts per billion by volume and tetrachloroethylene exceeded 1,000 parts per billion by volume in several diffusion samples. Although diffusion sample vapor concentrations are higher than water concentrations in surface waters and in ground water, and they should only be interpreted qualitatively as relative values, these values provide important information as to potential discharge areas of contaminants.

Unique Structural Modifications Are Present in the Lipopolysaccharide from Colistin-Resistant Strains of Acinetobacter baumannii

DTIC Science & Technology

2013-10-01

13). Freeze-dried bacteria were resuspended in endotoxin -free water at a concentration of 10 mg/ml. A 12.5-ml volume of 90% phenol was added, and the...temperature for 30 min. The aqueous phase was collected, and an equal volume of endotoxin -free water was added to the organic phase. The sample was...The resultant pel- let was resuspended at a concentration of 10 mg/ml in endotoxin -free water, treated with DNase (Sigma, St. Louis, MO) at 100 g/ml

Acoustically levitated droplets: a contactless sampling method for fluorescence studies.

PubMed

Leiterer, Jork; Grabolle, Markus; Rurack, Knut; Resch-Genger, Ute; Ziegler, Jan; Nann, Thomas; Panne, Ulrich

2008-01-01

Acoustic levitation is used as a new tool to study concentration-dependent processes in fluorescence spectroscopy. With this technique, small amounts of liquid and solid samples can be measured without the need for sample supports or containers, which often limits signal acquisition and can even alter sample properties due to interactions with the support material. We demonstrate that, because of the small sample volume, fluorescence measurements at high concentrations of an organic dye are possible without the limitation of inner-filter effects, which hamper such experiments in conventional, cuvette-based measurements. Furthermore, we show that acoustic levitation of liquid samples provides an experimentally simple way to study distance-dependent fluorescence modulations in semiconductor nanocrystals. The evaporation of the solvent during levitation leads to a continuous increase of solute concentration and can easily be monitored by laser-induced fluorescence.

40 CFR 98.344 - Monitoring and QA/QC requirements.

Code of Federal Regulations, 2014 CFR

2014-07-01

... minutes between samples and determine the methane composition of the landfill gas using one of the methods.... ER30OC09.136 Where: CCH4 = Methane concentration in the landfill gas (volume %) for use in Equation HH-4 of... landfill gas (volume %, dry basis). (f) The owner or operator shall document the procedures used to ensure...

No brain expansion in Australopithecus boisei.

PubMed

Hawks, John

2011-10-01

The endocranial volumes of robust australopithecine fossils appear to have increased in size over time. Most evidence with temporal resolution is concentrated in East African Australopithecus boisei. Including the KNM-WT 17000 cranium, this sample comprises 11 endocranial volume estimates ranging in date from 2.5 million to 1.4 million years ago. But the sample presents several difficulties to a test of trend, including substantial estimation error for some specimens and an unusually low variance. This study reevaluates the evidence, using randomization methods and a related test using an explicit model of variability. None of these tests applied to the A. boisei endocranial volume sample produces significant evidence for a trend in that species, whether or not the early KNM-WT 17000 specimen is included. Copyright © 2011 Wiley-Liss, Inc.

Dilution effects on ultrafine particle emissions from Euro 5 and Euro 6 diesel and gasoline vehicles

NASA Astrophysics Data System (ADS)

Louis, Cédric; Liu, Yao; Martinet, Simon; D'Anna, Barbara; Valiente, Alvaro Martinez; Boreave, Antoinette; R'Mili, Badr; Tassel, Patrick; Perret, Pascal; André, Michel

2017-11-01

Dilution and temperature used during sampling of vehicle exhaust can modify particle number concentration and size distribution. Two experiments were performed on a chassis dynamometer to assess exhaust dilution and temperature on particle number and particle size distribution for Euro 5 and Euro 6 vehicles. In the first experiment, the effects of dilution (ratio from 8 to 4 000) and temperature (ranging from 50 °C to 150 °C) on particle quantification were investigated directly from tailpipe for a diesel and a gasoline Euro 5 vehicles. In the second experiment, particle emissions from Euro 6 diesel and gasoline vehicles directly sampled from the tailpipe were compared to the constant volume sampling (CVS) measurements under similar sampling conditions. Low primary dilutions (3-5) induced an increase in particle number concentration by a factor of 2 compared to high primary dilutions (12-20). Low dilution temperatures (50 °C) induced 1.4-3 times higher particle number concentration than high dilution temperatures (150 °C). For the Euro 6 gasoline vehicle with direct injection, constant volume sampling (CVS) particle number concentrations were higher than after the tailpipe by a factor of 6, 80 and 22 for Artemis urban, road and motorway, respectively. For the same vehicle, particle size distribution measured after the tailpipe was centred on 10 nm, and particles were smaller than the ones measured after CVS that was centred between 50 nm and 70 nm. The high particle concentration (≈106 #/cm3) and the growth of diameter, measured in the CVS, highlighted aerosol transformations, such as nucleation, condensation and coagulation occurring in the sampling system and this might have biased the particle measurements.

Irreversible sorption of trace concentrations of perfluorocarboxylic acids to fiber filters used for air sampling

NASA Astrophysics Data System (ADS)

Arp, Hans Peter H.; Goss, Kai-Uwe

Due to the apparent environmental omnipresence of perfluorocarboxylic acids (PFAs), an increasing number of researchers are investigating their ambient particle- and gas-phase concentrations. Typically this is done using a high-volume air sampler equipped with Quartz Fiber Filters (QFFs) or Glass Fiber Filters (GFFs) to sample the particle-bound PFAs and downstream sorbents to sample the gas-phase PFAs. This study reports that at trace, ambient concentrations gas-phase PFAs sorb to QFFs and GFFs irreversibly and hardly pass through these filters to the downstream sorbents. As a consequence, it is not possible to distinguish between particle- and gas-phase concentrations, or to distinguish concentrations on different particle size fractions, unless precautions are taken. Failure to take such precautions could have already caused reported data to be misinterpreted. Here it is also reported that deactivating QFFs and GFFs with a silylating agent renders them suitable for sampling PFAs. Based on the presented study, a series of recommendations for air-sampling PFAs are provided.

High-accuracy measurements of N2O concentration and site-specific nitrogen isotopes in small or high concentration samples

NASA Astrophysics Data System (ADS)

Palmer, M. R.; Arata, C.; Huang, K.

2014-12-01

Nitrous oxide (N2O) gas is among the major contributors to global warming and ozone depletion in stratosphere. Quantitative estimate of N­2O production in various pathways and N­2O fluxes across different reservoirs is the key to understanding the role of N­2O in the global change. To achieve this goal, accurate and concurrent measurement of both N2O concentration ([N2O]) and its site-specific isotopic composition (SP-δ15N), namely δ15Nα and δ15Nβ, is desired. Recent developments in Cavity Ring-Down Spectroscopy (CRDS) have enabled high precision measurements of [N2O] and SP-δ15N of a continuous gas flow. However, many N­­2O samples are discrete with limited volume (< 500 ml), and/or high [N2O] (> 2 ppm), and are not suitable for direct measurements by CRDS. Here we present results of a Small Sample Isotope Module 2 (SSIM2) which is coupled to and automatically coordinated with a Picarro isotopic N2O CRDS analyzer to handle and measure high concentration and/or small volume samples. The SSIM2 requires 20 ml of sample per analysis, and transfers the sample to the CRDS for high precision measurement. When the sample injection is < 20 ml, a zero gas is optionally filled to make up the volume. We used the SSIM2 to dilute high [N2O] samples and < 20 ml samples, and tested the effect of dilution on the measured SP-δ15N. In addition, we employed and tested a newly developed double injection method for samples adequate for two 20 ml injections. After the SSIM2 and the CRDS cavity was primed with the first injection, the second injection, which has negligible dilution of the sample, can be accurately measured for both [N2O] and SP-δ15N. Results of these experiments indicate that the precision of SSIM2-CRDS is similar to that of the continuous measurements using the CRDS alone, and that dilution has minimal effect on SP-δ15N, as along as the [N2O] is > 300 ppb after dilution. Overall, the precision of SP-δ15N measured using the SSIM2 is < 0.5 ‰.

Effects of Heat Flux, Oxygen Concentration and Glass Fiber Volume Fraction on Pyrolysate Mass Flux from Composite Solids

NASA Technical Reports Server (NTRS)

Rich, D. B.; Lautenberger, C. W.; Yuan, Z.; Fernandez-Pello, A. C.

2004-01-01

Experimental work on the effects of heat flux, oxygen concentration and glass fiber volume fraction on pyrolysate mass flux from samples of polypropylene/glass fiber composite (PP/G) is underway. The research is conducted as part of a larger project to develop a test methodology for flammability of materials, particularly composites, in the microgravity and variable oxygen concentration environment of spacecraft and space structures. Samples of PP/G sized at 30 x 30 x 10 mm are flush mounted in a flow tunnel, which provides a flow of oxidizer over the surface of the samples at a fixed value of 1 m/s and oxygen concentrations varying between 18 and 30%. Each sample is exposed to a constant external radiant heat flux at a given value, which varies between tests from 10 to 24 kW/sq m. Continuous sample mass loss and surface temperature measurements are recorded for each test. Some tests are conducted with an igniter and some are not. In the former case, the research goal is to quantify the critical mass flux at ignition for the various environmental and material conditions described above. The later case generates a wider range of mass flux rates than those seen prior to ignition, providing an opportunity to examine the protective effects of blowing on oxidative pyrolysis and heating of the surface. Graphs of surface temperature and sample mass loss vs. time for samples of 30% PPG at oxygen concentrations of 18 and 21% are presented in the figures below. These figures give a clear indication of the lower pyrolysis rate and extended time to ignition that accompany a lower oxygen concentration. Analysis of the mass flux rate at the time of ignition gives good repeatability but requires further work to provide a clear indication of mass flux trends accompanying changes in environmental and material properties.

Effects of Heat Flux, Oxygen Concentration and Glass Fiber Volume Fraction on Pyrolysate Mass Flux from Composite Solids

NASA Technical Reports Server (NTRS)

Rich, D. B.; Lautenberger, C. W.; Yuan, Z.; Fernandez-Pello, A. C.

2004-01-01

Experimental work on the effects of heat flux, oxygen concentration and glass fiber volume fraction on pyrolysate mass flux from samples of polypropylene/glass fiber composite (PP/G) is underway. The research is conducted as part of a larger project to develop a test methodology for flammability of materials, particularly composites, in the microgravity and variable oxygen concentration environment of spacecraft and space structures. Samples of PP/G sized at 30x30x10 mm are flush mounted in a flow tunnel, which provides a flow of oxidizer over the surface of the samples at a fixed value of 1 m/s and oxygen concentrations varying between 18 and 30%. Each sample is exposed to a constant external radiant heat flux at a given value, which varies between tests from 10 to 24 kW/m2. Continuous sample mass loss and surface temperature measurements are recorded for each test. Some tests are conducted with an igniter and some are not. In the former case, the research goal is to quantify the critical mass flux at ignition for the various environmental and material conditions described above. The later case generates a wider range of mass flux rates than those seen prior to ignition, providing an opportunity to examine the protective effects of blowing on oxidative pyrolysis and heating of the surface. Graphs of surface temperature and sample mass loss vs. time for samples of 30% PPG at oxygen concentrations of 18 and 21% are presented in the figures below. These figures give a clear indication of the lower pyrolysis rate and extended time to ignition that accompany a lower oxygen concentration. Analysis of the mass flux rate at the time of ignition gives good repeatability but requires further work to provide a clear indication of mass flux trends accompanying changes in environmental and material properties.

[Evaluation of immunoglobulin G concentration in colostrum of mares by ELISA, refractometry and colostrometry].

PubMed

Venner, Monica; Markus, R G; Strutzberg-Minder, K; Nogai, K; Beyerbach, M; Klug, E

2008-01-01

In 360 samples of colostrum and 36 samples of blood of warmblood mares, the concentration of immunoglobulin G (IgG) was evaluated in the post partal period with an ELISA and the results were compared to values obtained with 2 field methods--refractometry and colostrometry. A significant correlation (p < 0.0001) was determined between ELISA and colostrometry (r = +0.88) and between ELISA and refractometry (r = +0.93). So both field-methods seem suitable for evaluation of the colostral IgG-concentration in mares. Further the kinetic of the IgG concentration in colostrum, the volume of colostrum and the total amount of IgG was measured in the 12 hours post partum (p.p.) in each half udder of 36 mares of different parity. Immediately p.p. primiparous mares have a greater mean concentration of IgG (68 mg/ml) than multiparous mares (51 mg/ml). However, multiparous mares have a mean colostral volume of 1020 ml whereas, in primiparous mares, a mean volume of 527 ml was determined within the first three hours p.p. As a result of this the total amount of IgG was lower in primiparous (31.5 g) than in multiparous mares (48.5 g). A significant decrease of IgG concentration was measured in multiparous mares in the 1.5 hours following partum versus 3 hours in primiparous mares. The mean IgG concentration in the blood serum of the 36 mares immediately p.p. was 13.4 +/- 3.6 mg/ml. No significant correlation was observed between values of IgG concentration in the blood and in the colostrum of the mares.

A method for nitrate collection for δ15N and δ18O analysis from waters with low nitrate concentrations

USGS Publications Warehouse

Chang, Cecily C.Y.; Langston, J.; Riggs, M.; Campbell, D.H.; Silva, S.R.; Kendall, C.

1999-01-01

 Recently, methods have been developed to analyze NO3- for δ15N and δ18O, improving our ability to identify NO3- sources and transformations. However, none of the existing methods are suited for waters with low NO3- concentrations (0.7-10 µM). We describe an improved method for collecting and recovering NO3- on exchange columns. To overcome the lengthy collection loading times imposed by the large sample volumes (7-70 L), the sample was prefiltered (0.45 µm) with a large surface area filter. Switching to AG2X anion resin and using a coarser mesh size (100-200) than previous methods also enhanced sample flow. Placement of a cation column in front of the anion column minimized clogging of the anion column by dissolved organic carbon (DOC) accumulation. This also served to minimize transfer of unwanted oxygen atoms from DOC to the 18O portion of the NO3- sample, thereby contaminating the sample and shifting δ18O. The cat-AG2X method is suited for on-site sample collection, making it possible to collect and recover NO3- from low ionic strength waters with modest DOC concentrations (80-800 µM), relieves the investigator of transporting large volumes of water back to the laboratory, and offers a means of sampling rain, snow, snowmelt, and stream samples from access-limited sites.

Accumulations of Heavy Metals in Roadside Soils Close to Zhaling, Eling and Nam Co Lakes in the Tibetan Plateau

PubMed Central

Yan, Xuedong; Zhang, Fan; Gao, Dan; Zeng, Chen; Xiang, Wang; Zhang, Man

2013-01-01

Concentrations of four typical heavy metals (Cu; Zn; Cd and Pb) in roadside soils close to three lakes in the Tibetan Plateau were investigated in this study. The hierarchical tree-based regression method was applied to classify concentrations of the heavy metals and analyze their potential influencing factors. It was found that the Tibetan Plateau meadow soils with higher content of sand lead to higher concentrations of Cu; Zn and Pb. The concentrations of Cd and Pb increase with road traffic volume; and for the road segments with higher traffic volume; the Cd and Pb concentrations significantly decrease with the roadside distance. Additionally; the concentrations of Zn and Pb increase as the altitude of sampling site increases. Furthermore; the Hakanson potential ecological risk index method was used to assess the contamination degree of the heavy metals for the study regions. The results show that accumulations of Cu; Zn and Pb in roadside soils remain an unpolluted level at all sites. However; the Cd indices in the regions with higher traffic volume have reached a strong potential ecological risk level; and some spots with peak concentrations have even been severely polluted due to traffic activities. PMID:23749055

High-throughput analysis using non-depletive SPME: challenges and applications to the determination of free and total concentrations in small sample volumes.

PubMed

Boyacı, Ezel; Bojko, Barbara; Reyes-Garcés, Nathaly; Poole, Justen J; Gómez-Ríos, Germán Augusto; Teixeira, Alexandre; Nicol, Beate; Pawliszyn, Janusz

2018-01-18

In vitro high-throughput non-depletive quantitation of chemicals in biofluids is of growing interest in many areas. Some of the challenges facing researchers include the limited volume of biofluids, rapid and high-throughput sampling requirements, and the lack of reliable methods. Coupled to the above, growing interest in the monitoring of kinetics and dynamics of miniaturized biosystems has spurred the demand for development of novel and revolutionary methodologies for analysis of biofluids. The applicability of solid-phase microextraction (SPME) is investigated as a potential technology to fulfill the aforementioned requirements. As analytes with sufficient diversity in their physicochemical features, nicotine, N,N-Diethyl-meta-toluamide, and diclofenac were selected as test compounds for the study. The objective was to develop methodologies that would allow repeated non-depletive sampling from 96-well plates, using 100 µL of sample. Initially, thin film-SPME was investigated. Results revealed substantial depletion and consequent disruption in the system. Therefore, new ultra-thin coated fibers were developed. The applicability of this device to the described sampling scenario was tested by determining the protein binding of the analytes. Results showed good agreement with rapid equilibrium dialysis. The presented method allows high-throughput analysis using small volumes, enabling fast reliable free and total concentration determinations without disruption of system equilibrium.

Methylmercury and other chemical constituents in Pacific coastal fog water from seven sites in Central/Northern California (FogNet) during the summer of 2014

NASA Astrophysics Data System (ADS)

Weiss-Penzias, P. S.; Heim, W. A.; Fernandez, D.; Coale, K. H.; Oliphant, A. J.; Dann, D.; Porter, M.; Hoskins, D.; Dodge, C.

2014-12-01

This project investigates the mercury content in summertime Pacific coastal fog in California and whether fog could be an important vector for ocean emissions of mercury to be deposited via fog drip to upland coastal ecosystems. Efforts began in early 2014 with the building of 7 active-strand fog collectors based on the Colorado State University Caltech CASCC design. The new UCSC CASCC includes doors sealing the collector which open under microcomputer control based on environmental sensing (relative humidity). Seven sites spanning from Trinidad in the north to Marina in the south have collected samples June-August 2014 under a project called FogNet. Fog conditions were favorable for collecting large water volumes (> 250 mL) at many sites. Fog samplers were cleaned with soap and deionized water daily and field blanks taken immediately following cleaning. Fog water samples were collected overnight, split into an aliquot for anion and DOC/DIC analysis and the remaining sample was acidified. Monomethyl mercury (MMHg) concentrations in samples and field blanks for 3 sites in FogNet are shown in the accompanying figure. The range of MMHg concentrations from 10 fog water samples > 100 mL in volume was 0.9-9.3 ng/L (4.5-46.4 pM). Elevated MMHg concentrations (> 5 ng/L, 25 pM) were observed at 2 sites: UC Santa Cruz and Bodega Bay. The field blanks produced MMHg concentrations of 0.08-0.4 ng/L (0.4-2.0 pM), which was on average < 10% of the sample concentration and suggests the artifact due to sampling was small. The observed MMHg concentrations in fog water observed is this study are 1-2 orders of magnitude greater than MMHg concentrations seen previously in rain water samples from the California coast suggesting an additional source of MMHg to fog. Shipboard measurements of dimethyl mercury (DMHg) in coastal California seawater during the time period of FogNet operations (summer 2014) reveal surface waters that were supersaturated in DMHg which represents a potential source of organic mercury to the overlying fog bank.

Particle concentration and Characteristics near a major freeway with heavy-duty diesel traffic.

PubMed

Ntziachristos, Leonidas; Ning, Zhi; Geller, Michael D; Sioutas, Constantinos

2007-04-01

This study presents the number, surface and volume concentrations, and size distribution of particles next to the 1-710 freeway during February through April 2006. 1-710 has the highest ratio (up to 25%) of heavy-duty diesel vehicles in the Los Angeles highway network. Particle concentration measurements were accompanied by measurements of black carbon, elemental and organic carbon, and gaseous species (CO, CO2). Using the incremental increase of CO2 over the background to calculate the dilution ratio, this study makes it possible to compare particle concentrations measured next to the freeway to concentrations measured in roadway tunnels and in vehicle exhaust. In addition to the effect of the dilution ratio on the measured particle concentrations, multivariate linear regressions showed that light and heavy organic carbon concentrations are positively correlated with the particle volume in the nucleation and accumulation modes, respectively. Solar radiation was also positively correlated with the particle surface concentration and the particle volume in the accumulation (40-638 nm) mode, presumably as a result of secondary particle formation. The methods developed in this study may be used to decouple the effect of sampling position, meteorology, and fleet operation on particle concentrations in the proximity of freeways, roadway tunnels, and in street canyons.

Multiparametric Flow System for the Automated Determination of Sodium, Potassium, Calcium, and Magnesium in Large-Volume Parenteral Solutions and Concentrated Hemodialysis Solutions

PubMed Central

Pistón, Mariela; Dol, Isabel

2006-01-01

A multiparametric flow system based on multicommutation and binary sampling has been designed for the automated determination of sodium, potassium, calcium, and magnesium in large-volume parenteral solutions and hemodialysis concentrated solutions. The goal was to obtain a computer-controlled system capable of determining the four metals without extensive modifications. The system involved the use of five solenoid valves under software control, allowing the establishment of the appropriate flow conditions for each analyte, that is, sample size, dilution, reagent addition, and so forth. Detection was carried out by either flame atomic emission spectrometry (sodium, potassium) or flame atomic absorption spectrometry (calcium, magnesium). The influence of several operating parameters was studied. Validation was carried out by analyzing artificial samples. Figures of merit obtained include linearity, accuracy, precision, and sampling frequency. Linearity was satisfactory: sodium, r 2 >0.999 ( 0.5 – 3.5 g/L), potassium, r 2 >0.996 (50–150 mg/L), calcium, r 2 >0.999 (30–120 mg/L), and magnesium, r 2 >0.999 (20–40 mg/L). Precision ( s r , %, n=5 ) was better than 2.1 %, and accuracy (evaluated through recovery assays) was in the range of 99.8 %– 101.0 % (sodium), 100.8 – 102.5 % (potassium), 97.3 %– 101.3 % (calcium), and 97.1 %– 99.8 % (magnesium). Sampling frequencies ( h −1 ) were 70 (sodium), 75 (potassium), 70 (calcium), and 58 (magnesium). According to the results obtained, the use of an automated multiparametric system based on multicommutation offers several advantages for the quality control of large-volume parenteral solutions and hemodialysis concentrated solutions. PMID:17671619

Dual dispersive liquid-liquid microextraction for determination of phenylpropenes in oils by gas chromatography-mass spectrometry.

PubMed

Tsai, Chia-Ju; Li, Jih-Heng; Feng, Chia-Hsien

2015-09-04

A novel, simple and quick sample preparation method was developed and used for pre-concentration and extraction of six phenylpropenes, including anethole, estragole, eugenol, methyl eugenol, safrole and myristicin, from oil samples by dual dispersive liquid-liquid microextraction. Gas chromatography-mass spectrometry was used for determination and separation of compounds. Several experimental parameters affecting extraction efficiency were evaluated and optimized, including forward-extractant type and volume, surfactant type and concentration, water volume, and back-extractant type and volume. For all analytes (10-1000ng/mL), the limits of detection (S/N≧3) ranged from 1.0 to 3.0ng/mL; the limits of quantification (S/N≧10) ranged from 2.5 to 10.0ng/mL; and enrichment factors ranged from 3.2 to 37.1 times. Within-run and between-run relative standard deviations (n=6) were less than 2.61% and less than 4.33%, respectively. Linearity was excellent with determination coefficients (r(2)) above 0.9977. The experiments showed that the proposed method is a simple, effective, and environmentally friendly method of analyzing phenylpropenes in oil samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Predicting runoff induced mass loads in urban watersheds: Linking land use and pyrethroid contamination.

PubMed

Chinen, Kazue; Lau, Sim-Lin; Nonezyan, Michael; McElroy, Elizabeth; Wolfe, Becky; Suffet, Irwin H; Stenstrom, Michael K

2016-10-01

Pyrethroid pesticide mass loadings in the Ballona Creek Watershed were calculated using the volume-concentration method with a Geographic Information Systems (GIS) to explore potential relationships between urban land use, impervious surfaces, and pyrethroid runoff flowing into an urban stream. A calibration of the GIS volume-concentration model was performed using 2013 and 2014 wet-weather sampling data. Permethrin and lambda-cyhalothrin were detected as the highest concentrations; deltamethrin, lambda-cyhalothrin, permethrin and cyfluthrin were the most frequently detected synthetic pyrethroids. Eight neighborhoods within the watershed were highlighted as target areas based on a Weighted Overlay Analysis (WOA) in GIS. Water phase concentration of synthetic pyrethroids (SPs) were calculated from the reported usage. The need for stricter BMP and consumer product controls was identified as a possible way of reducing the detections of pyrethroids in Ballona Creek. This model has significant implications for determining mass loadings due to land use influence, and offers a flexible method to extrapolate data for a limited amount of samplings for a larger watershed, particularly for chemicals that are not subject to environmental monitoring. Offered as a simple approach to watershed management, the GIS-volume concentration model has the potential to be applied to other target pesticides and is useful for simulating different watershed scenarios. Further research is needed to compare results against other similar urban watersheds situated in mediterranean climates. Copyright © 2016 Elsevier Ltd. All rights reserved.

Nanopore sensing at ultra-low concentrations using single-molecule dielectrophoretic trapping

NASA Astrophysics Data System (ADS)

Freedman, Kevin J.; Otto, Lauren M.; Ivanov, Aleksandar P.; Barik, Avijit; Oh, Sang-Hyun; Edel, Joshua B.

2016-01-01

Single-molecule techniques are being developed with the exciting prospect of revolutionizing the healthcare industry by generating vast amounts of genetic and proteomic data. One exceptionally promising route is in the use of nanopore sensors. However, a well-known complexity is that detection and capture is predominantly diffusion limited. This problem is compounded when taking into account the capture volume of a nanopore, typically 108-1010 times smaller than the sample volume. To rectify this disproportionate ratio, we demonstrate a simple, yet powerful, method based on coupling single-molecule dielectrophoretic trapping to nanopore sensing. We show that DNA can be captured from a controllable, but typically much larger, volume and concentrated at the tip of a metallic nanopore. This enables the detection of single molecules at concentrations as low as 5 fM, which is approximately a 103 reduction in the limit of detection compared with existing methods, while still maintaining efficient throughput.

Concentration of Enteroviruses, Adenoviruses, and Noroviruses from Drinking Water by Use of Glass Wool Filters▿

PubMed Central

Lambertini, Elisabetta; Spencer, Susan K.; Bertz, Phillip D.; Loge, Frank J.; Kieke, Burney A.; Borchardt, Mark A.

2008-01-01

Available filtration methods to concentrate waterborne viruses are either too costly for studies requiring large numbers of samples, limited to small sample volumes, or not very portable for routine field applications. Sodocalcic glass wool filtration is a cost-effective and easy-to-use method to retain viruses, but its efficiency and reliability are not adequately understood. This study evaluated glass wool filter performance to concentrate the four viruses on the U.S. Environmental Protection Agency contaminant candidate list, i.e., coxsackievirus, echovirus, norovirus, and adenovirus, as well as poliovirus. Total virus numbers recovered were measured by quantitative reverse transcription-PCR (qRT-PCR); infectious polioviruses were quantified by integrated cell culture (ICC)-qRT-PCR. Recovery efficiencies averaged 70% for poliovirus, 14% for coxsackievirus B5, 19% for echovirus 18, 21% for adenovirus 41, and 29% for norovirus. Virus strain and water matrix affected recovery, with significant interaction between the two variables. Optimal recovery was obtained at pH 6.5. No evidence was found that water volume, filtration rate, and number of viruses seeded influenced recovery. The method was successful in detecting indigenous viruses in municipal wells in Wisconsin. Long-term continuous filtration retained viruses sufficiently for their detection for up to 16 days after seeding for qRT-PCR and up to 30 days for ICC-qRT-PCR. Glass wool filtration is suitable for large-volume samples (1,000 liters) collected at high filtration rates (4 liters min−1), and its low cost makes it advantageous for studies requiring large numbers of samples. PMID:18359827

Method for Salmonella concentration from water at pH 3.5, using micro-fiber glass filters.

PubMed Central

Block, J C; Rolland, D

1979-01-01

A method is described for the concentration of Salmonella from water. As is done with enterovirus, Salmonella bacteria were concentrated from water in two steps: by pH 3.5 adsorption on and pH 9.5 elution from 8-micron porosity micro-fiber glass filter tubes. This method worked in less than 30 min, and Salmonella typhimurium was inactivated only slightly in spite of rapid pH variations (pH 3.5 to 9.5). It was demonstrated that the retention by the filters stems from two phenomena: a low retention in the micro-fiber glass labyrinth for small filtered volumes, and a high retention by adsorption at pH 3.5 for any filtered volume (experiments done with 15- and 80-liter samples). Addition in tap water of trivalent ions like Al3+ did not increase Salmonella adsorption. In most of the trials, Salmonella recovery varied from 42 to 93%. Preliminary field investigations indicate that enterovirus and Salmonella may both be concentrated from the same water sample by this procedure. PMID:39501

Comparison of a Point-of-Care Glucometer and a Laboratory Autoanalyzer for Measurement of Blood Glucose Concentrations in Domestic Pigeons ( Columba livia domestica).

PubMed

Mohsenzadeh, Mahdieh Sadat; Zaeemi, Mahdieh; Razmyar, Jamshid; Azizzadeh, Mohammad

2015-09-01

Biochemical analysis is necessary for diagnosis and monitoring of diseases in birds; however, the small volume of blood that can be safely obtained from small avian species often limits laboratory diagnostic testing. Consequently, a suitable methodology requiring only a small volume of blood must be used. This study was designed to compare blood glucose concentrations in domestic pigeons ( Columba livia domestica) as measured by a commercial, handheld, human glucometer and a standard autoanalyzer. During the first phase of the study, whole blood samples obtained from 30 domestic pigeons were used to measure the blood glucose concentration with a glucometer, the packed cell volume (PCV), and the total erythrocyte count (nRBC). Plasma separated from the each sample was then used to obtain the plasma glucose concentration with the autoanalyzer. During the second phase of the study, 30 pigeons were assigned to 2 equal groups (n = 15). Hypoglycemia or hyperglycemia was induced in each group by intravenous injection of insulin or glucose, respectively. Blood was collected and processed, and glucose concentrations, PCV, and nRBC were measured as previously described. Linear-regression models demonstrated a significant relationship between results measured by the glucometer and autoanalyzer results from normoglycemic (correlation coefficient [R] = 0.43, P = .02), hypoglycemic (R = 0.95; P < .001), and hyperglycemic (R = 0.81; P < .001) birds. The results of this study suggest that we can predict the real blood-glucose concentration of pigeons by using results obtained by a glucometer.

Determination of boron in produced water using the carminic acid assay.

PubMed

Floquet, Cedric F A; Sieben, Vincent J; MacKay, Bruce A; Mostowfi, Farshid

2016-04-01

Using the carminic acid assay, we determined the concentration of boron in oilfield waters. We investigated the effect of high concentrations of salts and dissolved metals on the assay performance. The influence of temperature, development time, reagent concentration, and water volume was studied. Ten produced and flowback water samples of different origins were measured, and the method was successfully validated against ICP-MS measurements. In water-stressed regions, produced water is a potential source of fresh water for irrigation, industrial applications, or consumption. Therefore, boron concentration must be determined and controlled to match the envisaged waste water reuse. Fast, precise, and onsite measurements are needed to minimize errors introduced by sample transportation to laboratories. We found that the optimum conditions for our application were a 5:1 mixing volume ratio (reagent to sample), a 1 g L(-1) carminic acid concentration in 99.99% sulfuric acid, and a 30 min reaction time at ambient temperature (20 °C to 23 °C). Absorption values were best measured at 610 nm and 630 nm and baseline corrected at 865 nm. Under these conditions, the sensitivity of the assay to boron was maximized while its cross-sensitivity to dissolved titanium, iron, barium and zirconium was minimized, alleviating the need for masking agents and extraction methods. Copyright © 2015 Elsevier B.V. All rights reserved.

Simple and quick determination of analgesics and other contaminants of emerging concern in environmental waters by on-line solid phase extraction coupled to liquid chromatography-tandem mass spectrometry.

PubMed

Ferrer-Aguirre, Alejandra; Romero-González, Roberto; Vidal, J L Martínez; Frenich, Antonia Garrido

2016-05-13

A simple and quick analytical method has been developed for the determination of pharmaceutical compounds in water. An on-line solid-phase extraction (SPE) coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been optimized to determine 7 contaminants of emerging concern in environmental waters at ngL(-1) levels. This procedure requires minimal sample handling and small sample volume (900μL) with a total running time of 18min. Several SPE parameters were evaluated and optimized in order to achieve a high sample throughput. Therefore sample volume, carryover and reusability of the cartridges were evaluated. Performance characteristics were evaluated and good linearity was obtained (R(2)>0.98). Recoveries were evaluated in spiked samples at three concentrations and the values ranged from 71 to 104%. Intra and inter-day precision was lower than 10 and 13% respectively. Limits of quantification were equal to or lower than 10ngL(-1), except for 1,7-dimethylxanthine (20ngL(-1)) and ibuprofen (50ngL(-1)). The method was applied to 20 environmental water samples, and ibuprofen was the compound most widely detected at concentrations up to 42.06μgL(-1), whereas the other compounds were detected in fewer samples at lower concentrations (up to 15.99μgL(-1)). Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of radionuclide concentrations in ground level air using the ASS-500 high volume sampler

DOE Office of Scientific and Technical Information (OSTI.GOV)

Frenzel, E.; Arnold, D.; Wershofen, H.

1996-06-01

A method for determination of radionuclide concentrations in air aerosol samples collected by the high volume aerosol sampler ASS-500 was elaborated. The aerosol sampling station ASS-500 is a Stand alone, all-weather proofed instrument. It is designed for representative sampling of airborne radionuclides from ground level air at a height of about 1.5 m above ground level. The ASS-500 station enables continuous air monitoring both normal and emergency Situations. The collection of aerosols on the Petrianov FPP-15-1.5 type filter out of an air volume of about 100,000 m{sup 3} (sampling period 1 wk) or of about 250,000 m{sup 3} (sampling periodmore » 3 wk) admits accurate spectrometric low level measurements of natural and artificial radionuclides. The achieved detection limit is 0.5 {mu}Bq m{sup -3} and 0.2 {mu}Bq m{sup -3} for {sup 137}Cs, respectively. A new developed air flow Meter system allows to enhance the collected air volume to about 150,000 m{sup 3} per week and lowers the detection limit to <0.4 {mu}Bq m{sup -3} for {sup 137}Cs for weekly collected aerosol samples. In Poland the CLOR uses 9 Stations ASS-500 at different sites as atmospheric radioactivity control system. On the basis of spectrometric measurements of natural and artificial radionuclides in the collected aerosol samples at the different sites, CLOR establishes a weekly report about the radiological situation at Poland for responsible authorities. The very low achievable detection limit of the Station ASS-500 due 10 the high air flow fate and the long possible sampling period were the key argument for other government radiation protection authorities in Europe to introduce the Station ASS-500 into their low level radionuclide atmospheric monitoring programs (Austria, Belarus, France, Germany, Iceland, Spain, Switzerland, Ukraine).« less

Environmental Validation of Legionella Control in a VHA Facility Water System.

PubMed

Jinadatha, Chetan; Stock, Eileen M; Miller, Steve E; McCoy, William F

2018-03-01

OBJECTIVES We conducted this study to determine what sample volume, concentration, and limit of detection (LOD) are adequate for environmental validation of Legionella control. We also sought to determine whether time required to obtain culture results can be reduced compared to spread-plate culture method. We also assessed whether polymerase chain reaction (PCR) and in-field total heterotrophic aerobic bacteria (THAB) counts are reliable indicators of Legionella in water samples from buildings. DESIGN Comparative Legionella screening and diagnostics study for environmental validation of a healthcare building water system. SETTING Veterans Health Administration (VHA) facility water system in central Texas. METHODS We analyzed 50 water samples (26 hot, 24 cold) from 40 sinks and 10 showers using spread-plate cultures (International Standards Organization [ISO] 11731) on samples shipped overnight to the analytical lab. In-field, on-site cultures were obtained using the PVT (Phigenics Validation Test) culture dipslide-format sampler. A PCR assay for genus-level Legionella was performed on every sample. RESULTS No practical differences regardless of sample volume filtered were observed. Larger sample volumes yielded more detections of Legionella. No statistically significant differences at the 1 colony-forming unit (CFU)/mL or 10 CFU/mL LOD were observed. Approximately 75% less time was required when cultures were started in the field. The PCR results provided an early warning, which was confirmed by spread-plate cultures. The THAB results did not correlate with Legionella status. CONCLUSIONS For environmental validation at this facility, we confirmed that (1) 100 mL sample volumes were adequate, (2) 10× concentrations were adequate, (3) 10 CFU/mL LOD was adequate, (4) in-field cultures reliably reduced time to get results by 75%, (5) PCR provided a reliable early warning, and (6) THAB was not predictive of Legionella results. Infect Control Hosp Epidemiol 2018;39:259-266.

Concentric micro-nebulizer for direct sample insertion

DOEpatents

Fassel, V.A.; Rice, G.W.; Lawrence, K.E.

1984-03-06

A concentric micro-nebulizer and method for introducing liquid samples into a plasma established in a plasma torch including a first tube connected to a source of plasma gas. The concentric micro-nebulizer has inner and outer concentric tubes extending upwardly within the torch for connection to a source of nebulizer gas and to a source of liquid solvent and to a source of sample liquid. The inner tube is connected to the source of liquid solvent and to the source of sample liquid and the outer tube is connected to the source of nebulizer gas. The outer tube has an orifice positioned slightly below the plasma when it is established, with the inner and outer tubes forming an annulus therebetween with the annular spacing between the tubes at said orifice being less than about 0.05mm. The dead volume of the inner tube is less than about 5 microliters.

Concentric micro-nebulizer for direct sample insertion

DOEpatents

Fassel, Velmer A.; Rice, Gary W.; Lawrence, Kimberly E.

1986-03-11

A concentric micro-nebulizer and method for introducing liquid samples into a plasma established in a plasma torch including a first tube connected to a source of plasma gas. The concentric micro-nebulizer has inner and outer concentric tubes extending upwardly within the torch for connection to a source of nebulizer gas and to a source of liquid solvent and to a source of sample liquid. The inner tube is connected to the source of liquid solvent and to the source of sample liquid and the outer tube is connected to the source of nebulizer gas. The outer tube has an orifice positioned slightly below the plasma when it is established, with the inner and outer tubes forming an annulus therebetween with the annular spacing between the tubes at said orifice being less than about 0.05 mm. The dead volume of the inner tube is less than about 5 microliters.

Effects of Lugol's iodine solution and formalin on cell volume of three bloom-forming dinoflagellates

NASA Astrophysics Data System (ADS)

Yang, Yang; Sun, Xiaoxia; Zhao, Yongfang

2017-07-01

Fixatives are traditionally used in marine ecosystem research. The bias introduced by fixatives on the dimensions of plankton cells may lead to an overestimation or underestimation of the carbon biomass. To determine the impact of traditional fixatives on dinoflagellates during short- and long-term fixation, we analyzed the degree of change in three bloom-forming dinoflagellates ( Prorocentrum micans, Scrippsiella trochoidea and Noctiluca scintillans) brought about by Lugol's iodine solution (hereafter Lugol's) and formalin. The fixation effects were species-specific. P. micans cell volume showed no significant change following long-term preservation, and S. trochoidea swelled by approximately 8.06% in Lugol's and by 20.97% in formalin as a percentage of the live cell volume, respectively. N. scintillans shrank significantly in both fixatives. The volume change due to formalin in N. scintillans was not concentration-dependent, whereas the volume shrinkage of N. scintillans cells fixed with Lugol's at a concentration of 2% was nearly six-fold that in cells fixed with Lugol's at a concentration of 0.6%-0.8%. To better estimate the volume of N. scintillans fixed in formalin at a concentration of 5%, we suggest that the conversion relationship was as follows: volume of live cell=volume of intact fixed cell/0.61. Apart from size change, damage induced by fixatives on N. scintillans was obvious. Lugol's is not a suitable fixative for N. scintillans due to high frequency of broken cells. Accurate carbon biomass estimate of N. scintillans should be performed on live samples. These findings help to improve the estimate of phytoplankton cell volume and carbon biomass in marine ecosystem.

Counting at low concentrations: the statistical challenges of verifying ballast water discharge standards

USGS Publications Warehouse

Frazier, Melanie; Miller, A. Whitman; Lee, Henry; Reusser, Deborah A.

2013-01-01

Discharge from the ballast tanks of ships is one of the primary vectors of nonindigenous species in marine environments. To mitigate this environmental and economic threat, international, national, and state entities are establishing regulations to limit the concentration of living organisms that may be discharged from the ballast tanks of ships. The proposed discharge standards have ranged from zero detectable organisms to 3. If standard sampling methods are used, verifying whether ballast discharge complies with these stringent standards will be challenging due to the inherent stochasticity of sampling. Furthermore, at low concentrations, very large volumes of water must be sampled to find enough organisms to accurately estimate concentration. Despite these challenges, adequate sampling protocols comprise a critical aspect of establishing standards because they help define the actual risk level associated with a standard. A standard that appears very stringent may be effectively lax if it is paired with an inadequate sampling protocol. We describe some of the statistical issues associated with sampling at low concentrations to help regulators understand the uncertainties of sampling as well as to inform the development of sampling protocols that ensure discharge standards are adequately implemented.

Comparison of pesticides and other compounds in carpet dust samples collected from used vacuum cleaner bags and from a high-volume surface sampler.

PubMed Central

Colt, J S

1998-01-01

Epidemiologic studies of the association between residential pesticide use and cancer risk require an assessment of past pesticide exposures. Pesticide levels in carpet dust are believed to reflect long-term pesticide use. Recent epidemiologic studies have found collection of dust samples using the high-volume surface sampler (HVS3) to be expensive and cumbersome. We compared the levels of pesticides and other compounds in dust obtained from subjects' personal used vacuum cleaner bags to that collected by the HVS3 to see if this simpler method could replace the HVS3 in epidemiologic research. We visited the homes of 15 subjects, took the used bags from their vacuums, and collected carpet dust samples with the HVS3. The samples were analyzed for 42 target compounds: 26 pesticides, 10 polycyclic aromatic hydrocarbons (PAHs), and six polychlorinated biphenyl (PCB) congeners using GC/MS in selected ion monitoring mode. The two methods agreed in detecting the presence of the target compounds between 80% and 100% of the time. Neither sampling method was consistently more sensitive. The median target compound concentrations were similar, and a paired t-test showed no significant differences. For many compounds, the concentrations of compounds in the HVS3 samples were higher than those in the used bag samples at the upper end of the concentration ranges. However, the Spearman rank correlation coefficients were 0.85 or higher for most compounds, indicating that homes would be ranked similarly using both methods. Overall, there appears to be no clear difference in the quality of the pesticide, PAH, or PCB concentration data for the two dust collection methods. Images Figure 1 PMID:9799187

Variation of semen parameters in healthy medical students due to exam stress.

PubMed

Lampiao, Fanuel

2009-12-01

This study was aimed at investigating semen parameters that vary most in samples of healthy donors undergoing stressful examination period. Samples were left to liquefy in an incubator at 37 degrees C, 5% CO2 for 30 minutes before volume was measured. Concentration and motility parameters were measured by means of computer assisted semen analysis (CASA) using Sperm Class Analyzer (Microptic S.L, Madrid, Spain). Sperm concentration was significantly decreased in samples donated close to the exam period as well as samples donated during the exam period when compared to samples donated at the beginning of the semester. Stress levels of donors might prove to be clinically relevant and important when designing experiment protocols.

Echographic detectability of optoacoustic signals from low-concentration PEG-coated gold nanorods

PubMed Central

Conversano, Francesco; Soloperto, Giulia; Greco, Antonio; Ragusa, Andrea; Casciaro, Ernesto; Chiriacò, Fernanda; Demitri, Christian; Gigli, Giuseppe; Maffezzoli, Alfonso; Casciaro, Sergio

2012-01-01

Purpose: To evaluate the diagnostic performance of gold nanorod (GNR)-enhanced optoacoustic imaging employing a conventional echographic device and to determine the most effective operative configuration in order to assure optoacoustic effectiveness, nanoparticle stability, and imaging procedure safety. Methods: The most suitable laser parameters were experimentally determined in order to assure nanoparticle stability during the optoacoustic imaging procedures. The selected configuration was then applied to a novel tissue-mimicking phantom, in which GNR solutions covering a wide range of low concentrations (25–200 pM) and different sample volumes (50–200 μL) were exposed to pulsed laser irradiation. GNR-emitted optoacoustic signals were acquired either by a couple of single-element ultrasound probes or by an echographic transducer. Off-line analysis included: (a) quantitative evaluation of the relationships between GNR concentration, sample volume, phantom geometry, and amplitude of optoacoustic signals propagating along different directions; (b) echographic detection of “optoacoustic spots,” analyzing their intensity, spatial distribution, and clinical exploitability. MTT measurements performed on two different cell lines were also used to quantify biocompatibility of the synthesized GNRs in the adopted doses. Results: Laser irradiation at 30 mJ/cm2 for 20 seconds resulted in the best compromise among the requirements of effectiveness, safety, and nanoparticle stability. Amplitude of GNR-emitted optoacoustic pulses was proportional to both sample volume and concentration along each considered propagation direction for all the tested boundary conditions, providing an experimental confirmation of isotropic optoacoustic emission. Average intensity of echographically detected spots showed similar behavior, emphasizing the presence of an “ideal” GNR concentration (100 pM) that optimized optoacoustic effectiveness. The tested GNRs also exhibited high biocompatibility over the entire considered concentration range. Conclusion: An optimal configuration for GNR-enhanced optoacoustic imaging was experimentally determined, demonstrating in particular its feasibility with a conventional echographic device. The proposed approach can be easily extended to quantitative performance evaluation of different contrast agents for optoacoustic imaging. PMID:22927756

The precision of wet atmospheric deposition data from national atmospheric deposition program/national trends network sites determined with collocated samplers

USGS Publications Warehouse

Nilles, M.A.; Gordon, J.D.; Schroder, L.J.

1994-01-01

A collocated, wet-deposition sampler program has been operated since October 1988 by the U.S. Geological Survey to estimate the overall sampling precision of wet atmospheric deposition data collected at selected sites in the National Atmospheric Deposition Program and National Trends Network (NADP/NTN). A duplicate set of wet-deposition sampling instruments was installed adjacent to existing sampling instruments at four different NADP/NTN sites for each year of the study. Wet-deposition samples from collocated sites were collected and analysed using standard NADP/NTN procedures. Laboratory analyses included determinations of pH, specific conductance, and concentrations of major cations and anions. The estimates of precision included all variability in the data-collection system, from the point of sample collection through storage in the NADP/NTN database. Sampling precision was determined from the absolute value of differences in the analytical results for the paired samples in terms of median relative and absolute difference. The median relative difference for Mg2+, Na+, K+ and NH4+ concentration and deposition was quite variable between sites and exceeded 10% at most sites. Relative error for analytes whose concentrations typically approached laboratory method detection limits were greater than for analytes that did not typically approach detection limits. The median relative difference for SO42- and NO3- concentration, specific conductance, and sample volume at all sites was less than 7%. Precision for H+ concentration and deposition ranged from less than 10% at sites with typically high levels of H+ concentration to greater than 30% at sites with low H+ concentration. Median difference for analyte concentration and deposition was typically 1.5-2-times greater for samples collected during the winter than during other seasons at two northern sites. Likewise, the median relative difference in sample volume for winter samples was more than double the annual median relative difference at the two northern sites. Bias accounted for less than 25% of the collocated variability in analyte concentration and deposition from weekly collocated precipitation samples at most sites.A collocated, wet-deposition sampler program has been operated since OCtober 1988 by the U.S Geological Survey to estimate the overall sampling precision of wet atmospheric deposition data collected at selected sites in the National Atmospheric Deposition Program and National Trends Network (NADP/NTN). A duplicate set of wet-deposition sampling instruments was installed adjacent to existing sampling instruments four different NADP/NTN sites for each year of the study. Wet-deposition samples from collocated sites were collected and analysed using standard NADP/NTN procedures. Laboratory analyses included determinations of pH, specific conductance, and concentrations of major cations and anions. The estimates of precision included all variability in the data-collection system, from the point of sample collection through storage in the NADP/NTN database.

Fast Cooling and Vitrification of Aqueous Solutions for Cryopreservation

NASA Astrophysics Data System (ADS)

Warkentin, Matt; Husseini, Naji; Berejnov, Viatcheslav; Thorne, Robert

2006-03-01

In many applications, a small volume of aqueous solution must be cooled at a rate sufficient to produce amorphous solid water. Two prominent examples include flash-freezing of protein crystals for X-ray data collection and freezing of cells (i.e. spermatozoa) for cryopreservation. The cooling rate required to vitrify pure water (˜10^6 K/s) is unattainable for volumes that might contain cells or protein crystals, but the required rate can be reduced by adding cryoprotectants. We report the first measurements of the critical concentration required to produce a vitrified sample as a function of the sample's volume, the cryogen into which the sample is plunged, and the temperature of the cryogen, for a wide range of cryoprotectants. These experiments have broad practical consequences for cryopreservation, and provide insight into the physics of glass formation in aqueous systems.

Determination of dissolved aluminum in water samples

USGS Publications Warehouse

Afifi, A.A.

1983-01-01

A technique has been modified for determination of a wide range of concentrations of dissolved aluminum (Al) in water and has been tested. In this technique, aluminum is complexed with 8-hydroxyquinoline at pH 8.3 to minimize interferences, then extracted with methyl isobutyl ketone (MIBK). The extract is analyzed colorimetrically at 395 nm. This technique is used to analyze two forms of monomeric Al, nonlabile (organic complexes) and labile (free, Al, Al sulfate, fluoride and hydroxide complexes). A detection limit 2 ug/L is possible with 25-ml samples and 10-ml extracts. The detection limit can be decreased by increasing the volume of the sample and (or) decreasing the volume of the methyl isobutyl ketone extract. The analytical uncertainty of this method is approximately + or - 5 percent. The standard addition technique provides a recovery test for this technique and ensures precision in samples of low Al concentrations. The average percentage recovery of the added Al plus the amount originally present was 99 percent. Data obtained from analyses of filtered standard solutions indicated that Al is adsorbed on various types of filters. However, the relationship between Al concentrations and adsorption remains linear. A test on standard solutions also indicated that Al is not adsorbed on nitric acid-washed polyethylene and polypropylene bottle wells. (USGS)

Energy dispersive X-ray fluorescence determination of cadmium in uranium matrix using Cd Kα line excited by continuum

NASA Astrophysics Data System (ADS)

Dhara, Sangita; Misra, N. L.; Aggarwal, S. K.; Venugopal, V.

2010-06-01

An energy dispersive X-ray fluorescence method for determination of cadmium (Cd) in uranium (U) matrix using continuum source of excitation was developed. Calibration and sample solutions of cadmium, with and without uranium were prepared by mixing different volumes of standard solutions of cadmium and uranyl nitrate, both prepared in suprapure nitric acid. The concentration of Cd in calibration solutions and samples was in the range of 6 to 90 µg/mL whereas the concentration of Cd with respect to U ranged from 90 to 700 µg/g of U. From the calibration solutions and samples containing uranium, the major matrix uranium was selectively extracted using 30% tri-n-butyl phosphate in dodecane. Fixed volumes (1.5 mL) of aqueous phases thus obtained were taken directly in specially designed in-house fabricated leak proof Perspex sample cells for the energy dispersive X-ray fluorescence measurements and calibration plots were made by plotting Cd Kα intensity against respective Cd concentration. For the calibration solutions not having uranium, the energy dispersive X-ray fluorescence spectra were measured without any extraction and Cd calibration plots were made accordingly. The results obtained showed a precision of 2% (1 σ) and the results deviated from the expected values by < 4% on average.

Sample stacking of fast-moving anions in capillary zone electrophoresis with pH-suppressed electroosmotic flow.

PubMed

Quirino, J P; Terabe, S

1999-07-30

On-line sample concentration of fast moving inorganic anions by large volume sample stacking (LVSS) and field enhanced sample injection (FESI) with a water plug under acidic conditions is presented. Detection sensitivity enhancements were around 100 and 1000-fold for LVSS and FESI, respectively. However, reproducibility and linearity of response in the LVSS approach is superior compared to the FESI approach.

Long-Term Bioeffects of 435MHz Radiofrequency Radiation on Selected Blood-Borne Endpoints in Cannulated Rats. Volume 2. Plasma ACTH (adrenocorticotropic Hormone) and Plasma Corticosterone

DTIC Science & Technology

1987-08-01

B.- and Soutas. Dpmptrio; I 13a. TYPE OF REPORT 13b. TIME COVERED 114. DATE OF REPORT (Year, Month, Day) S. PAGE COUNT Final FROM84/8/20 TO 86/2/16...cages and placed in sampling boxes. At this moment a first 0.2 mL sample of blood was withdrawn. At 0 time (20 min later) another 0.2 mL sample of blood...concentration data scatter diagram (exposure group) ............. . . . . . . . . . . . . . . . 18 10. Mean plasma ACTH concentrations versus time ....... 19

Incidence of enteroviruses in Mamala Bay, Hawaii using cell culture and direct polymerase chain reaction methodologies.

PubMed

Reynolds, K A; Roll, K; Fujioka, R S; Gerba, C P; Pepper, I L

1998-06-01

The consequence of point and nonpoint pollution sources, discharged into marine waters, on public recreational beaches in Mamala Bay, Hawaii was evaluated using virus cell culture and direct reverse transcriptase-polymerase chain reaction (RT-PCR). Twelve sites, nine marine, two freshwater (one stream and one canal), and one sewage, were assessed either quarterly or monthly for 1 year to detect the presence of human enteric viruses. Water samples were concentrated from initial volumes of 400 L to final volumes of 30 mL using Filterite electronegative cartridge filters and a modified beef extract elution procedure. Cell culture was applied using the Buffalo Green Monkey kidney cell line to analyze samples for enteroviruses. Positive samples were also evaluated by RT-PCR, using enterovirus-specific primers. Levels of RT-PCR inhibition varied with each concentrated sample. Resin column purification increased PCR detection sensitivity by at least one order of magnitude in a variety of sewage outfall and recreational marine water samples but not in the freshwater canal samples. Using cell culture, viable enteroviruses were found in 50 and 17% of all outfall and canal samples, respectively. Samples were positive at beaches 8% of the time. These data illustrate the potential public health hazard associated with recreational waters. Using direct PCR, viruses were detected at the outfall but were not found in any beach or canal samples, in part, owing to substances that inhibit PCR. Therefore, conventional cell culture is the most effective means of detecting low levels of infectious enteroviruses in environmental waters, whereas direct RT-PCR is rendered less effective by inhibitory compounds and low equivalent reaction volumes.

Evaluation of two portable meters for determination of blood triglyceride concentration in dogs.

PubMed

Kluger, Elissa K; Dhand, Navneet K; Malik, Richard; Ilkin, William J; Snow, David H; Govendir, Merran

2010-02-01

To evaluate agreement between 2 portable triglyceride meters and a veterinary laboratory for measurement of blood triglyceride concentrations in dogs and evaluate effects of Hct and blood volume analyzed. 97 blood samples collected from 60 dogs. Triglyceride concentrations were measured in blood by use of 2 meters and compared with serum triglyceride concentrations determined by a veterinary laboratory. Within- and between-day precision, accuracy, and effects of blood volume and Hct were analyzed. Accuracy of both meters varied with triglyceride concentration, although both accurately delineated dogs with triglyceride concentrations < 180 mg/dL versus > or = 180 mg/dL. One meter had results with excellent overall correlation with results of the standard laboratory method, with a concordance correlation coefficient of 0.94 and mean difference of 20.3 mg/dL. The other meter had a good overall concordance correlation coefficient of 0.86 with a higher absolute mean difference of -27.7 mg/dL. Results were only affected by blood volume; triglyceride concentrations determined via both meters were significantly lower when 7 microL of EDTA-anticoagulated blood was used, compared with larger volumes. 1 meter had greater accuracy in the range of 140 to 400 mg/dL and was therefore well suited to detect hypertriglyceridemia. The other meter was accurate with triglyceride values < 140 mg/dL and yielded results similar to those of the veterinary laboratory in the range of 140 to 400 mg/dL, therefore being suitable for determination of triglyceride concentrations in nonfed dogs and dogs with mildly high concentrations.

SAN PEDRO PARKS WILDERNESS, NEW MEXICO.

USGS Publications Warehouse

Santos, Elmer S.; Weisner, Robert C.

1984-01-01

The San Pedro Parks Wilderness occupies 62. 7 sq mi of the Santa Fe National Forest in north-central New Mexico. Several copper mines, many copper prospects, and a few uranium prospects occur in sedimentary units in the vicinity of the wilderness. These units, where they extend into the wilderness, constitute only a small volume of rock and, judging from analyses of samples and from field observations, are devoid of copper and uranium concentration. Prospects on several of about 65 mining claims within the wilderness revealed concentrations of manganese or barite but only in volumes too small to be considered a demonstrated resource.

A CFD Analysis of Hydrogen Leakage During On-Pad Purge in the ORION/ARES I Shared Volume

NASA Technical Reports Server (NTRS)

Ajmani, Kumud; Edwards, Daryl A.

2011-01-01

A common open volume is created by the stacking of the Orion vehicle onto the Ares I Upper Stage. Called the Shared Volume, both vehicles contribute to its gas, fluid, and thermal environment. One of these environments is related to hazardous hydrogen gas. While both vehicles use inert purge gas to mitigate any hazardous gas buildup, there are concerns that hydrogen gas may still accumulate and that the Ares I Hazardous Gas Detection System will not be sufficient for monitoring the integrated volume. This Computational Fluid Dynamics (CFD) analysis has been performed to examine these topics. Results of the analysis conclude that the Ares I Hazardous Gas Detection System will be able to sample the vent effluent containing the highest hydrogen concentrations. A second conclusion is that hydrogen does not accumulate under the Orion Service Module (SM) avionics ring as diffusion and purge flow mixing sufficiently dilute the hydrogen to safe concentrations. Finally the hydrogen concentrations within the Orion SM engine nozzle may slightly exceed the 1 percent volume fraction when the entire worse case maximum full leak is directed vertically into the engine nozzle.

Integrated hollow microneedle-optofluidic biosensor for therapeutic drug monitoring in sub-nanoliter volumes

NASA Astrophysics Data System (ADS)

Ranamukhaarachchi, Sahan A.; Padeste, Celestino; Dübner, Matthias; Häfeli, Urs O.; Stoeber, Boris; Cadarso, Victor J.

2016-07-01

Therapeutic drug monitoring (TDM) typically requires painful blood drawn from patients. We propose a painless and minimally-invasive alternative for TDM using hollow microneedles suitable to extract extremely small volumes (<1 nL) of interstitial fluid to measure drug concentrations. The inner lumen of a microneedle is functionalized to be used as a micro-reactor during sample collection to trap and bind target drug candidates during extraction, without requirements of sample transfer. An optofluidic device is integrated with this microneedle to rapidly quantify drug analytes with high sensitivity using a straightforward absorbance scheme. Vancomycin is currently detected by using volumes ranging between 50-100 μL with a limit of detection (LoD) of 1.35 μM. The proposed microneedle-optofluidic biosensor can detect vancomycin with a sample volume of 0.6 nL and a LoD of <100 nM, validating this painless point of care system with significant potential to reduce healthcare costs and patients suffering.

Integrated hollow microneedle-optofluidic biosensor for therapeutic drug monitoring in sub-nanoliter volumes

PubMed Central

Ranamukhaarachchi, Sahan A.; Padeste, Celestino; Dübner, Matthias; Häfeli, Urs O.; Stoeber, Boris; Cadarso, Victor J.

2016-01-01

Therapeutic drug monitoring (TDM) typically requires painful blood drawn from patients. We propose a painless and minimally-invasive alternative for TDM using hollow microneedles suitable to extract extremely small volumes (<1 nL) of interstitial fluid to measure drug concentrations. The inner lumen of a microneedle is functionalized to be used as a micro-reactor during sample collection to trap and bind target drug candidates during extraction, without requirements of sample transfer. An optofluidic device is integrated with this microneedle to rapidly quantify drug analytes with high sensitivity using a straightforward absorbance scheme. Vancomycin is currently detected by using volumes ranging between 50–100 μL with a limit of detection (LoD) of 1.35 μM. The proposed microneedle-optofluidic biosensor can detect vancomycin with a sample volume of 0.6 nL and a LoD of <100 nM, validating this painless point of care system with significant potential to reduce healthcare costs and patients suffering. PMID:27380889

The reciprocal iso-inhibition volume concept: A procedure for the evaluation in effect-directed analysis with thin-layer chromatography - using the thin-layer chromatography-luminescent bacteria assay as an example.

PubMed

Schulz, Wolfgang; Weiss, Stefan C; Weber, Walter H; Winzenbacher, Rudi

2017-10-13

In effect-directed analysis (EDA) with high-performance thin-layer chromatography (HPTLC), the effect is often detected using images. Thus, an approach to create inhibition chromatograms from these images was developed using the example of the HPTLC- bioluminescence inhibition test. A comparison between the cuvette test and the HPTLC test shows that the test on the plate is significantly more sensitive. To describe the strength of the effect, the EC 50 value is determined from the dose-response relationship. However, the inhibiting compounds are generally unknown and thus their concentrations are also unknown. Therefore, instead of the concentration, the known application volumes are used. This enables the calculation of the application volume necessary to achieve 50% inhibition. Since the volume is inversely proportional to the concentration, the reciprocal value of the calculated volume is indicated and is referred to as the reciprocal iso-inhibition volume (RIV). Using this RIV-concept, it is now possible to compare inhibition bands within and between plates. The entire evaluation is described by the means of two samples from a contaminated site using the bioluminescence inhibition. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of nanomolar chromate in drinking water with solid phase extraction and a portable spectrophotometer.

PubMed

Ma, Jian; Yang, Bo; Byrne, Robert H

2012-06-15

Determination of chromate at low concentration levels in drinking water is an important analytical objective for both human health and environmental science. Here we report the use of solid phase extraction (SPE) in combination with a custom-made portable light-emitting diode (LED) spectrophotometer to achieve detection of chromate in the field at nanomolar levels. The measurement chemistry is based on a highly selective reaction between 1,5-diphenylcarbazide (DPC) and chromate under acidic conditions. The Cr-DPC complex formed in the reaction can be extracted on a commercial C18 SPE cartridge. Concentrated Cr-DPC is subsequently eluted with methanol and detected by spectrophotometry. Optimization of analytical conditions involved investigation of reagent compositions and concentrations, eluent type, flow rate (sample loading), sample volume, and stability of the SPE cartridge. Under optimized conditions, detection limits are on the order of 3 nM. Only 50 mL of sample is required for an analysis, and total analysis time is around 10 min. The targeted analytical range of 0-500 nM can be easily extended by changing the sample volume. Compared to previous SPE-based spectrophotometric methods, this analytical procedure offers the benefits of improved sensitivity, reduced sample consumption, shorter analysis time, greater operational convenience, and lower cost. Copyright © 2012 Elsevier B.V. All rights reserved.

Liquid microjunction surface sampling probe fluid dynamics: Characterization and application of an analyte plug formation operational mode

DOE Office of Scientific and Technical Information (OSTI.GOV)

ElNaggar, Mariam S.; Van Berkel, Gary J.

2011-08-10

The recently discovered sample plug formation and injection operational mode of a continuous flow, coaxial tube geometry, liquid microjunction surface sampling probe (LMJ-SSP) (J. Am. Soc. Mass Spectrom, 2011) was further characterized and applied for concentration and mixing of analyte extracted from multiple areas on a surface and for nanoliter-scale chemical reactions of sampled material. A transparent LMJ-SSP was constructed and colored analytes were used so that the surface sampling process, plug formation, and the chemical reactions could be visually monitored at the sampling end of the probe before being analyzed by mass spectrometry of the injected sample plug. Injectionmore » plug peak widths were consistent for plug hold times as long as the 8 minute maximum attempted (RSD below 1.5%). Furthermore, integrated injection peak signals were not significantly different for the range of hold times investigated. The ability to extract and completely mix individual samples within a fixed volume at the sampling end of the probe was demonstrated and a linear mass spectral response to the number of equivalent analyte spots sampled was observed. Lastly, using the color and mass changing chemical reduction of the redox dye 2,6-dichlorophenol-indophenol with ascorbic acid, the ability to sample, concentrate, and efficiently run reactions within the same plug volume within the probe was demonstrated.« less

Monitoring well utility in a heterogeneous DNAPL source zone area: Insights from proximal multilevel sampler wells and sampling capture-zone modelling.

PubMed

McMillan, Lindsay A; Rivett, Michael O; Wealthall, Gary P; Zeeb, Peter; Dumble, Peter

2018-03-01

Groundwater-quality assessment at contaminated sites often involves the use of short-screen (1.5 to 3 m) monitoring wells. However, even over these intervals considerable variation may occur in contaminant concentrations in groundwater adjacent to the well screen. This is especially true in heterogeneous dense non-aqueous phase liquid (DNAPL) source zones, where cm-scale contamination variability may call into question the effectiveness of monitoring wells to deliver representative data. The utility of monitoring wells in such settings is evaluated by reference to high-resolution multilevel sampler (MLS) wells located proximally to short-screen wells, together with sampling capture-zone modelling to explore controls upon well sample provenance and sensitivity to monitoring protocols. Field data are analysed from the highly instrumented SABRE research site that contained an old trichloroethene source zone within a shallow alluvial aquifer at a UK industrial facility. With increased purging, monitoring-well samples tend to a flow-weighted average concentration but may exhibit sensitivity to the implemented protocol and degree of purging. Formation heterogeneity adjacent to the well-screen particularly, alongside pump-intake position and water level, influence this sensitivity. Purging of low volumes is vulnerable to poor reproducibility arising from concentration variability predicted over the initial 1 to 2 screen volumes purged. Marked heterogeneity may also result in limited long-term sample concentration stabilization. Development of bespoke monitoring protocols, that consider screen volumes purged, alongside water-quality indicator parameter stabilization, is recommended to validate and reduce uncertainty when interpreting monitoring-well data within source zone areas. Generalised recommendations on monitoring well based protocols are also developed. A key monitoring well utility is their proportionately greater sample draw from permeable horizons constituting a significant contaminant flux pathway and hence representative fraction of source mass flux. Acquisition of complementary, high-resolution, site monitoring data, however, vitally underpins optimal interpretation of monitoring-well datasets and appropriate advancement of a site conceptual model and remedial implementation. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

40 CFR 91.301 - Scope; applicability.

Code of Federal Regulations, 2010 CFR

2010-07-01

... this part 91. (b) Exhaust gases are sampled while the test engine is operated using a steady state test... analysis determining concentration of pollutant, exhaust volume, the fuel flow, and the power output during...

Electrolyte and Plasma Changes After Ingestion of Pickle Juice, Water, and a Common Carbohydrate-Electrolyte Solution

PubMed Central

Miller, Kevin C.; Mack, Gary; Knight, Kenneth L.

2009-01-01

Abstract Context: Health care professionals advocate that athletes who are susceptible to exercise-associated muscle cramps (EAMCs) should moderately increase their fluid and electrolyte intake by drinking sport drinks. Some clinicians have also claimed drinking small volumes of pickle juice effectively relieves acute EAMCs, often alleviating them within 35 seconds. Others fear ingesting pickle juice will enhance dehydration-induced hypertonicity, thereby prolonging dehydration. Objective: To determine if ingesting small quantities of pickle juice, a carbohydrate-electrolyte (CHO-e) drink, or water increases plasma electrolytes or other selected plasma variables. Design: Crossover study. Setting: Exercise physiology laboratory. Patients or Other Participants: Nine euhydrated, healthy men (age  =  25 ± 2 years, height  =  179.4 ± 7.2 cm, mass  =  86.3 ± 15.9 kg) completed the study. Intervention(s): Resting blood samples were collected preingestion (−0.5 minutes); immediately postingestion (0 minutes); and at 1, 5, 10, 15, 20, 25, 30, 45, and 60 minutes postingestion of 1 mL/kg body mass of pickle juice, CHO-e drink, or tap water. Main Outcome Measure(s): Plasma sodium concentration, plasma magnesium concentration, plasma calcium concentration, plasma potassium concentration, plasma osmolality, and changes in plasma volume were analyzed. Urine specific gravity, osmolality, and volume were also measured to characterize hydration status. Results: Mean fluid intake was 86.3 ± 16.7 mL. Plasma sodium concentration, plasma magnesium concentration, plasma calcium concentration, plasma osmolality, and plasma volume did not change during the 60 minutes after ingestion of each fluid (P ≥ .05). Water ingestion slightly decreased plasma potassium concentration at 60 minutes (0.21 ± 0.14 mg/dL [0.21 ± 0.14 mmol/L]; P ≤ .05). Conclusions: At these volumes, ingestion of pickle juice and CHO-e drink did not cause substantial changes in plasma electrolyte concentrations, plasma osmolality, or plasma volume in rested, euhydrated men. Concern that ingesting these volumes of pickle juice might exacerbate an athlete's risk of dehydration-induced hypertonicity may be unwarranted. If EAMCs are caused by large electrolyte loss due to sweating, these volumes of pickle juice or CHO-e drink are unlikely to restore any deficit incurred by exercise. PMID:19771282

DEVELOPMENT OF ALTERNATE PERFORMANCE STANDARD FOR RADON RESISTANT CONSTRUCTION BASED ON SHORT-TERM/LONG- TERM INDOOR RADON CONCENTRATIONS - VOLUME 2: APPENDICES

EPA Science Inventory

The report gives results of a study of short- and long-term variations in radon concentration in about 80 houses in Florida. The study involves comparative sampling using the most common radon measurement technologies during the past year. he study, providing the most detailed da...

DEVELOPMENT OF ALTERNATE PERFORMANCE STANDARD FOR RADON RESISTANT CONSTRUCTION BASED ON SHORT-TERM/LONG- TERM INDOOR RADON CONCENTRATIONS - VOLUME 1: TECHNICAL REPORT

EPA Science Inventory

The report gives results of a study of short- and long-term variations in radon concentration in about 80 houses in Florida. The study involves comparative sampling using the most common radon measurement technologies during the past year. he study, providing the most detailed da...

Lithography-free nanofluidic concentrator based on droplets-on-demand system

NASA Astrophysics Data System (ADS)

Yu, Miao; Zhou, Hongbo; Yao, Shuhuai

2013-11-01

Biomarkers are usually low-abundance proteins in biofluids and below detection limit of conventional biosensors. Nanofluidic concentration devices allow efficient biomolecules trapping by utilizing ion concentration polarization near nanochannels. However, once the electric field is turned off, the electrokinetic concentration plug cannot maintain its concentration status and starts to diffuse. In order to maintain the high concentration and extract the concentrated sample for further analysis, a good approach is to encapsulate these plugs into water-in-oil droplets. Here we developed a nanofluidic concentrator based on droplet-on-demand generator to encapsulate concentrated sample in nL droplets. The lithography-free nanochannels were patterned by thermal cracking on the surface of PS Petri-dish. The resulting nanochannel arrays were 30 nm in depth. In combination with microchannels on PDMS, the micro-nano hybrid chip was developed. We used FITC solution to demonstrate that the chip significantly increased the sample concentration for more than 100 folds within 5 minutes. By tuning the pulsed pressure imposed by the solenoid valve connected to the concentration channel, the system can generate a desired volume of droplet with a target sample concentration at a prescribed time. This work was supported by the Research Grants Council of Hong Kong under General Research Fund (Grant No. 621110).

Fabrication of graphene/Fe3O4@polythiophene nanocomposite and its application in the magnetic solid-phase extraction of polycyclic aromatic hydrocarbons from environmental water samples.

PubMed

Mehdinia, Ali; Khodaee, Nader; Jabbari, Ali

2015-04-08

Polythiophene (PT) was used as a surface modifier of graphene/Fe3O4 (G/Fe3O4) composite to increase merit of it, and also overcome some limitations and disadvantages of using G/Fe3O4 alone as solid phase extraction (SPE) sorbent. An in-situ chemical polymerization method was employed to prepare G/Fe3O4@PT nanocomposites. Application of this newly designed material in the magnetic SPE (MSPE) of polycyclic aromatic hydrocarbons (PAHs), as model analytes, in the environmental water samples was investigated. The characterization of the hybrid material was performed using transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray analysis, Fourier transform-infrared (FT-IR) spectroscopy and vibrating sample magnetometry. Seven important parameters, affecting the extraction efficiency of PAHs, including: amount of adsorbent, adsorption and desorption times, type and volume of the eluent solvent, initial sample volume and salt content of the sample were evaluated. The optimum extraction conditions were obtained as: 4 min for extraction time, 20 mg for sorbent amount, 100mL for initial sample volume, toluene as desorption solvent, 0.6 mL for desorption solvent volume, 6 min for desorption time and 30% (w/v) for NaCl concentration. Good performance data were obtained at the optimized conditions. Detection limits were in the range of 0.009-0.020 μg L(-1) in the real matrix. The calibration curves were linear over the concentration ranges from 0.03 to 80 μg L(-1) with correlation coefficients (R(2)) between 0.995 and 0.998 for all the analytes. Relative standard deviations were ranged from 4.3 to 6.3%. Appropriate recovery values, in the range of 83-107%, were also obtained for the real sample analysis. Copyright © 2014 Elsevier B.V. All rights reserved.

An on-line pre-concentration system for determination of cadmium in drinking water using FAAS.

PubMed

dos Santos, Walter N L; Costa, Jorge L O; Araujo, Rennan G O; de Jesus, Djane S; Costa, Antônio C S

2006-10-11

In the present paper, a minicolumn of polyurethane foam loaded with 4-(2-pyridylazo)-resorcinol (PAR) is proposed as pre-concentration system for cadmium determination in drinking water samples by flame atomic absorption spectrometry. The optimization step was performed using two-level full factorial design and Doehlert matrix, involving the variables: sampling flow rate, elution concentration, buffer concentration and pH. Using the established experimental conditions in the optimization step of: pH 8.2, sampling flow rate 8.5 mL min(-1), buffer concentration 0.05 mol L(-1) and elution concentration of 1.0 mol L(-1), this system allows the determination of cadmium with detection limit (LD) (3sigma/S) of 20.0 ng L(-1) and quantification limit (LQ) (10sigma/S) of 64 ng L(-1), precision expressed as relative standard deviation (R.S.D.) of 5.0 and 4.7% for cadmium concentration of 5.0 and 40.0 microg L(-1), respectively, and a pre-concentration factor of 158 for a sample volume of 20.0 mL. The accuracy was confirmed by cadmium determination in the standard reference material, NIST SRM 1643d trace elements in natural water. This procedure was applied for cadmium determination in drinking water samples collected from Salvador City, Bahia, Brazil. For five samples analyzed, the achieved concentrations varied from 0.31 to 0.86 microg L(-1).

Good performance of an immunoassay based method for nevirapine measurements in human breast milk.

PubMed

Salado-Rasmussen, Kirsten; Theilgaard, Zahra Persson; Chiduo, Mercy; Pedersen, Court; Gerstoft, Jan; Katzenstein, Terese Lea

2011-07-01

Understanding the distribution of antiretro-virals in breastfeeding HIV-positive mothers is essential, both for prevention of mother-to-child HIV transmission and for research on the development of drug resistance. The ARK nevirapine (NVP)-test is an immunoassay method for nevirapine measurements, developed and validated for plasma use. In this study, the ARK NVP-test was evaluated for measurement of nevirapine concentrations in breast milk. High performance liquid chromatography (HPLC) is the method currently used to determine nevirapine in breast milk. This method, however, requires complicated extraction techniques. The ARK method employs an immunoassay technology and requires a small sample volume (40 μL) and no pre-treatment of the samples. Commercial enzyme and antibody were used and calibration standards and quality controls were prepared from pooled breast milk from HIV-uninfected women. Clinical samples from HIV-infected women receiving a single-dose of nevirapine were analyzed. Precision and accuracy were evaluated with two concentrations of quality control materials analyzed in three replicates on four different days and was <4%, and between 96.5% and 104.6%, respectively. Clinical samples were analyzed and CVs ranged from 0.0% to 11.1%. The median nevirapine concentration in breast milk 1 week post-partum was 0.29 μg/mL (range 0.11-0.90 μg/mL) in women treated with a single-dose of nevirapine. The ease of use and small sample volume makes the ARK assay an attractive alternative to HPLC analyses for determinations of nevirapine concentrations in breast milk.

Inferring Groundwater Age in an Alluvial Aquifer from Tracer Concentrations in the Stream - Little Wind River, Wyoming

NASA Astrophysics Data System (ADS)

Goble, D.; Gardner, W. P.; Naftz, D. L.; Solder, J. E.

2017-12-01

We use environmental tracers: CFC's, SF6, and 222Rn measured in stream water to determine volume and mean age of groundwater discharging to the Little Wind River, near Riverton, Wyoming. Samples of 222Rn were collected every 200 m along a 2 km reach, surrounding a known groundwater discharge zone. Nearby groundwater wells, in-stream piezometers and seepage meters were sampled for 222Rn, CFC's and SF6. Tracer concentrations measured in groundwater and in-stream piezometers were used to estimate the mean age of the subsurface system. High resolution 222Rn samples were used to determine the location and volume of groundwater inflow using a model of instream transport that includes radioactive decay and gas exchange with the atmosphere. The age of groundwater entering the stream was then estimated from in-stream measured CFC and SF6 concentrations using a new coupled stream transport and lumped-parameter groundwater age model. Ages derived from in-stream measurements were then compared to the age of subsurface water measured in piezometers, seepage meters, and groundwater wells. We then asses the ability of groundwater age inferred from in-stream samples to provide constraint on the age of the subsurface discharge to the stream. The ability to asses groundwater age from in-stream samples can provide a convenient method to constrain the regional distribution of groundwater circulation rates when groundwater sampling is challenging or wells are not in place.

A combined application of thermal desorber and gas chromatography to the analysis of gaseous carbonyls with the aid of two internal standards.

PubMed

Kim, Ki-Hyun; Anthwal, A; Pandey, Sudhir Kumar; Kabir, Ehsanul; Sohn, Jong Ryeul

2010-11-01

In this study, a series of GC calibration experiments were conducted to examine the feasibility of the thermal desorption approach for the quantification of five carbonyl compounds (acetaldehyde, propionaldehyde, butyraldehyde, isovaleraldehyde, and valeraldehyde) in conjunction with two internal standard compounds. The gaseous working standards of carbonyls were calibrated with the aid of thermal desorption as a function of standard concentration and of loading volume. The detection properties were then compared against two types of external calibration data sets derived by fixed standard volume and fixed standard concentration approach. According to this comparison, the fixed standard volume-based calibration of carbonyls should be more sensitive and reliable than its fixed standard concentration counterpart. Moreover, the use of internal standard can improve the analytical reliability of aromatics and some carbonyls to a considerable extent. Our preliminary test on real samples, however, indicates that the performance of internal calibration, when tested using samples of varying dilution ranges, can be moderately different from that derivable from standard gases. It thus suggests that the reliability of calibration approaches should be examined carefully with the considerations on the interactive relationships between the compound-specific properties and the operation conditions of the instrumental setups.

The influence of the microbial quality of wastewater, lettuce cultivars and enumeration technique when estimating the microbial contamination of wastewater-irrigated lettuce.

PubMed

Makkaew, P; Miller, M; Cromar, N J; Fallowfield, H J

2017-04-01

This study investigated the volume of wastewater retained on the surface of three different varieties of lettuce, Iceberg, Cos, and Oak leaf, following submersion in wastewater of different microbial qualities (10, 10 2 , 10 3 , and 10 4 E. coli MPN/100 mL) as a surrogate method for estimation of contamination of spray-irrigated lettuce. Uniquely, Escherichia coli was enumerated, after submersion, on both the outer and inner leaves and in a composite sample of lettuce. E. coli were enumerated using two techniques. Firstly, from samples of leaves - the direct method. Secondly, using an indirect method, where the E. coli concentrations were estimated from the volume of wastewater retained by the lettuce and the E. coli concentration of the wastewater. The results showed that different varieties of lettuce retained significantly different volumes of wastewater (p < 0.01). No statistical differences (p > 0.01) were detected between E. coli counts obtained from different parts of lettuce, nor between the direct and indirect enumeration methods. Statistically significant linear relationships were derived relating the E. coli concentration of the wastewater in which the lettuces were submerged to the subsequent E. coli count on each variety the lettuce.

Digital LAMP in a sample self-digitization (SD) chip

PubMed Central

Herrick, Alison M.; Dimov, Ivan K.; Lee, Luke P.; Chiu, Daniel T.

2012-01-01

This paper describes the realization of digital loop-mediated DNA amplification (dLAMP) in a sample self-digitization (SD) chip. Digital DNA amplification has become an attractive technique to quantify absolute concentrations of DNA in a sample. While digital polymerase chain reaction is still the most widespread implementation, its use in resource—limited settings is impeded by the need for thermal cycling and robust temperature control. In such situations, isothermal protocols that can amplify DNA or RNA without thermal cycling are of great interest. Here, we showed the successful amplification of single DNA molecules in a stationary droplet array using isothermal digital loop-mediated DNA amplification. Unlike most (if not all) existing methods for sample discretization, our design allows for automated, loss-less digitization of sample volumes on-chip. We demonstrated accurate quantification of relative and absolute DNA concentrations with sample volumes of less than 2 μl. We assessed the homogeneity of droplet size during sample self-digitization in our device, and verified that the size variation was small enough such that straightforward counting of LAMP-active droplets sufficed for data analysis. We anticipate that the simplicity and robustness of our SD chip make it attractive as an inexpensive and easy-to-operate device for DNA amplification, for example in point-of-care settings. PMID:22399016

Solid-phase extraction and separation procedure for trace aluminum in water samples and its determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS).

PubMed

Ciftci, Harun; Er, Cigdem

2013-03-01

In the present study, a separation/preconcentration procedure for determination of aluminum in water samples has been developed by using a new atomic absorption spectrometer concept with a high-intensity xenon short-arc lamp as continuum radiation source, a high-resolution double-echelle monochromator, and a charge-coupled device array detector. Sample solution pH, sample volume, flow rate of sample solution, volume, and concentration of eluent for solid-phase extraction of Al chelates with 4-[(dicyanomethyl)diazenyl] benzoic acid on polymeric resin (Duolite XAD-761) have been investigated. The adsorbed aluminum on resin was eluted with 5 mL of 2 mol L(-1) HNO(3) and its concentration was determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimal conditions, limit of detection obtained with HR-CS FAAS and Line Source FAAS (LS-FAAS) were 0.49 μg L(-1) and 3.91 μg L(-1), respectively. The accuracy of the procedure was confirmed by analyzing certified materials (NIST SRM 1643e, Trace elements in water) and spiked real samples. The developed procedure was successfully applied to water samples.

Method and apparatus for analyzing the internal chemistry and compositional variations of materials and devices

DOEpatents

Kazmerski, Lawrence L.

1989-01-01

A method and apparatus is disclosed for obtaining and mapping chemical compositional data for solid devices. It includes a SIMS mass analyzer or similar system capable of being rastered over a surface of the solid to sample the material at a pattern of selected points, as the surface is being eroded away by sputtering or a similar process. The data for each point sampled in a volume of the solid is digitally processed and indexed by element or molecule type, exact spacial location within the volume, and the concentration levels of the detected element or molecule types. This data can then be recalled and displayed for any desired planar view in the volume.

Method and apparatus for analyzing the internal chemistry and compositional variations of materials and devices

DOEpatents

Kazmerski, L.L.

1985-04-30

A method and apparatus is disclosed for obtaining and mapping chemical compositional data for solid devices. It includes a SIMS mass analyzer or similar system capable of being rastered over a surface of the solid to sample the material at a pattern of selected points, as the surface is being eroded away by sputtering or a similar process. The data for each point sampled in a volume of the solid is digitally processed and indexed by element or molecule type, exact spacial location within the volume, and the concentration levels of the detected element or molecule types. This data can then be recalled and displayed for any desired planar view in the volume.

An epidemiological survey of children's iodine nutrition and goitre status in regions with mildly excessive iodine in drinking water in Hebei Province, China.

PubMed

Lv, Shengmin; Zhao, Jun; Xu, Dong; Chong, Zhenshui; Chong, Zhengshui; Jia, Lihui; Du, Yonggui; Ma, Jing; Rutherford, Shannon

2012-07-01

To identify children's iodine nutrition and goitre status in areas with mildly excessive iodine in drinking water. A cross-sectional survey. Probability proportional to size sampling was employed to randomly select children from thirty townships where the median iodine content in drinking water ranged from 150 to 300 μg/l; their urinary iodine concentrations were determined and their thyroid volumes were measured by ultrasound. Drinking water samples and salt samples from the villages where the children lived were collected using a systematic sampling method. Hebei Province of China. A total of 1259 children aged 8-10 years (621 boys and 638 girls). Children's median urinary iodine concentration was found to be 418·8 μg/l, and the iodine concentration was >300 μg/l for 68·3 % (248/363) of the urine samples. Children's median urinary iodine concentration in villages with median salt iodine >10 mg/kg was significantly higher than that in villages with median salt iodine <5 mg/kg (442·9 μg/l v. 305·4 μg/l, P ≈ 0). The goitre rate of 1259 children examined by ultrasound was 10·96 %. The iodine intake of children living in areas with mildly excessive iodine in drinking water in Hebei Province was found to be excessive. The measured iodine excess in the sampled children is exacerbated by consumption of iodized salt. Goitre was identified in these areas; however, due to the limitation of the current criteria for children's thyroid volume, a comprehensive assessment of the prevalence of goitre in these regions could not be made and further study is required.

Perilymph sampling from the cochlear apex: a reliable method to obtain higher purity perilymph samples from scala tympani.

PubMed

Salt, Alec N; Hale, Shane A; Plonkte, Stefan K R

2006-05-15

Measurements of drug levels in the fluids of the inner ear are required to establish kinetic parameters and to determine the influence of specific local delivery protocols. For most substances, this requires cochlear fluids samples to be obtained for analysis. When auditory function is of primary interest, the drug level in the perilymph of scala tympani (ST) is most relevant, since drug in this scala has ready access to the auditory sensory cells. In many prior studies, ST perilymph samples have been obtained from the basal turn, either by aspiration through the round window membrane (RWM) or through an opening in the bony wall. A number of studies have demonstrated that such samples are likely to be contaminated with cerebrospinal fluid (CSF). CSF enters the basal turn of ST through the cochlear aqueduct when the bony capsule is perforated or when fluid is aspirated. The degree of sample contamination has, however, not been widely appreciated. Recent studies have shown that perilymph samples taken through the round window membrane are highly contaminated with CSF, with samples greater than 2microL in volume containing more CSF than perilymph. In spite of this knowledge, many groups continue to sample from the base of the cochlea, as it is a well-established method. We have developed an alternative, technically simple method to increase the proportion of ST perilymph in a fluid sample. The sample is taken from the apex of the cochlea, a site that is distant from the cochlear aqueduct. A previous problem with sampling through a perforation in the bone was that the native perilymph rapidly leaked out driven by CSF pressure and was lost to the middle ear space. We therefore developed a procedure to collect all the fluid that emerged from the perforated apex after perforation. We evaluated the method using a marker ion trimethylphenylammonium (TMPA). TMPA was applied to the perilymph of guinea pigs either by RW irrigation or by microinjection into the apical turn. The TMPA concentration of the fluid sample was compared with that measured in perilymph prior to taking the sample using a TMPA-selective microelectrode sealed into ST. Data were interpreted with a finite element model of the cochlear fluids that was used to simulate each aspect of the experiment. The correction of sample concentration back to the perilymph concentration prior to sampling can be performed based on the known ST volume (4.7microL in the guinea pig) and the sample volume. A more precise correction requires some knowledge of the profile of drug distribution along the cochlear prior to sampling. This method of sampling from the apex is technically simple and provides a larger sample volume with a greater proportion of perilymph compared to sampling through the RW.

Perilymph Sampling from the Cochlear Apex: A Reliable Method to Obtain Higher Purity Perilymph Samples from Scala Tympani

PubMed Central

Salt, Alec N.; Hale, Shane A.; Plontke, Stefan K. R.

2006-01-01

Measurements of drug levels in the fluids of the inner ear are required to establish kinetic parameters and to determine the influence of specific local delivery protocols. For most substances, this requires cochlear fluids samples to be obtained for analysis. When auditory function is of primary interest, the drug level in the perilymph of scala tympani (ST) is most relevant, since drug in this scala has ready access to the auditory sensory cells. In many prior studies, ST perilymph samples have been obtained from the basal turn, either by aspiration through the round window membrane (RWM) or through an opening in the bony wall. A number of studies have demonstrated that such samples are likely to be contaminated with cerebrospinal fluid (CSF). CSF enters the basal turn of ST through the cochlear aqueduct when the bony capsule is perforated or when fluid is aspirated. The degree of sample contamination has, however, not been widely appreciated. Recent studies have shown that perilymph samples taken through the round window membrane are highly contaminated with CSF, with samples greater than 2 μL in volume containing more CSF than perilymph. In spite of this knowledge, many groups continue to sample from the base of the cochlea, as it is a well-established method. We have developed an alternative, technically simple method to increase the proportion of ST perilymph in a fluid sample. The sample is taken from the apex of the cochlea, a site that is distant from the cochlear aqueduct. A previous problem with sampling through a perforation in the bone was that the native perilymph rapidly leaked out driven by CSF pressure and was lost to the middle ear space. We therefore developed a procedure to collect all the fluid that emerged from the perforated apex after perforation. We evaluated the method using a marker ion trimethylphenylammonium (TMPA). TMPA was applied to the perilymph of guinea pigs either by RW irrigation or by microinjection into the apical turn. The TMPA concentration of the fluid sample was compared with that measured in perilymph prior to taking the sample using a TMPA-selective microelectrode sealed into ST. Data were interpreted with a finite element model of the cochlear fluids that was used to simulate each aspect of the experiment. The correction of sample concentration back to the perilymph concentration prior to sampling can be performed based on the known ST volume (4.7 μL in the guinea pig) and the sample volume. A more precise correction requires some knowledge of the profile of drug distribution along the cochlear prior to sampling. This method of sampling from the apex is technically simple and provides a larger sample volume with a greater proportion of perilymph compared to sampling through the RW. PMID:16310856

Ion beam promoted lithium absorption in glassy polymeric carbon

NASA Astrophysics Data System (ADS)

Ila, D.; Zimmerman, R. L.; Jenkins, G. M.; Maleki, H.; Poker, D. B.

1995-12-01

Glassy Polymeric Carbon (GPC) samples prepared from a precursor possess accessible pore volume that depends on the heat treatment temperature. We have shown that lithium percolates without diffusion into the accessible pores of GPC samples immersed in a molten lithium salt bath at 700°C. Ion bombardment with 10 MeV Au atoms increases the total pore volume available for lithium occupation even for samples normally impermeable to lithium. The lithium concentration depth profile is measured using Li7(p,2α) nuclear reaction analysis. We will report on lithium percolation into GPC prepared at temperatures between 500°C and 1000°C and activated by a 10 MeV gold ion bombardment.

Environmental and Cultural Impact. Proposed Tennessee Colony Reservoir, Trinity River, Texas. Volume III. Appendices D and E.

DTIC Science & Technology

1972-01-01

daily dissolved oxygen concentration above 5 mg/l, assuming there are normal seasonal and daily variations above this concentration, (2) dissovled oxygen ... Oxygen Concentrations: Surface oxygen determinations were made at each col- lecting station at monthly intervals. Determinations were done using a...Yellow Springs Oxygen Analyzer Model 54. G. Phosphorus and nitrogen determinations : Water samples for chemical analysis were collected at the surface

Analysis of dissolved organic carbon concentration and 13C isotopic signature by TOC-IRMS - assessment of analytical performance

NASA Astrophysics Data System (ADS)

Kirkels, Frédérique; Cerli, Chiara; Federherr, Eugen; Kalbitz, Karsten

2013-04-01

Stable carbon isotopes provide a powerful tool to assess carbon pools and their dynamics. Dissolved organic carbon (DOC) has been recognized to play an important role in ecosystem functioning and carbon cycling and has therefore gained increased research interest. However, direct measurement of 13C isotopic signature of carbon in the dissolved phase is technically challenging particularly using high temperature combustion. Until recently, mainly custom-made systems existed which were modified for coupling of TOC instruments with IRMS for simultaneous assessment of C content and isotopic signature. The variety of coupled systems showed differences in their analytical performances. For analysis of DOC high temperature combustion is recognized as best performing method, owing to its high efficiency of conversion to CO2 also for highly refractory components (e.g. humic, fulvic acids) present in DOC and soil extracts. Therefore, we tested high temperature combustion TOC coupled to IRMS (developed by Elementar Group) for bulk measurements of DOC concentration and 13C signature. The instruments are coupled via an Interface to exchange the carrier gas from O2 to He and to concentrate the derived CO2 for the isotope measurement. Analytical performance of the system was assessed for a variety of organic compounds characterized by different stability and complexity, including humic acid and DOM. We tested injection volumes between 0.2-3 ml, thereby enabling measurement of broad concentration ranges. With an injection volume of 0.5 ml (n=3, preceded by 1 discarded injection), DOC and 13C signatures for concentrations between 5-150 mg C/L were analyzed with high precision (standard deviation (SD) predominantly <0.1‰), good accuracy and linearity (overall SD <0.9‰). For the same settings, slightly higher variation in precision was observed among the lower concentration range and depending upon specific system conditions. Differences in 13C signatures of about 50‰ among samples did not affect the precision of the analysis of natural abundance and labeled samples. Natural DOM, derived from different soils and assessed at various concentrations, was measured with similar good analytical performance, and also tested for the effect of freezing and re-dissolving. We found good performance of TOC-IRMS in comparison with other systems capable of determining C concentration and isotopic signatures. We recognize the advantages of this system providing: - High sample throughput, short measurement time (15 minutes), flexible sample volume - Easy maintenance, handling, rapid sample preparation (no pretreatment) This preliminary assessment highlights wide-ranging opportunities for further research on concentrations and isotopic signatures by TOC-IRMS to elucidate the role of dissolved carbon in terrestrial and aquatic systems.

Cascading and Parallelising Curvilinear Inertial Focusing Systems for High Volume, Wide Size Distribution, Separation and Concentration of Particles

PubMed Central

Miller, B.; Jimenez, M.; Bridle, H.

2016-01-01

Inertial focusing is a microfluidic based separation and concentration technology that has expanded rapidly in the last few years. Throughput is high compared to other microfluidic approaches although sample volumes have typically remained in the millilitre range. Here we present a strategy for achieving rapid high volume processing with stacked and cascaded inertial focusing systems, allowing for separation and concentration of particles with a large size range, demonstrated here from 30 μm–300 μm. The system is based on curved channels, in a novel toroidal configuration and a stack of 20 devices has been shown to operate at 1 L/min. Recirculation allows for efficient removal of large particles whereas a cascading strategy enables sequential removal of particles down to a final stage where the target particle size can be concentrated. The demonstration of curved stacked channels operating in a cascaded manner allows for high throughput applications, potentially replacing filtration in applications such as environmental monitoring, industrial cleaning processes, biomedical and bioprocessing and many more. PMID:27808244

Monitoring of occupational exposure to methylene chloride: sampling protocol and stability of urine samples.

PubMed

Hoffer, Erica; Tabak, Arek; Shcherb, Inna; Wiener, Avi; Bentur, Yedidia

2005-01-01

A sampling protocol for biomonitoring of the volatile solvent methylene chloride (MeCl(2)) by analysis of urine from exposed workers was established. Storage temperature, sample volume in headspace vial (HSV), and time to sealing HSV on determination of MeCl(2) in urine were evaluated. MeCl(2) was analyzed by a solid-phase microextraction technique combined with gas chromatography. Volume of urine in HSV has no effect on MeCl(2) analysis. Delays of 30 and 60 min from collection of urine until sealing the HSV caused 14.47 +/- 6.98% and 26.17 +/- 9.57% decreases from baseline concentration, respectively. MeCl(2) concentration in spiked urine samples stored in sealed HSVs decreased on day 2 and then remained stable for 2 weeks. Refrigeration did not improve recovery although it seems to be associated with less variability. MeCl(2) in urine samples of seven exposed workers was in the range of 0.02-0.06 mg/L. Sampling of MeCl(2)-containing urine should include collection of urine in closed plastic bottles, transfer to HSV within 15 min, sealing and clamping of HSV within 15 s, and storage of HSV in refrigeration until analysis, but no longer than 2 weeks. Standard samples should be prepared on the day of test sample collection and handled under the same conditions.

A simple method to recover Norovirus from fresh produce with large sample size by using histo-blood group antigen-conjugated to magnetic beads in a recirculating affinity magnetic separation system (RCAMS).

PubMed

Tian, Peng; Yang, David; Mandrell, Robert

2011-06-30

Human norovirus (NoV) outbreaks are major food safety concerns. The virus has to be concentrated from food samples in order to be detected. PEG precipitation is the most common method to recover the virus. Recently, histo-blood group antigens (HBGA) have been recognized as receptors for human NoV, and have been utilized as an alternative method to concentrate human NoV for samples up to 40 mL in volume. However, to wash off the virus from contaminated fresh food samples, at least 250 mL of wash volume is required. Recirculating affinity magnetic separation system (RCAMS) has been tried by others to concentrate human NoV from large-volume samples and failed to yield consistent results with the standard procedure of 30 min of recirculation at the default flow rate. Our work here demonstrates that proper recirculation time and flow rate are key factors for success in using the RCAMS. The bead recovery rate was increased from 28% to 47%, 67% and 90% when recirculation times were extended from 30 min to 60 min, 120 min and 180 min, respectively. The kinetics study suggests that at least 120 min recirculation is required to obtain a good recovery of NoV. In addition, different binding and elution conditions were compared for releasing NoV from inoculated lettuce. Phosphate-buffered saline (PBS) and water results in similar efficacy for virus release, but the released virus does not bind to RCAMS effectively unless pH was adjusted to acidic. Either citrate-buffered saline (CBS) wash, or water wash followed by CBS adjustment, resulted in an enhanced recovery of virus. We also demonstrated that the standard curve generated from viral RNA extracted from serially-diluted virus samples is more accurate for quantitative analysis than standard curves generated from serially-diluted plasmid DNA or transcribed-RNA templates, both of which tend to overestimate the concentration power. The efficacy of recovery of NoV from produce using RCAMS was directly compared with that of the PEG method in NoV inoculated lettuce. 40, 4, 0.4, and 0.04 RTU can be detected by both methods. At 0.004 RTU, NoV was detectable in all three samples concentrated by the RCAMS method, while none could be detected by the PEG precipitation method. RCAMS is a simple and rapid method that is more sensitive than conventional methods for recovery of NoV from food samples with a large sample size. In addition, the RTU value detected through RCAMS-processed samples is more biologically relevant. Published by Elsevier B.V.

Using Isotope Ratio Infrared Spectrometer to determine δ13C and δ18O of carbonate samples

NASA Astrophysics Data System (ADS)

Smajgl, Danijela; Stöbener, Nils; Mandic, Magda

2017-04-01

The isotopic composition of calcifying organisms is a key tool for reconstruction past seawater temperature and water chemistry. Therefore stable carbon and oxygen isotopes (δ13C and δ18O) in carbonates have been widely used for reconstruction of paleoenvironments. Precise and accurate determination of isotopic composition of carbon (13C) and oxygen (18O) from carbonate sample with proper referencing and data evaluation algorithm presents a challenge for scientists. Mass spectrometry was the only widely used technique for this kind of analysis, but recent advances make laser based spectroscopy a viable alternative. The Thermo Scientific Delta Ray Isotope Ratio Infrared Spectrometer (IRIS) analyzer with the Universal Reference Interface (URI) Connect is one of those alternatives and with TELEDYNE Cetac ASX-7100 autosampler extends the traditional offerings with a system of high precision and throughput of samples. To establish precision and accuracy of measurements and also to develop optimal sample preparation method for measurements with Delta Ray IRIS and URI Connect, IAEA reference materials were used. Preparation is similar to a Gas Bench II method. Carbonate material is added into the vials, flushed with CO2 free synthetic air and acidified with few droplets of 104% H3PO4. Sample amount used for analysis can be as low as 200 μg. Samples are measured after acidification and equilibration time of one hour at 70°C. The CO2 gas generated by reaction is flushed into the variable volume inside the URI Connect through the Nafion based built-in water trap. For this step, carrier gas (CO2 free air) is used to flush the gas from the vial into the variable volume with a maximum volume of 100 ml. A small amount of the sample is then used for automatic concentration determination present in the variable volume. The Thermo Scientific Qtegra Software automatically adjusts any additional dilution of the sample to achieve the desired concentration (usually 400 ppm) in the analyzer. As part of the workflow, reference gas measurements are regularly measured at the same concentration as the sample to allow for automatic drift and linearity correction. With described sample preparation and measurement method, samples are measured with standard deviation less than 0.1‰ δ13C and δ18O, respectively and accuracy of <0.01‰. The system can measure up to 100 samples per day. Equivalent of about 80 µg of pure CO2 gas is needed to complete an analysis. Due to it's small weight and robustness, sample analysis can be performed in the field. Applying new technology of Isotope Ratio Infrared Spectrometers in environmental and paleoenvironmental research can extend the knowledge of complex seawater history and CO2 cycle.

Purge-and-trap ion chromatography for the determination of trace ammonium ion in high-salinity water samples.

PubMed

Wang, Po-Yen; Wu, Jing-Yi; Chen, Hung-Jhen; Lin, Tzung-Yi; Wu, Chien-Hou

2008-04-25

It has always been assumed that purge-and-trap (P&T) method is only used for the analysis of volatile organic compounds (VOCs) in aqueous samples. In this paper, a novel P&T preconcentrator has been developed for the determination of trace amounts of ammonium ion in high-salinity water samples by ion chromatography (IC). Method performance is evaluated as a function of concentration of assistant purging material, purging time, and flow rate. Under the optimum P&T conditions with the purified nitrogen gas at flow rate 40 mL/min for 15.0 min at 40 degrees C, the overall collection efficiency is independent of the concentration of ammonium over the range 1.2-5.9 microM. The enrichment factor (EF) of ammonium correlates the ratio of the sample volume to the acceptor solution volume in the trap vessel, providing potentially unlimited increase of the ammonium signal. Our results indicate that environmental samples with low levels of ammonium in matrices with high concentrations of sodium can be easily analyzed and the detection limit down to 75 nM (1.35 ppb) level, corresponding to picomole of ammonia in the injected sample. Calibration graph was constructed with ammonium standards ranging from 0.05 to 6.0 microM and the linearity of the present method was good as suggested by the square of correlation coefficients being better than 0.997. Thus, we have demonstrated that the P&T-IC method allows the routine determination of ammonium ion in seawater samples without cation interferences.

Chemical Method of Urine Volume Measurement

NASA Technical Reports Server (NTRS)

Petrack, P.

1967-01-01

A system has been developed and qualified as flight hardware for the measurement of micturition volumes voided by crewmen during Gemini missions. This Chemical Urine Volume Measurement System (CUVMS) is used for obtaining samples of each micturition for post-flight volume determination and laboratory analysis for chemical constituents of physiological interest. The system is versatile with respect to volumes measured, with a capacity beyond the largest micturition expected to be encountered, and with respect to mission duration of inherently indefinite length. The urine sample is used for the measurement of total micturition volume by a tracer dilution technique, in which a fixed, predetermined amount of tritiated water is introduced and mixed into the voided urine, and the resulting concentration of the tracer in the sample is determined with a liquid scintillation spectrometer. The tracer employed does not interfere with the analysis for the chemical constituents of the urine. The CUVMS hardware consists of a four-way selector valve in which an automatically operated tracer metering pump is incorporated, a collection/mixing bag, and tracer storage accumulators. The assembled system interfaces with a urine receiver at the selector valve inlet, sample bags which connect to the side of the selector valve, and a flexible hose which carries the excess urine to the overboard drain connection. Results of testing have demonstrated system volume measurement accuracy within the specification limits of +/-5%, and operating reliability suitable for system use aboard the GT-7 mission, in which it was first used.

Evaluation of National Atmospheric Deposition Program measurements for co-located Sites CO89 and CO98 at Rocky Mountain National Park, 2012

USGS Publications Warehouse

,

2013-01-01

Median weekly absolute percent differences for selected parameters including: sample volume, 8.0 percent; ammonium concentration, 9.1 percent; nitrate concentration, 8.5 percent; sulfate concentration, 10.2 percent. Annual precipitation-weighted mean concentrations were higher for CO98 compared to CO89 for all analytes. The chemical concentration record for CO98 contains more valid samples than the CO89 record. Therefore, the CO98 record is more representative of 2012 total annual deposition at Loch Vale. Daily precipitation-depth records for the co-located precipitation gages were 100 percent complete, and the total annual precipitation depths between the sites differed by 0.1 percent for the year (91.5 and 91.4 cm).

Application of a Receptor-Binding Capture Quantitative Reverse Transcription-PCR Assay To Concentrate Human Norovirus from Sewage and To Study the Distribution and Stability of the Virus

PubMed Central

Yang, David; Pan, Liangwen; Mandrell, Robert

2012-01-01

Water is an important route for human norovirus (HuNoV) transmission. Using magnetic beads conjugated with blood group-like antigens (HuNoV receptors), we developed a simple and rapid receptor-binding capture and magnetic sequestration (RBCMS) method and compared it to the existing negatively charged membrane absorption/elution (NCMAE) method for concentrating HuNoV from sewage effluent. RBCMS required 6-fold-less sample volume than the NCMAE method and also resulted in a significantly higher yield of HuNoV. The NCMAE and RBCMS concentrations of genogroup I (GI) HuNoV measured by quantitative reverse transcription-PCR (qRT-PCR) resulted in average threshold cycle (CT) values of 34.68 (8.68 copies, 252-fold concentration) versus 34.07 (13.05 copies, 477-fold concentration), respectively; the NCMAE and RBCMS concentrations of genogroup II (GII) HuNoV were measured as average CT values of 33.32 (24.7 copies, 239-fold concentration) versus 32.38 (46.9 copies, 333-fold concentration), respectively. The specificity of qRT-PCR was confirmed by traditional RT-PCR and an RNase I protection assay. The qRT-PCR signal from RBCMS-concentrated HuNoV treated with RNase I indicated that it was from encapsidated RNA and, probably, viable virus. In contrast, the qRT-PCR signal from NCMAE-concentrated HuNoV was not protected from RNase I and, likely, degradation. Both GI and GII HuNoV were detected from sewage effluent samples collected between April and July with average concentrations of 7.8 × 103 genomic copies per liter (gc/liter) and 4.3 × 104 gc/liter, respectively. No GI and <2% GII HuNoV were detected in sewage samples stored at room temperature for 4 weeks. We conclude that RBCMS requires less sample volume, has better recovery and sensitivity, and is faster than NCMAE for detection of HuNoV in sewage. PMID:22101044

Determination of Se in biological samples by axial view inductively coupled plasma optical emission spectrometry after digestion with aqua regia and on-line chemical vapor generation

NASA Astrophysics Data System (ADS)

dos Santos, Éder José; Herrmann, Amanda Beatriz; de Caires, Suzete Kulik; Frescura, Vera Lúcia Azzolin; Curtius, Adilson José

2009-06-01

A simple and fast method for the determination of Se in biological samples, including food, by axial view inductively coupled plasma optical emission spectrometry using on-line chemical vapor generation (CVG-ICP OES) is proposed. The concentrations of HCl and NaBH 4, used in the chemical vapor generation were optimized by factorial analysis. Six certified materials (non-fat milk powder, lobster hepatopancreas, human hair, whole egg powder, oyster tissue, and lyophilised pig kidney) were treated with 10 mL of aqua regia in a microwave system under reflux for 15 min followed by additional 15 min in an ultrasonic bath. The solutions were transferred to a 100 mL volumetric flask and the final volume was made up with water. The Se was determined directly in these solutions by CVG-ICP OES, using the analytical line at 196.026 nm. Calibration against aqueous standards in 10% v/v aqua regia in the concentration range of 0.5-10.0 µg L - 1 Se(IV) was used for the analysis. The quantification limit, considering a 0.5 g sample weight in a final volume of 100 mL - 1 was 0.10 µg g - 1. The obtained concentration values were in agreement with the total certified concentrations, according to the t-test for a 95% confidence level.

Sequential injection spectrophotometric determination of oxybenzone in lipsticks.

PubMed

Salvador, A; Chisvert, A; Camarasa, A; Pascual-Martí, M C; March, J G

2001-08-01

A sequential injection (SI) procedure for the spectrophotometric determination of oxybenzone in lipsticks is reported. The colorimetric reaction between nickel and oxybenzone was used. SI parameters such as sample solution volume, reagent solution volume, propulsion flow rate and reaction coil length were studied. The limit of detection was 3 microg ml(-1). The sensitivity was 0.0108+/-0.0002 ml microg(-1). The relative standard deviations of the results were between 6 and 12%. The real concentrations of samples and the values obtained by HPLC were comparable. Microwave sample pre-treatment allowed the extraction of oxybenzone with ethanol, thus avoiding the use of toxic organic solvents. Ethanol was also used as carrier in the SI system. Seventy-two injections per hour can be performed, which means a sample frequency of 24 h(-1) if three replicates are measured for each sample.

40 CFR 63.1426 - Process vent requirements for determining organic HAP concentration, control efficiency, and...

Code of Federal Regulations, 2010 CFR

2010-07-01

... percent reduction may be measured as total epoxide, total organic HAP, or as TOC minus methane and ethane... TOC (minus methane and ethane) concentrations in all process vent streams and primary and secondary... million by volume total epoxide or TOC limit in § 63.1425(b)(1)(ii) or (b)(2)(iii), the sampling site...

The role of phytoplankton composition, biomass and cell volume in accumulation and transfer of endocrine disrupting compounds in the Southern Baltic Sea (The Gulf of Gdansk).

PubMed

Staniszewska, Marta; Nehring, Iga; Zgrundo, Aleksandra

2015-12-01

Endocrine disrupting compounds (EDCs) like bisphenol A (BPA), 4-tert-octylphenol (OP) and 4-nonylphenol (NP) are introduced to the trophic webs through among others phytoplankton. This paper describes BPA, OP and NP concentrations in phytoplankton in the Gulf of Gdansk (Southern Baltic Sea) in the years 2011-2012. The assays of BPA, OP and NP in samples were performed using HPLC with fluorescence detection. The concentrations of BPA, the most commonly used of the three compounds, were over ten times higher than OP and NP concentrations. The concentrations of the studied EDCs in phytoplankton from the Gulf of Gdansk depended on anthropogenic factors and on phytoplankton properties (species composition, biomass, volume). An increase in phytoplankton biomass did not always result in an increase of BPA, OP and NP concentrations. However, the load of the studied EDCs accumulated in phytoplankton biomass increase with a rise of biomass. An increase in BPA, OP and NP concentrations was effected by biomass growth and the proportions ofciliates, dinoflagellates, diatoms and green algae. A strong positive correlation between OP and NP concentrations and negative correlation between BPA concentrations and biomass of organisms with cells measuring <1000 μm(3) in volume results from the differing properties of these compounds. Copyright © 2015 Elsevier Ltd. All rights reserved.

In vivo quantification of chromophore concentration using fluorescence differential path length spectroscopy

NASA Astrophysics Data System (ADS)

Kruijt, Bastiaan; Kascakova, Slavka; de Bruijn, Henriette S.; van der Ploeg-van den Heuvel, Angelique; Sterenborg, Henricus J. C. M.; Robinson, Dominic J.; Amelink, Arjen

2009-05-01

We present an optical method based on fluorescence spectroscopy for measuring chromophore concentrations in vivo. Fluorescence differential path length spectroscopy (FPDS) determines chromophore concentration based on the fluorescence intensity corrected for absorption. The concentration of the photosensitizer m-THPC (Foscan®) was studied in vivo in normal rat liver, which is highly vascularized and therefore highly absorbing. Concentration estimates of m-THPC measured by FDPS on the liver are compared with chemical extraction. Twenty-five rats were injected with 0.3 mg/kg m-THPC. In vivo optical concentration measurements were performed on tissue 3, 24, 48, and 96 h after m-THPC administration to yield a 10-fold variation in tissue concentration. After the optical measurements, the liver was harvested for chemical extraction. FDPS showed good correlation with chemical extraction. FDPS also showed a correlation between m-THPC fluorescence and blood volume fraction at the two shortest drug-light intervals. This suggests different compartmental localization of m-THPC for different drug-light intervals that can be resolved using fluorescence spectroscopy. Differences in measured m-THPC concentration between FDPS and chemical extraction are related to the interrogation volume of each technique; ~0.2 mm3 and ~102 mm3, respectively. This indicates intra-animal variation in m-THPC distribution in the liver on the scale of the FDPS sampling volume.

Hall and Seebeck measurements estimate the thickness of a (buried) carrier system: Identifying interface electrons in In-doped SnO{sub 2} films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Papadogianni, Alexandra; Bierwagen, Oliver; White, Mark E.

2015-12-21

We propose a simple method based on the combination of Hall and Seebeck measurements to estimate the thickness of a carrier system within a semiconductor film. As an example, this method can distinguish “bulk” carriers, with homogeneous depth distribution, from “sheet” carriers, that are accumulated within a thin layer. The thickness of the carrier system is calculated as the ratio of the integral sheet carrier concentration, extracted from Hall measurements, to the volume carrier concentration, derived from the measured Seebeck coefficient of the same sample. For rutile SnO{sub 2}, the necessary relation of Seebeck coefficient to volume electron concentration inmore » the range of 3 × 10{sup 17} to 3 × 10{sup 20 }cm{sup −3} has been experimentally obtained from a set of single crystalline thin films doped with varying Sb-doping concentrations and unintentionally doped bulk samples, and is given as a “calibration curve.” Using this calibration curve, our method demonstrates the presence of interface electrons in homogeneously deep-acceptor (In) doped SnO{sub 2} films on sapphire substrates.« less

Alginate Hydrogel Microencapsulation Inhibits Devitrification and Enables Large-Volume Low-CPA Cell Vitrification

PubMed Central

Huang, Haishui; Choi, Jung Kyu; Rao, Wei; Zhao, Shuting; Agarwal, Pranay; Zhao, Gang

2015-01-01

Cryopreservation of stem cells is important to meet their ever-increasing demand by the burgeoning cell-based medicine. The conventional slow freezing for stem cell cryopreservation suffers from inevitable cell injury associated with ice formation and the vitrification (i.e., no visible ice formation) approach is emerging as a new strategy for cell cryopreservation. A major challenge to cell vitrification is intracellular ice formation (IIF, a lethal event to cells) induced by devitrification (i.e., formation of visible ice in previously vitrified solution) during warming the vitrified cells at cryogenic temperature back to super-zero temperatures. Consequently, high and toxic concentrations of penetrating cryoprotectants (i.e., high CPAs, up to ~8 M) and/or limited sample volumes (up to ~2.5 μl) have been used to minimize IIF during vitrification. We reveal that alginate hydrogel microencapsulation can effectively inhibit devitrification during warming. Our data show that if ice formation were minimized during cooling, IIF is negligible in alginate hydrogel-microencapsulated cells during the entire cooling and warming procedure of vitrification. This enables vitrification of pluripotent and multipotent stem cells with up to ~4 times lower concentration of penetrating CPAs (up to 2 M, low CPA) in up to ~100 times larger sample volume (up to ~250 μl, large volume). PMID:26640426

Alginate Hydrogel Microencapsulation Inhibits Devitrification and Enables Large-Volume Low-CPA Cell Vitrification.

PubMed

Huang, Haishui; Choi, Jung Kyu; Rao, Wei; Zhao, Shuting; Agarwal, Pranay; Zhao, Gang; He, Xiaoming

2015-11-25

Cryopreservation of stem cells is important to meet their ever-increasing demand by the burgeoning cell-based medicine. The conventional slow freezing for stem cell cryopreservation suffers from inevitable cell injury associated with ice formation and the vitrification ( i.e. , no visible ice formation) approach is emerging as a new strategy for cell cryopreservation. A major challenge to cell vitrification is intracellular ice formation (IIF, a lethal event to cells) induced by devitrification ( i.e. , formation of visible ice in previously vitrified solution) during warming the vitrified cells at cryogenic temperature back to super-zero temperatures. Consequently, high and toxic concentrations of penetrating cryoprotectants ( i.e. , high CPAs, up to ~8 M) and/or limited sample volumes (up to ~2.5 μl) have been used to minimize IIF during vitrification. We reveal that alginate hydrogel microencapsulation can effectively inhibit devitrification during warming. Our data show that if ice formation were minimized during cooling, IIF is negligible in alginate hydrogel-microencapsulated cells during the entire cooling and warming procedure of vitrification. This enables vitrification of pluripotent and multipotent stem cells with up to ~4 times lower concentration of penetrating CPAs (up to 2 M, low CPA) in up to ~100 times larger sample volume (up to ~250 μl, large volume).

Defect evolution and impurity migration in Na-implanted ZnO

NASA Astrophysics Data System (ADS)

Neuvonen, Pekka T.; Vines, Lasse; Venkatachalapathy, Vishnukanthan; Zubiaga, Asier; Tuomisto, Filip; Hallén, Anders; Svensson, Bengt G.; Kuznetsov, Andrej Yu.

2011-11-01

Secondary ion mass spectrometry (SIMS) and positron annihilation spectroscopy (PAS) have been applied to study impurity migration and open volume defect evolution in Na+ implanted hydrothermally grown ZnO samples. In contrast to most other elements, the presence of Na tends to decrease the concentration of open volume defects upon annealing and for temperatures above 600∘C, Na exhibits trap-limited diffusion correlating with the concentration of Li. A dominating trap for the migrating Na atoms is most likely Li residing on Zn site, but a systematic analysis of the data suggests that zinc vacancies also play an important role in the trapping process.

Assessing Stress Responses in Beaked and Sperm Whales in the Bahamas

DTIC Science & Technology

2012-09-30

acceptable extraction efficiency for steroids (Hayward et al. 2010; Wasser et al. 2010). The"small sample size" effect on hormone concentration was...efficiency ( Wasser pers. comm., Hunt et al. unpub. data). 4) Pilot test of hormone content in seawater removed from samples. The large volume of...2006), and Wasser et al. (2010), with extraction modifications discussed above. RESULTS Sample processing Using a consistent fecal:solvent

Nanopore sensing at ultra-low concentrations using single-molecule dielectrophoretic trapping

PubMed Central

Freedman, Kevin J.; Otto, Lauren M.; Ivanov, Aleksandar P.; Barik, Avijit; Oh, Sang-Hyun; Edel, Joshua B.

2016-01-01

Single-molecule techniques are being developed with the exciting prospect of revolutionizing the healthcare industry by generating vast amounts of genetic and proteomic data. One exceptionally promising route is in the use of nanopore sensors. However, a well-known complexity is that detection and capture is predominantly diffusion limited. This problem is compounded when taking into account the capture volume of a nanopore, typically 108–1010 times smaller than the sample volume. To rectify this disproportionate ratio, we demonstrate a simple, yet powerful, method based on coupling single-molecule dielectrophoretic trapping to nanopore sensing. We show that DNA can be captured from a controllable, but typically much larger, volume and concentrated at the tip of a metallic nanopore. This enables the detection of single molecules at concentrations as low as 5 fM, which is approximately a 103 reduction in the limit of detection compared with existing methods, while still maintaining efficient throughput. PMID:26732171

Customization of Advia 120 thresholds for canine erythrocyte volume and hemoglobin concentration, and effects on morphology flagging results.

PubMed

Grimes, Carolyn N; Fry, Michael M

2014-12-01

This study sought to develop customized morphology flagging thresholds for canine erythrocyte volume and hemoglobin concentration [Hgb] on the ADVIA 120 hematology analyzer; compare automated morphology flagging with results of microscopic blood smear evaluation; and examine effects of customized thresholds on morphology flagging results. Customized thresholds were determined using data from 52 clinically healthy dogs. Blood smear evaluation and automated morphology flagging results were correlated with mean cell volume (MCV) and cellular hemoglobin concentration mean (CHCM) in 26 dogs. Customized thresholds were applied retroactively to complete blood (cell) count (CBC) data from 5 groups of dogs, including a reference sample group, clinical cases, and animals with experimentally induced iron deficiency anemia. Automated morphology flagging correlated more highly with MCV or CHCM than did blood smear evaluation; correlation with MCV was highest using customized thresholds. Customized morphology flagging thresholds resulted in more sensitive detection of microcytosis, macrocytosis, and hypochromasia than default thresholds.

Determination of phenylurea herbicides in water samples using online sorptive preconcentration and high-performance liquid chromatography with UV or electrospray mass spectrometric detection.

PubMed

Baltussen, E; Snijders, H; Janssen, H G; Sandra, P; Cramers, C A

1998-04-10

A recently developed method for the extraction of organic micropollutants from aqueous samples based on sorptive enrichment in columns packed with 100% polydimethylsiloxane (PDMS) particles was coupled on-line with HPLC analysis. The sorptive enrichment procedure originally developed for relatively nonpolar analytes was used to preconcentrate polar phenylurea herbicides from aqueous samples. PDMS extraction columns of 5, 10 and 25 cm were used to extract the herbicides from distilled, tap and river water samples. A model that allows prediction of retention and breakthrough volumes is presented. Despite the essentially apolar nature of the PDMS material, it is possible to concentrate sample volumes up to 10 ml on PDMS cartridges without losses of the most polar analyte under investigation, fenuron. For less polar analytes significantly larger sample volumes can be applied. Since standard UV detection does not provide adequate selectivity for river water samples, an electrospray (ES)-MS instrument was used to determine phenylurea herbicides in a water sample from the river Dommel. Methoxuron was present at a level of 80 ng/l. The detection limit of the current set-up, using 10 ml water samples and ES-MS detection is 10 ng/l in river water samples. Strategies for further improvement of the detection limits are identified.

EPA Method 1615. Measurement of Enterovirus and Norovirus Occurrence in Water by Culture and RT-qPCR. I. Collection of Virus Samples

PubMed Central

Fout, G. Shay; Cashdollar, Jennifer L.; Varughese, Eunice A.; Parshionikar, Sandhya U.; Grimm, Ann C.

2015-01-01

EPA Method 1615 was developed with a goal of providing a standard method for measuring enteroviruses and noroviruses in environmental and drinking waters. The standardized sampling component of the method concentrates viruses that may be present in water by passage of a minimum specified volume of water through an electropositive cartridge filter. The minimum specified volumes for surface and finished/ground water are 300 L and 1,500 L, respectively. A major method limitation is the tendency for the filters to clog before meeting the sample volume requirement. Studies using two different, but equivalent, cartridge filter options showed that filter clogging was a problem with 10% of the samples with one of the filter types compared to 6% with the other filter type. Clogging tends to increase with turbidity, but cannot be predicted based on turbidity measurements only. From a cost standpoint one of the filter options is preferable over the other, but the water quality and experience with the water system to be sampled should be taken into consideration in making filter selections. PMID:25867928

Measuring and Modeling Xenon Uptake in Plastic Beta-Cells

NASA Astrophysics Data System (ADS)

Suarez, R.; Hayes, J. C.; Harper, W. W.; Humble, P.; Ripplinger, M. D.; Stephenson, D. E.; Williams, R. M.

2013-12-01

The precision of the stable xenon volume measurement in atmospheric monitoring radio-xenon systems is a critical parameter used to determine the activity concentration of a radio-xenon sample. Typically these types of systems use a plastic scintillating beta-cell as part of a beta-gamma detection scheme to measure the radioactivity present in the gas sample. Challenges arise when performing the stable xenon calculation during or after radioactive counting of the sample due to xenon uptake into the plastic beta-cells. Plastic beta cells can adsorb as much as 5% of the sample during counting. If quantification is performed after counting, the uptake of xenon into the plastic results in an underestimation of the xenon volume measurement. This behavior also causes what is typically known as 'memory effect' in the cell. Experiments were conducted using a small volume low pressure range thermal conductivity sensor to quantify the amount of xenon uptake into the cell over a given period of time. Understanding the xenon uptake in the cell provides a better estimate of the stable volume which improves the overall measurement capability of the system. The results from these experiments along with modeling will be presented.

Uncertainty Estimation for the Determination of Ni, Pb and Al in Natural Water Samples by SPE-ICP-OES

NASA Astrophysics Data System (ADS)

Ghorbani, A.; Farahani, M. Mahmoodi; Rabbani, M.; Aflaki, F.; Waqifhosain, Syed

2008-01-01

In this paper we propose uncertainty estimation for the analytical results we obtained from determination of Ni, Pb and Al by solidphase extraction and inductively coupled plasma optical emission spectrometry (SPE-ICP-OES). The procedure is based on the retention of analytes in the form of 8-hydroxyquinoline (8-HQ) complexes on a mini column of XAD-4 resin and subsequent elution with nitric acid. The influence of various analytical parameters including the amount of solid phase, pH, elution factors (concentration and volume of eluting solution), volume of sample solution, and amount of ligand on the extraction efficiency of analytes was investigated. To estimate the uncertainty of analytical result obtained, we propose assessing trueness by employing spiked sample. Two types of bias are calculated in the assessment of trueness: a proportional bias and a constant bias. We applied Nested design for calculating proportional bias and Youden method to calculate the constant bias. The results we obtained for proportional bias are calculated from spiked samples. In this case, the concentration found is plotted against the concentration added and the slop of standard addition curve is an estimate of the method recovery. Estimated method of average recovery in Karaj river water is: (1.004±0.0085) for Ni, (0.999±0.010) for Pb and (0.987±0.008) for Al.

Comparative analyses of semen and endocrine characteristics of free-living versus captive jaguars (Panthera onca).

PubMed

Morato, R G; Conforti, V A; Azevedo, F C; Jacomo, A T; Silveira, L; Sana, D; Nunes, A L; Guimarães, M A; Barnabe, R C

2001-11-01

Semen and blood samples were obtained from free-living (n = 6) and captive (n = 8) jaguars (Panthera onca) to compare reproductive characteristics between the two populations. Semen samples were analysed for volume (ml), percentage of motile spermatozoa, rate of forward progression (0-5), concentration (10(6) ml(-1)), total sperm count (10(6)) and sperm morphology. Serum testosterone concentration was determined by radioimmunoassay. Although ejaculate volume was greater in captive jaguars (n = 47 samples) than in free-living jaguars (n = 7 samples) (P < 0.05), the free-living jaguars produced more total spermatozoa (59.3 +/- 12.8 versus 152.0 +/- 88.0 x 10(6), respectively; not significant) with better viability and forward progression (2.8 +/- 0.1 versus 3.5 +/- 0.2, respectively; P < 0.05) and more spermatozoa with normal morphology (73.5 +/- 3.9 versus 5.0 +/- 1.1%, respectively; P < 0.05). Serum testosterone concentrations were similar for captive and free-living male jaguars (3.1 +/- 0.7 and 2.1 +/- 0.8 ng ml(-1), respectively). In summary, the data showed that semen may be collected successfully from free-living jaguars and evaluated under field conditions to establish normative reproductive values in this species. The results also indicate that jaguars maintained in zoos show inferior seminal characteristics compared with free-living animals.

Development of a nucleic Acid extraction procedure for simultaneous recovery of DNA and RNA from diverse microbes in water.

PubMed

Hill, Vincent R; Narayanan, Jothikumar; Gallen, Rachel R; Ferdinand, Karen L; Cromeans, Theresa; Vinjé, Jan

2015-05-26

Drinking and environmental water samples contain a diverse array of constituents that can interfere with molecular testing techniques, especially when large volumes of water are concentrated to the small volumes needed for effective molecular analysis. In this study, a suite of enteric viruses, bacteria, and protozoan parasites were seeded into concentrated source water and finished drinking water samples, in order to investigate the relative performance of nucleic acid extraction techniques for molecular testing. Real-time PCR and reverse transcription-PCR crossing threshold (CT) values were used as the metrics for evaluating relative performance. Experimental results were used to develop a guanidinium isothiocyanate-based lysis buffer (UNEX buffer) that enabled effective simultaneous extraction and recovery of DNA and RNA from the suite of study microbes. Procedures for bead beating, nucleic acid purification, and PCR facilitation were also developed and integrated in the protocol. The final lysis buffer and sample preparation procedure was found to be effective for a panel of drinking water and source water concentrates when compared to commercial nucleic acid extraction kits. The UNEX buffer-based extraction protocol enabled PCR detection of six study microbes, in 100 L finished water samples from four drinking water treatment facilities, within three CT values (i.e., within 90% difference) of the reagent-grade water control. The results from this study indicate that this newly formulated lysis buffer and sample preparation procedure can be useful for standardized molecular testing of drinking and environmental waters.

Development of a Nucleic Acid Extraction Procedure for Simultaneous Recovery of DNA and RNA from Diverse Microbes in Water

PubMed Central

Hill, Vincent R.; Narayanan, Jothikumar; Gallen, Rachel R.; Ferdinand, Karen L.; Cromeans, Theresa; Vinjé, Jan

2015-01-01

Drinking and environmental water samples contain a diverse array of constituents that can interfere with molecular testing techniques, especially when large volumes of water are concentrated to the small volumes needed for effective molecular analysis. In this study, a suite of enteric viruses, bacteria, and protozoan parasites were seeded into concentrated source water and finished drinking water samples, in order to investigate the relative performance of nucleic acid extraction techniques for molecular testing. Real-time PCR and reverse transcription-PCR crossing threshold (CT) values were used as the metrics for evaluating relative performance. Experimental results were used to develop a guanidinium isothiocyanate-based lysis buffer (UNEX buffer) that enabled effective simultaneous extraction and recovery of DNA and RNA from the suite of study microbes. Procedures for bead beating, nucleic acid purification, and PCR facilitation were also developed and integrated in the protocol. The final lysis buffer and sample preparation procedure was found to be effective for a panel of drinking water and source water concentrates when compared to commercial nucleic acid extraction kits. The UNEX buffer-based extraction protocol enabled PCR detection of six study microbes, in 100 L finished water samples from four drinking water treatment facilities, within three CT values (i.e., within 90% difference) of the reagent-grade water control. The results from this study indicate that this newly formulated lysis buffer and sample preparation procedure can be useful for standardized molecular testing of drinking and environmental waters. PMID:26016775

Integrated microfluidic systems for sample preparation and detection of respiratory pathogen Bordetella pertussis.

PubMed

de la Rosa, Carlos; Prakash, Ranjit; Tilley, Peter A; Fox, Julie D; Kaler, Karan V i S

2007-01-01

An integrated microfluidic system for combined manipulation, pre-concentration, and lysis of samples containing Bordetella pertussis by dielectrophoresis and electroporation has been developed and implemented. The microfluidic device was able to pre-concentrate the amount of B. pertussis cells present in 200 microl of a B. pertussis suspension stock into a 20 microl volume. The device exhibited optimal sample pre-concentration of 6.7x at a stock value of 10(3) cfu/ml and at a flow rate of 250 microl/h. Electro-disruption experiments showed that on-chip-based electroporation is an effective solution for lysis of B. pertussis cells that is easily integrated with dielectrophoresis assisted pre-concentration procedures. Pulsed voltage applied, number of pulses, and presence of potassium chloride in a B. pertussis suspension showed a reduction in B. pertussis cell viability by electroporation; and transmission electron microscopy confirmed B. pertussis cell disruption by electroporation. Genetic amplification and detection of the pre-concentrated sample employing an integrated chip-based system demonstrated a complete chip approach for pathogen detection.

Relationship between sample volumes and modulus of human vertebral trabecular bone in micro-finite element analysis.

PubMed

Wen, Xin-Xin; Xu, Chao; Zong, Chun-Lin; Feng, Ya-Fei; Ma, Xiang-Yu; Wang, Fa-Qi; Yan, Ya-Bo; Lei, Wei

2016-07-01

Micro-finite element (μFE) models have been widely used to assess the biomechanical properties of trabecular bone. How to choose a proper sample volume of trabecular bone, which could predict the real bone biomechanical properties and reduce the calculation time, was an interesting problem. Therefore, the purpose of this study was to investigate the relationship between different sample volumes and apparent elastic modulus (E) calculated from μFE model. 5 Human lumbar vertebral bodies (L1-L5) were scanned by micro-CT. Cubic concentric samples of different lengths were constructed as the experimental groups and the largest possible volumes of interest (VOI) were constructed as the control group. A direct voxel-to-element approach was used to generate μFE models and steel layers were added to the superior and inferior surface to mimic axial compression tests. A 1% axial strain was prescribed to the top surface of the model to obtain the E values. ANOVA tests were performed to compare the E values from the different VOIs against that of the control group. Nonlinear function curve fitting was performed to study the relationship between volumes and E values. The larger cubic VOI included more nodes and elements, and more CPU times were needed for calculations. E values showed a descending tendency as the length of cubic VOI decreased. When the volume of VOI was smaller than (7.34mm(3)), E values were significantly different from the control group. The fit function showed that E values approached an asymptotic values with increasing length of VOI. Our study demonstrated that apparent elastic modulus calculated from μFE models were affected by the sample volumes. There was a descending tendency of E values as the length of cubic VOI decreased. Sample volume which was not smaller than (7.34mm(3)) was efficient enough and timesaving for the calculation of E. Copyright © 2016 Elsevier Ltd. All rights reserved.

Reducing the risk of fatal and disabling hypoglycaemia: a comparison of arterial blood sampling systems.

PubMed

Brennan, K A; Eapen, G; Turnbull, D

2010-04-01

In 2008, the National Patient Safety Agency (NPSA) published a report after 42 incidents and two deaths where glucose-containing flush solutions were attached to the arterial line. The molar concentration of 5% glucose is 277 mmol litre(-1). Only a tiny amount of sample contamination will lead to an artificially high glucose. As the NPSA sought a solution, a bench model was constructed to compare the performance of three open and three closed arterial line systems in limiting sample contamination. All arterial line systems were set up in a standard manner and pressurized to 300 mm Hg with 5% glucose used as the flush solution. This was connected to the 'radial artery' using an 18 G needle representing the radial cannula. The radial artery was simulated using a wide-bore extension set with 'blood' flow at 60 ml min(-1). Blood was simulated by the addition of red dye to Hartmann's solution. Increasing multiples of arterial line dead space were aspirated and discarded. Blood samples were then obtained and glucose concentration was measured. Significant glucose contamination (3 mmol litre(-1) +/-3.4) was detected in all open arterial line systems up to an aspiration volume of five times the dead space. No samples from the closed systems recorded glucose concentration >1 mmol litre(-1). Recommended minimal discard volumes are inadequate in the presence of glucose as the flush solution and can lead to high blood glucose readings, inappropriate insulin use, and iatrogenic neuroglycopaenia. Our study demonstrates that the closed-loop arterial sampling system could be the universal solution sought by the NPSA.

Determination of uptake kinetics (sampling rates) by lipid-containing semipermeable membrane devices (SPMDs) for polycyclic aromatic hydrocarbons (PAHs) in water

USGS Publications Warehouse

Huckins, J.N.; Petty, J.D.; Orazio, C.E.; Lebo, J.A.; Clark, R.C.; Gibson, V.L.; Gala, W.R.; Echols, K.R.

1999-01-01

The use of lipid-containing semipermeable membrane devices (SPMDs) is becoming commonplace, but very little sampling rate data are available for the estimation of ambient contaminant concentrations from analyte levels in exposed SPMDs. We determined the aqueous sampling rates (R(s)s; expressed as effective volumes of water extracted daily) of the standard (commercially available design) 1-g triolein SPMD for 15 of the priority pollutant (PP) polycyclic aromatic hydrocarbons (PAHs) at multiple temperatures and concentrations. Under the experimental conditions of this study, recovery- corrected R(s) values for PP PAHs ranged from ???1.0 to 8.0 L/d. These values would be expected to be influenced by significant changes (relative to this study) in water temperature, degree of biofouling, and current velocity- turbulence. Included in this paper is a discussion of the effects of temperature and octanol-water partition coefficient (K(ow)); the impacts of biofouling and hydrodynamics are reported separately. Overall, SPMDs responded proportionally to aqueous PAH concentrations; i.e., SPMD R(s) values and SPMD-water concentration factors were independent of aqueous concentrations. Temperature effects (10, 18, and 26 ??C) on Rs values appeared to be complex but were relatively small.The use of lipid-containing semipermeable membrane devices (SPMDs) is becoming commonplace, but very little sampling rate data are available for the estimation of ambient contaminant concentrations from analyte levels in exposed SPMDs. We determined the aqueous sampling rates (Rss; expressed as effective volumes of water extracted daily) of the standard (commercially available design) 1-g triolein SPMD for 15 of the priority pollutant (PP) polycyclic aromatic hydrocarbons (PAHs) at multiple temperatures and concentrations. Under the experimental conditions of this study, recovery-corrected Rs values for PP PAHs ranged from ???1.0 to 8.0 L/d. These values would be expected to be influenced by significant changes (relative to this study) in water temperature, degree of biofouling, and current velocity-turbulence. Included in this paper is a discussion of the effects of temperature and octanol-water partition coefficient (KOW); the impacts of biofouling and hydrodynamics are reported separately. Overall, SPMDs responded proportionally to aqueous PAH concentrations; i.e., SPMD RS values and SPMD-water concentration factors were independent of aqueous concentrations. Temperature effects (10, 18, and 26??C) on RS values appeared to be complex but were relatively small.

Detecting bacteria and Determining Their Susceptibility to Antibiotics by Stochastic Confinement in Nanoliter Droplets using Plug-Based Microfluidics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Boedicker, J.; Li, L; Kline, T

2008-01-01

This article describes plug-based microfluidic technology that enables rapid detection and drug susceptibility screening of bacteria in samples, including complex biological matrices, without pre-incubation. Unlike conventional bacterial culture and detection methods, which rely on incubation of a sample to increase the concentration of bacteria to detectable levels, this method confines individual bacteria into droplets nanoliters in volume. When single cells are confined into plugs of small volume such that the loading is less than one bacterium per plug, the detection time is proportional to plug volume. Confinement increases cell density and allows released molecules to accumulate around the cell, eliminatingmore » the pre-incubation step and reducing the time required to detect the bacteria. We refer to this approach as stochastic confinement. Using the microfluidic hybrid method, this technology was used to determine the antibiogram - or chart of antibiotic sensitivity - of methicillin-resistant Staphylococcus aureus (MRSA) to many antibiotics in a single experiment and to measure the minimal inhibitory concentration (MIC) of the drug cefoxitin (CFX) against this strain. In addition, this technology was used to distinguish between sensitive and resistant strains of S. aureus in samples of human blood plasma. High-throughput microfluidic techniques combined with single-cell measurements also enable multiple tests to be performed simultaneously on a single sample containing bacteria. This technology may provide a method of rapid and effective patient-specific treatment of bacterial infections and could be extended to a variety of applications that require multiple functional tests of bacterial samples on reduced timescales.« less

Clinical evaluation of a miniaturized desktop breath hydrogen analyzer.

PubMed

Duan, L P; Braden, B; Clement, T; Caspary, W F; Lembcke, B

1994-10-01

A small desktop electrochemical H2 analyzer (EC-60-Hydrogen monitor) was compared with a stationary electrochemical H2 monitor (GMI-exhaled Hydrogen monitor). The EC-60-H2 monitor shows a high degree of precision for repetitive (n = 10) measurements of standard hydrogen mixtures (CV 1-8%). The response time for completion of measurement is shorter than that of the GMI-exhaled H2 monitor (37 sec. vs 53 sec.; p < 0.0001), while reset times are almost identical (54 sec. vs 51 sec. n.s). In a clinical setting, breath H2-concentrations measured with the EC-60-H2 monitor and the GMI-exhaled H2 monitor were in excellent agreement with a linear correlation (Y = 1.12X + 1.022, r2 = 0.9617, n = 115). With increasing H2-concentrations the EC-60-H2 monitor required larger sample volumes for maintaining sufficient precision, and sample volumes greater than 200 ml were required with H2-concentrations > 30 ppm. For routine gastrointestinal function testing, the EC-60-H2 monitor is an satisfactory and reliable, easy to use and inexpensive desktop breath hydrogen analyzer, whereas in patients with difficulty in cooperating (children, people with severe pulmonary insufficiency), special care has to be applied to obtain sufficiently large breath samples.

Measurement of activity coefficients of mixtures by head-space gas chromatography: general procedure.

PubMed

Luis, Patricia; Wouters, Christine; Van der Bruggen, Bart; Sandler, Stanley I

2013-08-09

Head-space gas chromatography (HS-GC) is an applicable method to perform vapor-liquid equilibrium measurements and determine activity coefficients. However, the reproducibility of the data may be conditioned by the experimental procedure concerning to the automated pressure-balanced system. The study developed in this work shows that a minimum volume of liquid in the vial is necessary to ensure the reliability of the activity coefficients since it may become a parameter that influences the magnitude of the peak areas: the helium introduced during the pressurization step may produce significant variations of the results when too small volume of liquid is selected. The minimum volume required should thus be evaluated prior to obtain experimentally the concentration in the vapor phase and the activity coefficients. In this work, the mixture acetonitrile-toluene is taken as example, requiring a sample volume of more than 5mL (about more than 25% of the vial volume). The vapor-liquid equilibrium and activity coefficients of mixtures at different concentrations (0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 molar fraction) and four temperatures (35, 45, 55 and 70°C) have been determined. Relative standard deviations (RSD) lower than 5% have been obtained, indicating the good reproducibility of the method when a sample volume larger than 5mL is used. Finally, a general procedure to measure activity coefficients by means of pressure-balanced head-space gas chromatography is proposed. Copyright © 2013 Elsevier B.V. All rights reserved.

Determination of silver in soils, sediments, and rocks by organic-chelate extraction and atomic absorption spectrophotometry

USGS Publications Warehouse

Chao, T.T.; Ball, J.W.; Nakagawa, H.M.

1971-01-01

A useful method for the determination of silver in soil, sediment, and rock samples in geochemical exploration has been developed. The sample is digested with concentrated nitric acid, and the silver extracted with triisooctyl thiophosphate (TOTP) in methyl isobutyl ketone (MIBK) after dilution of the acid digest to approximately 6 M. The extraction of silver into the organic extractant is quantitative and not affected by the nitric acid concentration from 4 M to 8 M, or by different volumes of TOTP-MIBK. The extracted silver is stable and remains in the organic phase up to several days. The silver concentration is determined by atomic absorption spectrophotometry. ?? 1971.

Thyroid volumes and urinary iodine in German school children.

PubMed

Rendl, J; Juhran, N; Reiners, C

2001-01-01

Several recently published investigations showed a significant improvement in the iodine supply of the German population, but so far Germany is still considered an iodine deficient country. However most of the studies presented do not meet the epidemiological criteria established by WHO, UNICEF and ICCIDD and may therefore suffer from a selection bias with respect to goiter prevalence estimates. School children, owing to their easy recruitment, representativeness of different socio-economic classes and high vulnerability of Iodine deficiency disorders (IDD), are one of the best target groups for surveillance of IDD. In this field study a total of 591 children were investigated. The total sample included 268 females and 323 males aged 7-17 years. The following data were collected: thyroid size by ultrasound, urinary iodine concentration in a first-morning spot urine, weight, height, sex and age. The median urinary iodine concentration of the children was 183 microg/L. The proportion of samples with concentrations below 100 microg/L or below 50 microg/L was 15.4% and 4.3% respectively. Urine samples with high iodine concentrations were also found amounting to 17.3%. Almost all families (97%) declared to use iodized kitchen salt and 19.6% of all children are taking regularly iodine tablets. Application of the WHO/ICCIDD thyroid volume references to the German children resulted in a goiter prevalence of 0.2%, using either age/sex-specific or body surface area (BSA)/sex-specific cut-off values. Comparison with the P97 values of the original normative data of Gutekunst and Martin-Teichert however gives a goiter prevalence of 3% as expected. The thyroid volumes of the children in our study appear comparable with those reported recently for iodine sufficient children from Switzerland and for iodine replete Berlin children and for children with sufficient iodine supply in the region of Leipzig, so that Germany probably has no longer to be considered an iodine deficient country. Our own study and the most recently published studies on iodine replete children give rise to the supposition that the WHO/ICCIDD recommended thyroid volume references are too high.

Tracer-monitored flow titrations.

PubMed

Sasaki, Milton K; Rocha, Diogo L; Rocha, Fábio R P; Zagatto, Elias A G

2016-01-01

The feasibility of implementing tracer-monitored titrations in a flow system is demonstrated. A dye tracer is used to estimate the instant sample and titrant volumetric fractions without the need for volume, mass or peak width measurements. The approach was applied to spectrophotometric flow titrations involving variations of sample and titrant flow-rates (i.e. triangle programmed technique) or concentration gradients established along the sample zone (i.e. flow injection system). Both strategies required simultaneous monitoring of two absorbing species, namely the titration indicator and the dye tracer. Mixing conditions were improved by placing a chamber with mechanical stirring in the analytical path aiming at to minimize diffusional effects. Unlike most of flow-based titrations, the innovation is considered as a true titration, as it does not require a calibration curve thus complying with IUPAC definition. As an application, acidity evaluation in vinegars involving titration with sodium hydroxide was selected. Phenolphthalein and brilliant blue FCF were used as indicator and dye tracer, respectively. Effects of sample volume, titrand/titrant concentrations and flow rates were investigated aiming at improved accuracy and precision. Results were reliable and in agreement with those obtained by a reference titration procedure. Copyright © 2015 Elsevier B.V. All rights reserved.

Grey matter, an endophenotype for schizophrenia? A voxel-based morphometry study in siblings of patients with schizophrenia.

PubMed

van der Velde, Jorien; Gromann, Paula M; Swart, Marte; de Haan, Lieuwe; Wiersma, Durk; Bruggeman, Richard; Krabbendam, Lydia; Aleman, André

2015-05-01

Grey matter, both volume and concentration, has been proposed as an endophenotype for schizophrenia given a number of reports of grey matter abnormalities in relatives of patients with schizophrenia. However, previous studies on grey matter abnormalities in relatives have produced inconsistent results. The aim of the present study was to examine grey matter differences between controls and siblings of patients with schizophrenia and to examine whether the age, genetic loading or subclinical psychotic symptoms of selected individuals could explain the previously reported inconsistencies. We compared the grey matter volume and grey matter concentration of healthy siblings of patients with schizophrenia and healthy controls matched for age, sex and education using voxel-based morphometry (VBM). Furthermore, we selected subsamples based on age (< 30 yr), genetic loading and subclinical psychotic symptoms to examine whether this would lead to different results. We included 89 siblings and 69 controls in our study. The results showed that siblings and controls did not differ significantly on grey matter volume or concentration. Furthermore, specifically selecting participants based on age, genetic loading or subclinical psychotic symptoms did not alter these findings. The main limitation was that subdividing the sample resulted in smaller samples for the subanalyses. Furthermore, we used MRI data from 2 different scanner sites. These results indicate that grey matter measured through VBM might not be a suitable endophenotype for schizophrenia.

Salting-out assisted liquid-liquid extraction combined with capillary HPLC for the determination of sulfonylurea herbicides in environmental water and banana juice samples.

PubMed

Gure, Abera; Lara, Francisco J; Moreno-González, David; Megersa, Negussie; del Olmo-Iruela, Monsalud; García-Campaña, Ana M

2014-09-01

A salting-out assisted liquid-liquid extraction (SALLE) combined with capillary high performance liquid chromatography with diode array detector (capillary HPLC-DAD) was proposed for extraction and determination of residues of nine sulfonylurea herbicides (SUHs) in environmental water and banana juice samples. Various parameters affecting the extraction process such as the type and volume of the organic solvent, sample volume, type and amount of salt, pH of the sample and vortex time were optimized. Under optimum conditions, matrix matched calibration curves were established using river water and banana juice samples. Good linear relationships as well as low limits of detection, LODs (0.4-1.3 and 3-13 µg/L) and quantification, LOQs (1.3-4.3 and 10-43 µg/L) were obtained in water and banana juice samples, respectively. The precision (intra- and inter-day) of the peak areas expressed as relative standard deviations (%, RSD), at two concentration levels were below 10 % in both matrices. Recoveries obtained from spiked environmental waters (river water and groundwater) and banana juice samples, at two concentration levels, ranged from 72 to 115%. The results of the analysis revealed that the proposed SALLE-capillary HPLC method is simple, rapid, cheap and environmentally friendly, being successfully applicable for the determination of SUH residues in waters and banana juices. Copyright © 2014 Elsevier B.V. All rights reserved.

Design and characterization of poly(dimethylsiloxane)-based valves for interfacing continuous-flow sampling to microchip electrophoresis.

PubMed

Li, Michelle W; Huynh, Bryan H; Hulvey, Matthew K; Lunte, Susan M; Martin, R Scott

2006-02-15

This work describes the fabrication and evaluation of a poly(dimethyl)siloxane (PDMS)-based device that enables the discrete injection of a sample plug from a continuous-flow stream into a microchannel for subsequent analysis by electrophoresis. Devices were fabricated by aligning valving and flow channel layers followed by plasma sealing the combined layers onto a glass plate that contained fittings for the introduction of liquid sample and nitrogen gas. The design incorporates a reduced-volume pneumatic valve that actuates (on the order of hundreds of milliseconds) to allow analyte from a continuously flowing sampling channel to be injected into a separation channel for electrophoresis. The injector design was optimized to include a pushback channel to flush away stagnant sample associated with the injector dead volume. The effect of the valve actuation time, the pushback voltage, and the sampling stream flow rate on the performance of the device was characterized. Using the optimized design and an injection frequency of 0.64 Hz showed that the injection process is reproducible (RSD of 1.77%, n = 15). Concentration change experiments using fluorescein as the analyte showed that the device could achieve a lag time as small as 14 s. Finally, to demonstrate the potential uses of this device, the microchip was coupled to a microdialysis probe to monitor a concentration change and sample a fluorescein dye mixture.

Occurrence of selected pharmaceutical and non-pharmaceutical compounds, and stable hydrogen and oxygen isotope ratios in a riverbank filtration study, Platte River, Nebraska, 2002 to 2005, Volume 2

USGS Publications Warehouse

Vogel, J.R.; Barber, L.B.; Furlong, E.T.; Coplen, T.B.; Verstraeten, Ingrid M.; Meyer, M.T.

2005-01-01

This document is the second volume of a data series report that describes the data collected during a study conducted during 2001 through 2005 by the U.S. Geological Survey, in cooperation with the U.S. Environmental Protection Agency and the City of Lincoln, at an established riverbank-filtration well field with horizontal collector wells and vertical wells. The data were collected as part of a study designed to help researchers better understand the efficiency of riverbank filtration with respect to endocrine disrupting compounds and to evaluate the use of riverbank filtration as an effective means of drinking-water treatment. This study provides information that will be useful for (1) increased understanding of the processes and factors controlling the transport of endocrine disrupters, such as pesticides and pharmaceuticals during riverbank filtration, (2) better understanding of the physical and chemical processes that affect riverbank-filtration efficiency, and (3) managing the water resources of the eastern Platte River Basin. This report presents analytical methods and additional data for pharmaceuticals, dissolved organic carbon (DOC), ultraviolet absorbance at 254 nanometer (nm) wavelength (UV254), specific ultraviolet absorbance (SUVA), nitrilotriacetic acid (NTA), ethylenediaminetetraacetic acid (EDTA), nonylphenol ethoxycarboxylates (NPECs), and stable hydrogen and oxygen isotope ratios that were not available at the time of publication of Volume 1 in the data series. Data are presented as generalized statistics and in figures showing temporal variations. Sites from which water-quality samples were collected for this study included wastewater sites (a cattle feedlot lagoon, a hog confinement lagoon, and wastewater-treatment plant effluent), surface-water sites (Platte River, Salt Creek, and Loup Power Canal), ground-water sites (one collector well and five vertical wells), and drinking-water sites (raw and finished). Field water-quality properties also were measured in samples from these sites. Pharmaceuticals detected at least once in samples collected from the Platte River included 1,7-dimethylxanthine, acetaminophen, caffeine, carbamazapine, and cotinine. Among the ground-water samples, pharmaceutical compounds detected at low concentrations in at least one sample included 1,7-dimethylxanthine, acetaminophen, carbamazapine, and trimethoprim. When analyzing for non-pharmaceutical compounds in samples from the wastewater sites, the wastewater-treatment plant effluent samples had the highest concentrations of each of NTA, EDTA, and NPECs compounds. Surface-water samples from Salt Creek had higher concentrations of EDTA and NPECs than samples from the Platte River. NTA was not detected in any samples from the ground-water sites. EDTA was detected in all samples from all wells. Detectable concentrations of EDTA were also observed in all samples from the raw water and finished water.

Plasma volume, osmolality, vasopressin, and renin activity during graded exercise in man

NASA Technical Reports Server (NTRS)

Convertino, V. A.; Keil, L. C.; Bernauer, E. M.; Greenleaf, J. E.

1981-01-01

The influence of work intensity on plasma volume, osmolality, vasopressin and renin activity and the interrelationships between these responses are investigated. Plasma volume, renin activity and osmotic, sodium and arginine vasopressin concentrations were measured in venous blood samples taken from 15 healthy male subjects before and after six minutes of bicycle ergometer exercise at 100, 175 and 225 W. Plasma volume is found to decrease significantly with increasing work intensity, while increases in Na(+) concentration, osmolality and vasopressin are only observed to be significant when the work intensity exceeds 40% maximal aerobic capacity and plasma resin activity increased linearly at all work levels. In addition, significant correlations are observed between plasma volume and osmolality and sodium changes, and between vasopressin and osmolality and sodium content changes. Data thus support the hypotheses that (1) vasopressin may be the primary controlling endocrine for fluid and electrolyte levels following exercise; (2) an exercise intensity greater than 40% maximal aerobic capacity is required to stimulate vasopressin release through changes in plasma osmolality; and (3) the stimulation of the renin-angiotensin system is a more general stress response.

Protein aggregation studied by forward light scattering and light transmission analysis

NASA Astrophysics Data System (ADS)

Penzkofer, A.; Shirdel, J.; Zirak, P.; Breitkreuz, H.; Wolf, E.

2007-12-01

The aggregation of the circadian blue-light photo-receptor cryptochrome from Drosophila melanogaster (dCry) is studied by transmission and forward light scattering measurement in the protein transparent wavelength region. The light scattering in forward direction is caused by Rayleigh scattering which is proportional to the degree of aggregation. The light transmission through the samples in the transparent region is reduced by Mie light scattering in all directions. It depends on the degree of aggregation and the monomer volume fill factor of the aggregates (less total scattering with decreasing monomer volume fill factor of protein globule) allowing a distinction between tightly packed protein aggregation (monomer volume fill factor 1) and loosely packed protein aggregation (monomer volume fill factor less than 1). An increase in aggregation with temperature, concentration, and blue-light exposure is observed. At a temperature of 4 °C and a protein concentration of less than 0.135 mM no dCry aggregation was observed, while at 24 °C and 0.327 mM gelation occurred (loosely packed aggregates occupying the whole solution volume).

A microfluidic platform for precision small-volume sample processing and its use to size separate biological particles with an acoustic microdevice [Precision size separation of biological particles in small-volume samples by an acoustic microfluidic system

DOE PAGES

Fong, Erika J.; Huang, Chao; Hamilton, Julie; ...

2015-11-23

Here, a major advantage of microfluidic devices is the ability to manipulate small sample volumes, thus reducing reagent waste and preserving precious sample. However, to achieve robust sample manipulation it is necessary to address device integration with the macroscale environment. To realize repeatable, sensitive particle separation with microfluidic devices, this protocol presents a complete automated and integrated microfluidic platform that enables precise processing of 0.15–1.5 ml samples using microfluidic devices. Important aspects of this system include modular device layout and robust fixtures resulting in reliable and flexible world to chip connections, and fully-automated fluid handling which accomplishes closed-loop sample collection,more » system cleaning and priming steps to ensure repeatable operation. Different microfluidic devices can be used interchangeably with this architecture. Here we incorporate an acoustofluidic device, detail its characterization, performance optimization, and demonstrate its use for size-separation of biological samples. By using real-time feedback during separation experiments, sample collection is optimized to conserve and concentrate sample. Although requiring the integration of multiple pieces of equipment, advantages of this architecture include the ability to process unknown samples with no additional system optimization, ease of device replacement, and precise, robust sample processing.« less

Ambient concentrations of total suspended particulate matter and its elemental constituents at the wider area of the mining facilities of TVX Hellas in Chalkidiki, Greece.

PubMed

Gaidajis, George

2003-01-01

To assess ambient air quality at the wider area of TVX Hellas mining facilities, the Total Suspended Particulate matter (TSP) and its content in characteristic elements, i.e., As, Cd, Cu, Fe, Mn, Pb, Zn are being monitored for more than thirty months as part of the established Environmental Monitoring Program. High Volume air samplers equipped with Tissue Quartz filters were employed for the collection of TSP. Analyses were effected after digestion of the suspended particulate with an HNO3-HCl solution and determination of elemental concentrations with an Atomic Absorption Spectroscopy equipped with graphite furnace. The sampling stations were selected to record representatively the existing ambient air quality in the vicinity of the facilities and at remote sites not affected from industrial activities. Monitoring data indicated that the background TSP concentrations ranged from 5-60 microg/m3. Recorded TSP concentrations at the residential sites close to the facilities ranged between 20-100 microg/m3, indicating only a minimal influence from the mining and milling activities. Similar spatial variation was observed for the TSP constituents and specifically for Pb and Zn. To validate the monitoring procedures, a parallel sampling campaign took place with different High Volume samplers at days where low TSP concentrations were expected. The satisfactory agreement (+/- 11%) at low concentrations (50-100 microg/m3) clearly supported the reproducibility of the techniques employed specifically at the critical range of lower concentrations.

NanoDrop Microvolume Quantitation of Nucleic Acids

PubMed Central

Desjardins, Philippe; Conklin, Deborah

2010-01-01

Biomolecular assays are continually being developed that use progressively smaller amounts of material, often precluding the use of conventional cuvette-based instruments for nucleic acid quantitation for those that can perform microvolume quantitation. The NanoDrop microvolume sample retention system (Thermo Scientific NanoDrop Products) functions by combining fiber optic technology and natural surface tension properties to capture and retain minute amounts of sample independent of traditional containment apparatus such as cuvettes or capillaries. Furthermore, the system employs shorter path lengths, which result in a broad range of nucleic acid concentration measurements, essentially eliminating the need to perform dilutions. Reducing the volume of sample required for spectroscopic analysis also facilitates the inclusion of additional quality control steps throughout many molecular workflows, increasing efficiency and ultimately leading to greater confidence in downstream results. The need for high-sensitivity fluorescent analysis of limited mass has also emerged with recent experimental advances. Using the same microvolume sample retention technology, fluorescent measurements may be performed with 2 μL of material, allowing fluorescent assays volume requirements to be significantly reduced. Such microreactions of 10 μL or less are now possible using a dedicated microvolume fluorospectrometer. Two microvolume nucleic acid quantitation protocols will be demonstrated that use integrated sample retention systems as practical alternatives to traditional cuvette-based protocols. First, a direct A260 absorbance method using a microvolume spectrophotometer is described. This is followed by a demonstration of a fluorescence-based method that enables reduced-volume fluorescence reactions with a microvolume fluorospectrometer. These novel techniques enable the assessment of nucleic acid concentrations ranging from 1 pg/ μL to 15,000 ng/ μL with minimal consumption of sample. PMID:21189466

Radiolytic Hydrogen Production in the Subseafloor Basaltic Aquifer.

PubMed

Dzaugis, Mary E; Spivack, Arthur J; Dunlea, Ann G; Murray, Richard W; D'Hondt, Steven

2016-01-01

Hydrogen (H2) is produced in geological settings by dissociation of water due to radiation from radioactive decay of naturally occurring uranium ((238)U, (235)U), thorium ((232)Th) and potassium ((40)K). To quantify the potential significance of radiolytic H2 as an electron donor for microbes within the South Pacific subseafloor basaltic aquifer, we use radionuclide concentrations of 43 basalt samples from IODP Expedition 329 to calculate radiolytic H2 production rates in basement fractures. The samples are from three sites with very different basement ages and a wide range of alteration types. U, Th, and K concentrations vary by up to an order of magnitude from sample to sample at each site. Comparison of our samples to each other and to the results of previous studies of unaltered East Pacific Rise basalt suggests that significant variations in radionuclide concentrations are due to differences in initial (unaltered basalt) concentrations (which can vary between eruptive events) and post-emplacement alteration. However, there is no clear relationship between alteration type and calculated radiolytic yields. Local maxima in U, Th, and K produce hotspots of H2 production, causing calculated radiolytic rates to differ by up to a factor of 80 from sample to sample. Fracture width also greatly influences H2 production, where microfractures are hotspots for radiolytic H2 production. For example, H2 production rates normalized to water volume are 190 times higher in 1 μm wide fractures than in fractures that are 10 cm wide. To assess the importance of water radiolysis for microbial communities in subseafloor basaltic aquifers, we compare electron transfer rates from radiolysis to rates from iron oxidation in subseafloor basalt. Radiolysis appears likely to be a more important electron donor source than iron oxidation in old (>10 Ma) basement basalt. Radiolytic H2 production in the volume of water adjacent to a square cm of the most radioactive SPG basalt may support as many as 1500 cells.

Analysis of problems and failures in the measurement of soil-gas radon concentration.

PubMed

Neznal, Martin; Neznal, Matěj

2014-07-01

Long-term experience in the field of soil-gas radon concentration measurements allows to describe and explain the most frequent causes of failures, which can appear in practice when various types of measurement methods and soil-gas sampling techniques are used. The concept of minimal sampling depth, which depends on the volume of the soil-gas sample and on the soil properties, is shown in detail. Consideration of minimal sampling depth at the time of measurement planning allows to avoid the most common mistakes. The ways how to identify influencing parameters, how to avoid a dilution of soil-gas samples by the atmospheric air, as well as how to recognise inappropriate sampling methods are discussed. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Optimization of methane production by combining organic waste and cow manure as feedstock in anaerobic digestion

NASA Astrophysics Data System (ADS)

Theresia, Martha; Priadi, Cindy Rianti

2017-03-01

The anaerobic digestion (AD) process from organic waste is often unstable due to the high concentration of Volatile Fatty Acids (VFAs). The purpose of this research was to determine/evaluate the production of methane using biochemical methane potential (BMP) test with two substrate combinations, consisted of organic waste and cow manure as buffer. BMP test conducted for 35 days at a temperature of ± 35°C by measuring the volume and concentration of biogas every week and testing the sample characteristics before and after the test. The result of the sample variation showed there was no significantly difference of methane volume in the 5th week except the variation of organic waste/cow manure: 12/1 to 3/1, but the sample with a ratio of 3/1 yielded the highest methane potential of 0,58 ± 0.015 (n = 3) LCH4/gr Volatile Solid. The addition of cow manure stabilized the condition of all variations during BMP test with VFAs/alkalinity <0.3 although Carbon/Nitogen ratio of each variation is <20.

Development of a magnetic lab-on-a-chip for point-of-care sepsis diagnosis

NASA Astrophysics Data System (ADS)

Schotter, Joerg; Shoshi, Astrit; Brueckl, Hubert

2009-05-01

We present design criteria, operation principles and experimental examples of magnetic marker manipulation for our magnetic lab-on-a-chip prototype. It incorporates both magnetic sample preparation and detection by embedded GMR-type magnetoresistive sensors and is optimized for the automated point-of-care detection of four different sepsis-indicative cytokines directly from about 5 μl of whole blood. The sample volume, magnetic particle size and cytokine concentration determine the microfluidic volume, sensor size and dimensioning of the magnetic gradient field generators. By optimizing these parameters to the specific diagnostic task, best performance is expected with respect to sensitivity, analysis time and reproducibility.

Influence of Bisphenol A on Thyroid Volume and Structure Independent of Iodine in School Children

PubMed Central

Wang, Na; Zhou, Ying; Fu, Chaowei; Wang, Hexing; Huang, Peixin; Wang, Bin; Su, Meifang; Jiang, Feng; Fang, Hong; Zhao, Qi; Chen, Yue; Jiang, Qingwu

2015-01-01

Background Although several studies have evaluated the relationship between bisphenol A (BPA) and thyroid functions, their results are not entirely consistent. Little is known about BPA in relation to thyroid volume and structure. Methods We examined the association of BPA with thyroid volume and thyroid nodules using data from 718 Chinese children living in the East Coast of China in 2012. First morning urine samples were collected for the determination of urinary BPA, creatinine, and urinary iodine concentrations (UIC). Thyroid volume (TV) and nodules were assessed by thyroid ultrasonography. Results The median of TV was 3.14ml. 459(63.9%) children took iodized salt at home and the median of UIC was 159μg/l. BPA was detected in 99.9% of the urine samples and the medians for boys and girls were 2.64 and 2.35μg/g creatinine, respectively. Of all participants 14.0% had thyroid nodules. Urinary BPA concentration was inversely associated with thyroid volume (β = -0.033, 95% CI: -0.053, -0.013) and the risk for multiple nodules (OR = 0.78; 95% CI: 0.63, 0.97). The associations above were similar for children who consumed iodized salt and those consumed non-iodized salt. Conclusions The data suggest that BPA may be one of the influencing factors for TV and thyroid nodules and its effects are independent of iodine nutrition status in children. PMID:26496713

The effect of operating conditions on the performance of soil slurry-SBRs.

PubMed

Cassidy, D P; Irvine, R L

2001-01-01

Biological treatment of a silty clay loam with aged diesel fuel contamination was conducted in 8 L Soil Slurry-Sequencing Batch Reactors (SS-SBRs). The purpose was to monitor slurry conditions and evaluate reactor performance for varying solids concentration (5%, 25%, 40%, 50%), mixing speed (300 rpm, 700 rpm, 1200 rpm), retention time (8 d, 10 d, 20 d), and volume replaced per cycle (10%, 50%, 90%). Diesel fuel was measured in slurry and in filtered aqueous samples. Oxygen uptake rate (OUR) was monitored. Aggregate size was measured with sieve analyses. Biosurfactant production was quantified with surface tension measurements. Increasing solids concentration and decreasing mixing speed resulted in increased aggregate size, which in turn increased effluent diesel fuel concentrations. Diesel fuel removal was unaffected by retention time and volume replaced per cycle. Biosurfactant production occurred with all operating strategies. Foam thickness was related to surfactant concentration and mixing speed. OUR, surfactant concentration, and foam thickness increased with increasing diesel fuel added per cycle.

A Comparative Study of Serum Exosome Isolation Using Differential Ultracentrifugation and Three Commercial Reagents.

PubMed

Helwa, Inas; Cai, Jingwen; Drewry, Michelle D; Zimmerman, Arthur; Dinkins, Michael B; Khaled, Mariam Lotfy; Seremwe, Mutsa; Dismuke, W Michael; Bieberich, Erhard; Stamer, W Daniel; Hamrick, Mark W; Liu, Yutao

2017-01-01

Exosomes play a role in cell-to-cell signaling and serve as possible biomarkers. Isolating exosomes with reliable quality and substantial concentration is a major challenge. Our purpose is to compare the exosomes extracted by three different exosome isolation kits (miRCURY, ExoQuick, and Invitrogen Total Exosome Isolation Reagent) and differential ultracentrifugation (UC) using six different volumes of a non-cancerous human serum (5 ml, 1 ml, 500 μl, 250 μl, 100 μl, and 50 μl) and three different volumes (1 ml, 500 μl and 100 μl) of six individual commercial serum samples collected from human donors. The smaller starting volumes (100 μl and 50 μl) are used to mimic conditions of limited availability of heterogeneous biological samples. The isolated exosomes were characterized based upon size, quantity, zeta potential, CD63 and CD9 protein expression, and exosomal RNA (exRNA) quality and quantity using several complementary methods: nanoparticle tracking analysis (NTA) with ZetaView, western blot, transmission electron microscopy (TEM), the Agilent Bioanalyzer system, and droplet digital PCR (ddPCR). Our NTA results showed that all isolation techniques produced exosomes within the expected size range (40-150 nm). The three kits, though, produced a significantly higher yield (80-300 fold) of exosomes as compared to UC for all serum volumes, except 5 mL. We also found that exosomes isolated by the different techniques and serum volumes had similar zeta potentials to previous studies. Western blot analysis and TEM immunogold labelling confirmed the expression of two common exosomal protein markers, CD63 and CD9, in samples isolated by all techniques. All exosome isolations yielded high quality exRNA, containing mostly small RNA with a peak between 25 and 200 nucleotides in size. ddPCR results indicated that exosomes isolated from similar serum volumes but different isolation techniques rendered similar concentrations of two selected exRNA: hsa-miR-16 and hsa-miR-451. In summary, the three commercial exosome isolation kits are viable alternatives to UC, even when limited amounts of biological samples are available.

Glass wool filters for concentrating waterborne viruses and agricultural zoonotic pathogens

USGS Publications Warehouse

Millen, Hana T.; Gonnering, Jordan C.; Berg, Ryan K.; Spencer, Susan K.; Jokela, William E.; Pearce, John M.; Borchardt, Jackson S.; Borchardt, Mark A.

2012-01-01

The key first step in evaluating pathogen levels in suspected contaminated water is concentration. Concentration methods tend to be specific for a particular pathogen group, for example US Environmental Protection Agency Method 1623 for Giardia and Cryptosporidium1, which means multiple methods are required if the sampling program is targeting more than one pathogen group. Another drawback of current methods is the equipment can be complicated and expensive, for example the VIRADEL method with the 1MDS cartridge filter for concentrating viruses2. In this article we describe how to construct glass wool filters for concentrating waterborne pathogens. After filter elution, the concentrate is amenable to a second concentration step, such as centrifugation, followed by pathogen detection and enumeration by cultural or molecular methods. The filters have several advantages. Construction is easy and the filters can be built to any size for meeting specific sampling requirements. The filter parts are inexpensive, making it possible to collect a large number of samples without severely impacting a project budget. Large sample volumes (100s to 1,000s L) can be concentrated depending on the rate of clogging from sample turbidity. The filters are highly portable and with minimal equipment, such as a pump and flow meter, they can be implemented in the field for sampling finished drinking water, surface water, groundwater, and agricultural runoff. Lastly, glass wool filtration is effective for concentrating a variety of pathogen types so only one method is necessary. Here we report on filter effectiveness in concentrating waterborne human enterovirus, Salmonella enterica, Cryptosporidium parvum, and avian influenza virus.

Glass Wool Filters for Concentrating Waterborne Viruses and Agricultural Zoonotic Pathogens

PubMed Central

Millen, Hana T.; Gonnering, Jordan C.; Berg, Ryan K.; Spencer, Susan K.; Jokela, William E.; Pearce, John M.; Borchardt, Jackson S.; Borchardt, Mark A.

2012-01-01

The key first step in evaluating pathogen levels in suspected contaminated water is concentration. Concentration methods tend to be specific for a particular pathogen group, for example US Environmental Protection Agency Method 1623 for Giardia and Cryptosporidium1, which means multiple methods are required if the sampling program is targeting more than one pathogen group. Another drawback of current methods is the equipment can be complicated and expensive, for example the VIRADEL method with the 1MDS cartridge filter for concentrating viruses2. In this article we describe how to construct glass wool filters for concentrating waterborne pathogens. After filter elution, the concentrate is amenable to a second concentration step, such as centrifugation, followed by pathogen detection and enumeration by cultural or molecular methods. The filters have several advantages. Construction is easy and the filters can be built to any size for meeting specific sampling requirements. The filter parts are inexpensive, making it possible to collect a large number of samples without severely impacting a project budget. Large sample volumes (100s to 1,000s L) can be concentrated depending on the rate of clogging from sample turbidity. The filters are highly portable and with minimal equipment, such as a pump and flow meter, they can be implemented in the field for sampling finished drinking water, surface water, groundwater, and agricultural runoff. Lastly, glass wool filtration is effective for concentrating a variety of pathogen types so only one method is necessary. Here we report on filter effectiveness in concentrating waterborne human enterovirus, Salmonella enterica, Cryptosporidium parvum, and avian influenza virus. PMID:22415031

Improved sperm kinematics in semen samples collected after 2 h versus 4-7 days of ejaculation abstinence.

PubMed

Alipour, H; Van Der Horst, G; Christiansen, O B; Dardmeh, F; Jørgensen, N; Nielsen, H I; Hnida, C

2017-07-01

Does a short abstinence period of only 2 h yield spermatozoa with better motility characteristics than samples collected after 4-7 days? Despite lower semen volume, sperm concentration, total sperm counts and total motile counts, higher percentages of motile spermatozoa with higher velocity and progressiveness were detected in samples obtained after 2 h. Most studies that have assessed the effect of abstinence periods on sperm motility parameters in men with a sperm concentration below 15 million/ml have detected a higher percentage of motile spermatozoa in samples obtained after short abstinence periods. Studies of men with sperm concentrations above 15 million/ml have reported significantly decreased motile sperm counts after 24 h of abstinence compared with longer abstinence periods. This study had a controlled repeated-measures design based on semen samples from 43 male partners, in couples attending for IVF treatment, who had a sperm concentration above 15 million/ml. Data were collected between June 2014 and December 2015 in the Fertility Unit of Aalborg University Hospital (Aalborg, Denmark). Participants provided a semen sample after 4-7 days of abstinence followed by another sample after only 2 h. For both ejaculates, sperm concentration, total sperm counts, motility groups and detailed kinematic parameters were assessed and compared by using the Sperm Class Analyzer (SCA) computer-aided sperm analysis system before and after density gradient selection. The laboratory's local manual method (Makler chamber) was used for comparison. The second raw ejaculate demonstrated lower semen volume (P < 0.0001), sperm concentration (P = 0.003) and sperm counts in all motility sub-groups (P < 0.001) but higher percentages of spermatozoa with higher velocity (P < 0.01), progressiveness (P < 0.001) and hyperactivation (P < 0.001), compared with the first raw ejaculate. The first ejaculate in this study was also used for the IVF/ICSI treatments and therefore only patients with a semen volume ≥2 ml and concentration ≥15 million/ml were included. Further validation in large prospective randomized controlled trials, more purposely directed at normozoospermic males with partners having problems conceiving when there appears to be no female factor, is needed to confirm the potential advantage of using a second semen sample in improving fertilization and pregnancy rates in assisted reproduction. Despite the significantly lower semen volume, sperm concentration and total sperm counts in all motility sub-groups, the significantly higher percentage of spermatozoa with better motility characteristics (velocity, progressiveness and hyperactivation) in the second ejaculate, may provide and allow for a simpler and more effective selection of higher quality spermatozoa. This could prove to be an advantage for ART procedures such as intracytoplasmic sperm injection where a large number of spermatozoa is not needed. It can also be speculated that pooling two consecutive ejaculates obtained after 4-7 days and after 2 h, could be an advantage for intrauterine insemination where a large number of motile spermatozoa are needed. This study was supported by internal grants from the Department of Health Science and Technology, Faculty of Medicine, Aalborg University (Aalborg, Denmark). The SCA® was provided by a grant from 'Ferring Pharmaceuticals' to Aalborg University Hospital (H.I.N). G.V.D.H. is an external senior scientific consultant to Microptic S/L (Barcelona, Spain). H.A. has provided scientific input and presentations for Microptic S/L (Barcelona, Spain) on several occasions. All other authors declare no conflict of interest. N/A. © The Author 2017. Published by Oxford University Press on behalf of the European Society of Human Reproduction and Embryology. All rights reserved. For Permissions, please e-mail: journals.permissions@oup.com

DOE Office of Scientific and Technical Information (OSTI.GOV)

Robison, W L; Hamilton, T F; Bogen, K

Inter-plant concentration ratios (IPCR), [Bq g{sup -1} {sup 137}Cs in coral atoll tree food-crops/Bq g{sup -1} {sup 137}Cs in leaves of native plant species whose roots share a common soil volume], can replace transfer factors (TF) to predict {sup 137}Cs concentration in tree food-crops in a contaminated area with an aged source term. The IPCR strategy has significant benefits relative to TF strategy for such purposes in the atoll ecosystem. IPCR strategy applied to specific assessments takes advantage of the fact tree roots naturally integrate 137Cs over large volumes of soil. Root absorption of {sup 137}Cs replaces large-scale, expensive soilmore » sampling schemes to reduce variability in {sup 137}Cs concentration due to inhomogeneous radionuclide distribution. IPCR [drinking-coconut meat (DCM)/Scaevola (SCA) and Tournefortia (TOU) leaves (native trees growing on all atoll islands)] are log normally distributed (LND) with geometric standard deviation (GSD) = 1.85. TF for DCM from Enewetak, Eneu, Rongelap and Bikini Atolls are LND with GSD's of 3.5, 3.0, 2.7, and 2.1, respectively. TF GSD for Rongelap copra coconut meat is 2.5. IPCR of Pandanus fruit to SCA and TOU leaves are LND with GSD = 1.7 while TF GSD is 2.1. Because IPCR variability is much lower than TF variability, relative sampling error of an IPCR field sample mean is up 6- to 10-fold lower than that of a TF sample mean if sample sizes are small (10 to 20). Other IPCR advantages are that plant leaf samples are collected and processed in far less time with much less effort and cost than soil samples.« less

A new design of groundwater sampling device and its application.

PubMed

Tsai, Yih-jin; Kuo, Ming-ching T

2005-01-01

Compounds in the atmosphere contaminate samples of groundwater. An inexpensive and simple method for collecting groundwater samples is developed to prevent contamination when the background concentration of contaminants is high. This new design of groundwater sampling device involves a glass sampling bottle with a Teflon-lined valve at each end. A cleaned and dried sampling bottle was connected to a low flow-rate peristaltic pump with Teflon tubing and was filled with water. No headspace volume was remained in the sampling bottle. The sample bottle was then packed in a PVC bag to prevent the target component from infiltrating into the water sample through the valves. In this study, groundwater was sampled at six wells using both the conventional method and the improved method. The analysis of trichlorofluoromethane (CFC-11) concentrations at these six wells indicates that all the groundwater samples obtained by the conventional sampling method were contaminated by CFC-11 from the atmosphere. The improved sampling method greatly eliminated the problems of contamination, preservation and quantitative analysis of natural water.

Purifying, Separating, and Concentrating Cells From a Sample Low in Biomass

NASA Technical Reports Server (NTRS)

Benardini, James N.; LaDuc, Myron T.; Diamond, Rochelle

2012-01-01

Frequently there is an inability to process and analyze samples of low biomass due to limiting amounts of relevant biomaterial in the sample. Furthermore, molecular biological protocols geared towards increasing the density of recovered cells and biomolecules of interest, by their very nature, also concentrate unwanted inhibitory humic acids and other particulates that have an adversarial effect on downstream analysis. A novel and robust fluorescence-activated cell-sorting (FACS)-based technology has been developed for purifying (removing cells from sampling matrices), separating (based on size, density, morphology), and concentrating cells (spores, prokaryotic, eukaryotic) from a sample low in biomass. The technology capitalizes on fluorescent cell-sorting technologies to purify and concentrate bacterial cells from a low-biomass, high-volume sample. Over the past decade, cell-sorting detection systems have undergone enhancements and increased sensitivity, making bacterial cell sorting a feasible concept. Although there are many unknown limitations with regard to the applicability of this technology to environmental samples (smaller cells, few cells, mixed populations), dogmatic principles support the theoretical effectiveness of this technique upon thorough testing and proper optimization. Furthermore, the pilot study from which this report is based proved effective and demonstrated this technology capable of sorting and concentrating bacterial endospore and bacterial cells of varying size and morphology. Two commercial off-the-shelf bacterial counting kits were used to optimize a bacterial stain/dye FACS protocol. A LIVE/DEAD BacLight Viability and Counting Kit was used to distinguish between the live and dead cells. A Bacterial Counting Kit comprising SYTO BC (mixture of SYTO dyes) was employed as a broad-spectrum bacterial counting agent. Optimization using epifluorescence microscopy was performed with these two dye/stains. This refined protocol was further validated using varying ratios and mixtures of cells to ensure homogenous staining compared to that of individual cells, and were utilized for flow analyzer and FACS labeling. This technology focuses on the purification and concentration of cells from low-biomass spacecraft assembly facility samples. Currently, purification and concentration of low-biomass samples plague planetary protection downstream analyses. Having a capability to use flow cytometry to concentrate cells out of low-biomass, high-volume spacecraft/ facility sample extracts will be of extreme benefit to the fields of planetary protection and astrobiology. Successful research and development of this novel methodology will significantly increase the knowledge base for designing more effective cleaning protocols, and ultimately lead to a more empirical and true account of the microbial diversity present on spacecraft surfaces. Refined cleaning and an enhanced ability to resolve microbial diversity may decrease the overall cost of spacecraft assembly and/or provide a means to begin to assess challenging planetary protection missions.

Quantification of Protozoa and Viruses from Small Water Volumes

PubMed Central

Bonilla, J. Alfredo; Bonilla, Tonya D.; Abdelzaher, Amir M.; Scott, Troy M.; Lukasik, Jerzy; Solo-Gabriele, Helena M.; Palmer, Carol J.

2015-01-01

Large sample volumes are traditionally required for the analysis of waterborne pathogens. The need for large volumes greatly limits the number of samples that can be processed. The goals of this study were to compare extraction and detection procedures for quantifying protozoan parasites and viruses from small volumes of marine water. The intent was to evaluate a logistically simpler method of sample collection and processing that would facilitate direct pathogen measures as part of routine monitoring programs. Samples were collected simultaneously using a bilayer device with protozoa capture by size (top filter) and viruses capture by charge (bottom filter). Protozoan detection technologies utilized for recovery of Cryptosporidium spp. and Giardia spp. were qPCR and the more traditional immunomagnetic separation—IFA-microscopy, while virus (poliovirus) detection was based upon qPCR versus plaque assay. Filters were eluted using reagents consistent with the downstream detection technologies. Results showed higher mean recoveries using traditional detection methods over qPCR for Cryptosporidium (91% vs. 45%) and poliovirus (67% vs. 55%) whereas for Giardia the qPCR-based methods were characterized by higher mean recoveries (41% vs. 28%). Overall mean recoveries are considered high for all detection technologies. Results suggest that simultaneous filtration may be suitable for isolating different classes of pathogens from small marine water volumes. More research is needed to evaluate the suitability of this method for detecting pathogens at low ambient concentration levels. PMID:26114244

Quantification of Protozoa and Viruses from Small Water Volumes.

PubMed

Bonilla, J Alfredo; Bonilla, Tonya D; Abdelzaher, Amir M; Scott, Troy M; Lukasik, Jerzy; Solo-Gabriele, Helena M; Palmer, Carol J

2015-06-24

Large sample volumes are traditionally required for the analysis of waterborne pathogens. The need for large volumes greatly limits the number of samples that can be processed. The aims of this study were to compare extraction and detection procedures for quantifying protozoan parasites and viruses from small volumes of marine water. The intent was to evaluate a logistically simpler method of sample collection and processing that would facilitate direct pathogen measures as part of routine monitoring programs. Samples were collected simultaneously using a bilayer device with protozoa capture by size (top filter) and viruses capture by charge (bottom filter). Protozoan detection technologies utilized for recovery of Cryptosporidium spp. and Giardia spp. were qPCR and the more traditional immunomagnetic separation-IFA-microscopy, while virus (poliovirus) detection was based upon qPCR versus plaque assay. Filters were eluted using reagents consistent with the downstream detection technologies. Results showed higher mean recoveries using traditional detection methods over qPCR for Cryptosporidium (91% vs. 45%) and poliovirus (67% vs. 55%) whereas for Giardia the qPCR-based methods were characterized by higher mean recoveries (41% vs. 28%). Overall mean recoveries are considered high for all detection technologies. Results suggest that simultaneous filtration may be suitable for isolating different classes of pathogens from small marine water volumes. More research is needed to evaluate the suitability of this method for detecting pathogens at low ambient concentration levels.

Calculating the refractive index for pediatric parenteral nutrient solutions.

PubMed

Nelson, Scott; Barrows, Jason; Haftmann, Richard; Helm, Michael; MacKay, Mark

2013-02-15

The utility of refractometric analysis for calculating the refractive index (RI) of compounded parenteral nutrient solutions for pediatric patients was examined. An equation for calculating the RI of parenteral nutrient solutions was developed by chemical and linear regression analysis of 154 pediatric parenteral nutrient solutions. This equation was then validated by analyzing 1057 pediatric parenteral nutrition samples. The RI for the parenteral nutrient solutions could be calculated by summing the RI contribution for each ingredient and then adding the RI of water. The RI contribution for each ingredient was determined by multiplying the RI of the manufacturer's concentrate by the volume of the manufacturer's concentrate mixed into the parenteral nutrient solution divided by the total volume of the parenteral nutrient solution. The calculated RI was highly correlated with the measured RI (R(2) = 0.94, p < 0.0001). Using a range of two standard deviations (±0.0045), 99.8% of the samples fell into the comparative range. RIs of electrolytes, vitamins, and trace elements in the concentrations used did not affect the RI, similar to the findings of other studies. There was no statistical difference between the calculated RI and the measured RI in the final product of a pediatric parenteral nutrient solution. This method of quality control can be used by personnel compounding parenteral nutrient solutions to confirm the compounding accuracy of dextrose and amino acid concentrations in the final product, and a sample can be sent to the hospital laboratory for electrolyte verification.

Atmospheric ammonia mixing ratios at an open-air cattle feeding facility.

PubMed

Hiranuma, Naruki; Brooks, Sarah D; Thornton, Daniel C O; Auvermann, Brent W

2010-02-01

Mixing ratios of total and gaseous ammonia were measured at an open-air cattle feeding facility in the Texas Panhandle in the summers of 2007 and 2008. Samples were collected at the nominally upwind and downwind edges of the facility. In 2008, a series of far-field samples was also collected 3.5 km north of the facility. Ammonium concentrations were determined by two complementary laboratory methods, a novel application of visible spectrophotometry and standard ion chromatography (IC). Results of the two techniques agreed very well, and spectrophotometry is faster, easier, and cheaper than chromatography. Ammonia mixing ratios measured at the immediate downwind site were drastically higher (approximately 2900 parts per billion by volume [ppbv]) than thos measured at the upwind site (< or = 200 ppbv). In contrast, at 3.5 km away from the facility, ammonia mixing ratios were reduced to levels similar to the upwind site (< or = 200 ppbv). In addition, PM10 (particulate matter < 10 microm in optical diameter) concentrations obtained at each sampling location using Grimm portable aerosol spectrometers are reported. Time-averaged (1-hr) volume concentrations of PM10 approached 5 x 10(12) nm3 cm(-3). Emitted ammonia remained largely in the gas phase at the downwind and far-field locations. No clear correlation between concentrations of ammonia and particles was observed. Overall, this study provides a better understanding of ammonia emissions from open-air animal feeding operations, especially under the hot and dry conditions present during these measurements.

Monitoring Heavy Metal Contents with Sphagnum Junghuhnianum Moss Bags in Relation to Traffic Volume in Wuxi, China.

PubMed

Hu, Rong; Yan, Yun; Zhou, Xiaoli; Wang, Yanan; Fang, Yanming

2018-02-22

Despite its small size, a moss bag can reveal the different temporal and spatial deposition patterns of pollutants at a particular site; therefore, researchers can use moss bags to determine pollution sources and to put forward strategies for pollution control. Although the use of moss bags to monitor atmospheric pollution has been widely reported in Europe, there are few such empirical studies in China. Thus, in this study, bags containing the moss Sphagnum junghuhnianum were used to assess the concentrations of heavy metals (chromium (Cr), copper (Cu), lead (Pb), vanadium (V), and zinc (Zn)) at five sampling sites (four roads and a forest park) during the summer and winter of 2012. According to the relative accumulation factor (RAF) and contamination factor (CF) results, pollution in winter was heavier than that in summer, and Cr was found to be the most contaminating, having the highest mean CF. There was a significant positive correlation ( p < 0.05) between traffic volume and concentration for three heavy metals (Cr, Cu, and V) in winter, whereas a significant positive correlation ( p < 0.05) was observed between traffic volume and concentrations for four heavy metal elements (Cr, Pb, V, and Zn) in summer, indicating a close relationship between heavy metal contents and traffic volume. Although there was substantial variation in the concentrations of the five heavy metals in the moss bags, significant correlations between heavy metals suggested that the contaminants originated from a common source, namely vehicle emissions. The results demonstrated that the four roads were subject to different degrees of pollution depending on the volume of traffic using each road. Therefore, the results of this study suggest that traffic volume is a major reason for heavy metal pollution.

Monitoring Heavy Metal Contents with Sphagnum Junghuhnianum Moss Bags in Relation to Traffic Volume in Wuxi, China

PubMed Central

Hu, Rong; Yan, Yun; Zhou, Xiaoli; Wang, Yanan; Fang, Yanming

2018-01-01

Despite its small size, a moss bag can reveal the different temporal and spatial deposition patterns of pollutants at a particular site; therefore, researchers can use moss bags to determine pollution sources and to put forward strategies for pollution control. Although the use of moss bags to monitor atmospheric pollution has been widely reported in Europe, there are few such empirical studies in China. Thus, in this study, bags containing the moss Sphagnum junghuhnianum were used to assess the concentrations of heavy metals (chromium (Cr), copper (Cu), lead (Pb), vanadium (V), and zinc (Zn)) at five sampling sites (four roads and a forest park) during the summer and winter of 2012. According to the relative accumulation factor (RAF) and contamination factor (CF) results, pollution in winter was heavier than that in summer, and Cr was found to be the most contaminating, having the highest mean CF. There was a significant positive correlation (p < 0.05) between traffic volume and concentration for three heavy metals (Cr, Cu, and V) in winter, whereas a significant positive correlation (p < 0.05) was observed between traffic volume and concentrations for four heavy metal elements (Cr, Pb, V, and Zn) in summer, indicating a close relationship between heavy metal contents and traffic volume. Although there was substantial variation in the concentrations of the five heavy metals in the moss bags, significant correlations between heavy metals suggested that the contaminants originated from a common source, namely vehicle emissions. The results demonstrated that the four roads were subject to different degrees of pollution depending on the volume of traffic using each road. Therefore, the results of this study suggest that traffic volume is a major reason for heavy metal pollution. PMID:29470433

A novel device for quantitative measurement of chloride concentration by fluorescence indicator

NASA Astrophysics Data System (ADS)

Wang, Junsheng; Wu, Xudong; Chon, Chanhee; Gonska, Tanja; Li, Dongqing

2012-02-01

Cystic fibrosis (CF) is a life-threatening genetic disease. At present, the common method for diagnosis of CF is to detect the chloride concentration in sweat using ion-selective electrodes. However, the current sweat testing methods require a relatively large quantity of sweat sample, at least 25 µL, which is very difficult to obtain, especially for newborns. This paper presents a new method and a new device for rapid detection of the chloride concentration from a small volume of solution. In this method, the chloride concentration is determined quantitatively by the fluorescence intensity of MQAE, a chloride ion fluorescent indicator. In this device, the sample is carried by a small piece of filter paper on a cover glass exposed to an UV LED light source. The resulting fluorescent signals are detected by a Si photodiode. Data acquisition and processing are accomplished by LabVIEW software in a PDA. Based on the Stern-Volmer relationship, the effects of different parameters on the fluorescence intensity were analyzed. The observed significant difference between 40 and 60 mM (the borderline of chloride concentration for CF) is discussed in this paper. The results show that detection can be completed within 10 s. The minimum detectable volume of the chloride solution is 1 μL. The novel method and the device are of great potential for CF diagnosis.

Nitric Oxide Measurement Study. Volume II. Probe Methods,

DTIC Science & Technology

1980-05-01

case of the Task I study, it should be pointed out that at lower gas temperatures where much of the study was performed, the mass flow through the...third body as pointed out by Matthews, et al. (1977) but also dependent on the viscosity of the sampled gas for standard commercial units (Folsom and...substantially above the dew point (based on the maximum pressure in the sampling system and the initial water concentration) or (2) sample line and

Micro-apparatus for rapid determinations of protein solubilities

NASA Technical Reports Server (NTRS)

Pusey, Marc L.; Munson, Sibyl

1991-01-01

We have developed a column-based micro-technique for rapid determinations of protein solubilities. While retaining a large crystal surface area, the column dead volume has been reduced to equal to or less than 5 micro liters. The technique was tested with tetragonal lysozyme (pH 4.5, 0.1 M acetate, 3.0 percent NaCl, 5-25 C) and column volumes of about 60, 300, and 900 micro liters. Identical solubility data were obtained, indicating that equilibration was obtained even in the smallest columns. In addition, solubility data for Br- and I- salts of lysozyme (pH 4.5, 0.1 M acetate buffer, 0.5 M salt concentrations) were obtained. It appears that the technique can be further miniaturized. The limit in further reducing the crystalline column volume is determined by the minimum solution sample size needed to determine the protein concentration.

Comparison of traditional and molecular analytical methods for detecting biological agents in raw and drinking water following ultrafiltration

USGS Publications Warehouse

Francy, D.S.; Bushon, R.N.; Brady, A.M.G.; Bertke, E.E.; Kephart, C.M.; Likirdopulos, C.A.; Mailot, B.E.; Schaefer, F. W.; Lindquist, H.D. Alan

2009-01-01

Aims: To compare the performance of traditional methods to quantitative polymerase chain reaction (qPCR) for detecting five biological agents in large-volume drinking-water samples concentrated by ultrafiltration (UF). Methods and Results: Drinking-water samples (100 l) were seeded with Bacillus anthracis, Cryptospordium parvum, Francisella tularensis, Salmonella Typhi, and Vibrio cholerae and concentrated by UF. Recoveries by traditional methods were variable between samples and between some replicates; recoveries were not determined by qPCR. Francisella tularensis and V. cholerae were detected in all 14 samples after UF, B. anthracis was detected in 13, and C. parvum was detected in 9 out of 14 samples. Numbers found by qPCR after UF were significantly or nearly related to those found by traditional methods for all organisms except for C. parvum. A qPCR assay for S. Typhi was not available. Conclusions: qPCR can be used to rapidly detect biological agents after UF as well as traditional methods, but additional work is needed to improve qPCR assays for several biological agents, determine recoveries by qPCR, and expand the study to other areas. Significance and Impact of the Study: To our knowledge, this is the first study to compare the use of traditional and qPCR methods to detect biological agents in large-volume drinking-water samples. ?? 2009 The Society for Applied Microbiology.

Effects of breathing pattern and inspired air conditions on breath condensate volume, pH, nitrite, and protein concentrations.

PubMed

McCafferty, J B; Bradshaw, T A; Tate, S; Greening, A P; Innes, J A

2004-08-01

The effects of breathing pattern and inspired air conditions on the volume and content of exhaled breath condensate (EBC) were investigated. Total exhaled water (TEW), EBC volume, pH, nitrite and protein concentrations were measured in three groups of 10 healthy subjects breathing into a condenser at different target minute ventilations (Vm), tidal volumes (Vt), and inspired air conditions. The volumes of both TEW and EBC increased significantly with Vm. For Vm 7.5, 15 and 22.5 l/min, mean (SD) EBC was 627 (258) microl, 1019 (313) microl, and 1358 (364) microl, respectively (p<0.001) and TEW was 1879 (378) microl, 2986 (496) microl, and 4679 (700) microl, respectively (p<0.001). TEW was significantly higher than EBC, reflecting a condenser efficiency of 40% at a target Vm of 7.5 l/min which reduced to 29% at Vm 22.5 l/min. Lower Vt gave less TEW than higher Vt (26.6 v 30.7 microl/l, mean difference 4.1 (95% CI 2.6 to 5.6), p<0.001) and a smaller EBC volume (4.3 v 7.6 microl/l, mean difference 3.4 (95% CI 2.3 to 4.5), p<0.001). Cooler and drier inspired air yielded less water vapour and less breath condensate than standard conditions (p<0.05). Changes in the breathing pattern had no effect on EBC protein and nitrite concentrations and pH. These results show that condensate volume can be increased by using high Vt and increased Vm without compromising the dilution of the sample.

Comparison of use of an infrared anesthetic gas monitor and refractometry for measurement of anesthetic agent concentrations.

PubMed

Ambrisko, Tamas D; Klide, Alan M

2011-10-01

To assess agreement between anesthetic agent concentrations measured by use of an infrared anesthetic gas monitor (IAGM) and refractometry. SAMPLE-4 IAGMs of the same type and 1 refractometer. Mixtures of oxygen and isoflurane, sevoflurane, desflurane, or N(2)O were used. Agent volume percent was measured simultaneously with 4 IAGMs and a refractometer at the common gas outlet. Measurements obtained with each of the 4 IAGMs were compared with the corresponding refractometer measurements via the Bland-Altman method. Similarly, Bland-Altman plots were also created with either IAGM or refractometer measurements and desflurane vaporizer dial settings. Bias ± 2 SD for comparisons of IAGM and refractometer measurements was as follows: isoflurane, -0.03 ± 0.18 volume percent; sevoflurane, -0.19 ± 0.23 volume percent; desflurane, 0.43 ± 1.22 volume percent; and N(2)O, -0.21 ± 1.88 volume percent. Bland-Altman plots comparing IAGM and refractometer measurements revealed nonlinear relationships for sevoflurane, desflurane, and N(2)O. Desflurane measurements were notably affected; bias ± limits of agreement (2 SD) were small (0.1 ± 0.22 volume percent) at < 12 volume percent, but both bias and limits of agreement increased at higher concentrations. Because IAGM measurements did not but refractometer measurements did agree with the desflurane vaporizer dial settings, infrared measurement technology was a suspected cause of the nonlinear relationships. Given that the assumption of linearity is a cornerstone of anesthetic monitor calibration, this assumption should be confirmed before anesthetic monitors are used in experiments.

Validation of high-throughput measurement system with microwave-assisted extraction, fully automated sample preparation device, and gas chromatography-electron capture detector for determination of polychlorinated biphenyls in whale blubber.

PubMed

Fujita, Hiroyuki; Honda, Katsuhisa; Hamada, Noriaki; Yasunaga, Genta; Fujise, Yoshihiro

2009-02-01

Validation of a high-throughput measurement system with microwave-assisted extraction (MAE), fully automated sample preparation device (SPD), and gas chromatography-electron capture detector (GC-ECD) for the determination of polychlorinated biphenyls (PCBs) in minke whale blubber was performed. PCB congeners accounting for > 95% of the total PCBs burden in blubber were efficiently extracted with a small volume (20 mL) of n-hexane using MAE due to simultaneous saponification and extraction. Further, the crude extract obtained by MAE was rapidly purified and automatically substituted to a small volume (1 mL) of toluene using SPD without using concentrators. Furthermore, the concentration of PCBs in the purified and concentrated solution was accurately determined by GC-ECD. Moreover, the result of accuracy test using a certified material (SRM 1588b; Cod liver oil) showed good agreement with the NIST certified concentration values. In addition, the method quantification limit of total-PCB in whale blubbers was 41 ng g(-1). This new measurement system for PCBs takes only four hours. Consequently, it indicated this method is the most suitable for the monitoring and screening of PCBs in the conservation of the marine ecosystem and safe distribution of foods.

Confocal Raman Microscopy for pH-Gradient Preconcentration and Quantitative Analyte Detection in Optically Trapped Phospholipid Vesicles.

PubMed

Hardcastle, Chris D; Harris, Joel M

2015-08-04

The ability of a vesicle membrane to preserve a pH gradient, while allowing for diffusion of neutral molecules across the phospholipid bilayer, can provide the isolation and preconcentration of ionizable compounds within the vesicle interior. In this work, confocal Raman microscopy is used to observe (in situ) the pH-gradient preconcentration of compounds into individual optically trapped vesicles that provide sub-femtoliter collectors for small-volume samples. The concentration of analyte accumulated in the vesicle interior is determined relative to a perchlorate-ion internal standard, preloaded into the vesicle along with a high-concentration buffer. As a guide to the experiments, a model for the transfer of analyte into the vesicle based on acid-base equilibria is developed to predict the concentration enrichment as a function of source-phase pH and analyte concentration. To test the concept, the accumulation of benzyldimethylamine (BDMA) was measured within individual 1 μm phospholipid vesicles having a stable initial pH that is 7 units lower than the source phase. For low analyte concentrations in the source phase (100 nM), a concentration enrichment into the vesicle interior of (5.2 ± 0.4) × 10(5) was observed, in agreement with the model predictions. Detection of BDMA from a 25 nM source-phase sample was demonstrated, a noteworthy result for an unenhanced Raman scattering measurement. The developed model accurately predicts the falloff of enrichment (and measurement sensitivity) at higher analyte concentrations, where the transfer of greater amounts of BDMA into the vesicle titrates the internal buffer and decreases the pH gradient. The predictable calibration response over 4 orders of magnitude in source-phase concentration makes it suitable for quantitative analysis of ionizable compounds from small-volume samples. The kinetics of analyte accumulation are relatively fast (∼15 min) and are consistent with the rate of transfer of a polar aromatic molecule across a gel-phase phospholipid membrane.

Concentration of seeded simian rotavirus SA-11 from potable waters by using talc-celite layers and hydroextraction.

PubMed

Ramia, S; Sattar, S A

1980-03-01

There is mounting evidence for the waterborne transmission of diarrhea caused by rotaviruses. As a result, proper techniques are required for their recovery from samples of incriminated water. The combined efficiency of the talc-Celite technique and polyethylene glycol 6000 hydroextraction was, therefore, tested for this purpose, using Simian rotavirus SA-11 and MA-104 cells. Conditioning of the dechlorinated tap water samples was carried out by pH adjustment to 6.0 and the addition of Earle balanced salt solution to a final concentration of 1:100. Passage of a 1-liter volume of such a conditioned sample through a layer containing a mixture of talc (300 mg) and Celite 503 (100 mg) led to the adsorption of nearly 93% of the added SA-11 plaque-forming units. For the recovery of the layer-adsorbed virus, 3% beef extract and 1x tryptose phosphate broth were found to be superior to a variety of other eluents tested. When we tested 100-liter sample volumes, layers containing 1.2 g of talc and 0.4 g of Celite were employed. Virus elution was carried out with 100 ml of tryptose phosphate broth. The eluate was concentrated 10-fold by overnight (4 degrees C) hydroextraction with polyethylene glycol. With a total input virus of 7.0 x 10(5) and 1.4 x 10(2) plaque-forming units, the recoveries were about 71 and 59%, respectively.

Magnetized graphene layers synthesized on the carbon nanofibers as novel adsorbent for the extraction of polycyclic aromatic hydrocarbons from environmental water samples.

PubMed

Rezvani-Eivari, Mostafa; Amiri, Amirhassan; Baghayeri, Mehdi; Ghaemi, Ferial

2016-09-23

The application of magnetized graphene (G) layers synthesized on the carbon nanofibers (CNFs) (m-G/CNF) was investigated as novel adsorbent for the magnetic solid-phase extraction (MSPE) of polycyclic aromatic hydrocarbons (PAHs) in water samples followed by gas chromatography-flame ionization detector (GC-FID). Six important parameters, affecting the extraction efficiency of PAHs, including: amount of adsorbent, adsorption and desorption times, type and volume of the eluent solvent and salt content of the sample were evaluated. The optimum extraction conditions were obtained as: 5min for extraction time, 20mg for sorbent amount, dichloromethane as desorption solvent, 1mL for desorption solvent volume, 5min for desorption time and 15% (w/v) for NaCl concentration. Good performance data were obtained at the optimized conditions. The calibration curves were linear over the concentration ranges from 0.012 to 100ngmL(-1) with correlation coefficients (r) between 0.9950 and 0.9967 for all the analytes. The limits of detection (LODs, S/N=3) of the proposed method for the studied PAHs were 0.004-0.03ngmL(-1). The relative standard deviations (RSDs) for five replicates at two concentration levels (0.1 and 50ngmL(-1)) of PAHs were ranged from 3.4 to 5.7%. Appropriate relative recovery values, in the range of 95.5-99.9%, were also obtained for the real water sample analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

Large volume sample stacking of positively chargeable analytes in capillary zone electrophoresis without polarity switching: use of low reversed electroosmotic flow induced by a cationic surfactant at acidic pH.

PubMed

Quirino, J P; Terabe, S

2000-01-01

A simple and effective way to improve detection sensitivity of positively chargeable analytes in capillary zone electrophoresis more than 100-fold is described. Cationic species were made to migrate toward the cathode even under reversed electroosmotic flow caused by a cationic surfactant by using a low pH run buffer. For the first time, with such a configuration, large volume sample stacking of cationic analytes is achieved without a polarity-switching step and loss of efficiency. Samples are prepared in water or aqueous acetonitrile. Aromatic amines and a variety of drugs were concentrated using background solutions containing phosphoric acid and cetyltrimethylammonium bromide. Qualitative and quantitative aspects are also investigated.

Changes in apple liquid phase concentration throughout equilibrium in osmotic dehydration.

PubMed

Barat, J M; Barrera, C; Frías, J M; Fito, P

2007-03-01

Previous results on apple tissue equilibration during osmotic dehydration showed that, at very long processing times, the solute concentrations of the fruit liquid phase and the osmotic solution were the same. In the present study, changes in apple liquid phase composition throughout equilibrium in osmotic dehydration were analyzed and modeled. Results showed that, by the time osmosed samples reached the maximum weight and volume loss, solute concentration of the fruit liquid phase was higher than that of the osmotic solution. The reported overconcentration could be explained in terms of the apple structure shrinkage that occurred during the osmotic dehydration with highly concentrated osmotic solutions due to the elastic response of the food structure to the loss of water and intake of solutes. The fruit liquid phase overconcentration rate was observed to depend on the concentration of the osmotic solution, the processing temperature, the sample size, and shape of the cellular tissue.

Perils of categorical thinking: "Oxic/anoxic" conceptual model in environmental remediation

USGS Publications Warehouse

Bradley, Paul M.

2012-01-01

Given ambient atmospheric oxygen concentrations of about 21 percent (by volume), the lower limit for reliable quantitation of dissolved oxygen concentrations in groundwater samples is in the range of 0.1–0.5 mg/L. Frameworks for assessing in situ redox condition are often applied using a simple two-category (oxic/anoxic) model of oxygen condition. The "oxic" category defines the environmental range in which dissolved oxygen concentrations are clearly expected to impact contaminant biodegradation, either by supporting aerobic biodegradation of electron-donor contaminants like petroleum hydrocarbons or by inhibiting anaerobic biodegradation of electron-acceptor contaminants like chloroethenes. The tendency to label the second category "anoxic" leads to an invalid assumption that oxygen is insignificant when, in fact, the dissolved oxygen concentration is less than detection but otherwise unknown. Expressing dissolved oxygen concentrations as numbers of molecules per volume, dissolved oxygen concentrations that fall below the 0.1 mg/L field detection limit range from 1 to 1017 molecules/L. In light of recent demonstrations of substantial oxygen-linked biodegradation of chloroethene contaminants at dissolved oxygen concentrations well below the 0.1–0.5 mg/L field detection limit, characterizing "less than detection" oxygen concentrations as "insignificant" is invalid.

Method to make accurate concentration and isotopic measurements for small gas samples

NASA Astrophysics Data System (ADS)

Palmer, M. R.; Wahl, E.; Cunningham, K. L.

2013-12-01

Carbon isotopic ratio measurements of CO2 and CH4 provide valuable insight into carbon cycle processes. However, many of these studies, like soil gas, soil flux, and water head space experiments, provide very small gas sample volumes, too small for direct measurement by current constant-flow Cavity Ring-Down (CRDS) isotopic analyzers. Previously, we addressed this issue by developing a sample introduction module which enabled the isotopic ratio measurement of 40ml samples or smaller. However, the system, called the Small Sample Isotope Module (SSIM), does dilute the sample during the delivery with inert carrier gas which causes a ~5% reduction in concentration. The isotopic ratio measurements are not affected by this small dilution, but researchers are naturally interested accurate concentration measurements. We present the accuracy and precision of a new method of using this delivery module which we call 'double injection.' Two portions of the 40ml of the sample (20ml each) are introduced to the analyzer, the first injection of which flushes out the diluting gas and the second injection is measured. The accuracy of this new method is demonstrated by comparing the concentration and isotopic ratio measurements for a gas sampled directly and that same gas measured through the SSIM. The data show that the CO2 concentration measurements were the same within instrument precision. The isotopic ratio precision (1σ) of repeated measurements was 0.16 permil for CO2 and 1.15 permil for CH4 at ambient concentrations. This new method provides a significant enhancement in the information provided by small samples.

Experimental study of subaqueous, clay-rich, gravity flows

NASA Astrophysics Data System (ADS)

Marr, J.; Pratson, L.

2003-04-01

Recent laboratory experiments suggest a broad spectrum of flow and depositional behavior for compositionally varied subaqueous gravity flows. Dilute turbidity currents and cohesive debris flows are the end members of the spectrum. In this study we used geometrically scaled laboratory experiments to examine the flow dynamics and deposits associated with slurries of varying sediment composition. Slurries were composed of a mixture of tap water, kaolinite clay, 45 micron silt and 120 micron sand and were introduced into a 0.2m wide submerged channel. Slurry sediment concentrations ranged from 1-30% by volume. In all slurries, sediment was added in a ratio of 8:1:1 by volume of clay, silt, sand. A total volume of one cubic meter of slurry was used for each experiment and was introduced through a constant head tank allowing examination of sustained and steady gravity flow events lasting up to 5 minutes in duration. The dynamics of the flows (turbulence, hydroplaning, laminar shearing, etc.) were examined through the use of digital video cameras, dye injection tracking, high frequency sonar and visual observation. Vertical suspended sediment concentration and vertical grain size distributions were measured for each run from samples collected from siphon rakes. Deposit thicknesses and grain size distributions were measured from sediment samples taken from flow deposits. Rheological measurements and Atterberg limits of the slurries were made in an effort to link flow and depositional characteristics to bulk properties of the slurry mixture. The experiments show a clear linkage between the initial compositions of the slurries, their rheological properties, flow dynamics and deposits. Slurries with clay concentrations below 10% by volume appeared to be very turbulent. The silt and sand deposited during these events were transported along the bed as ripples. Flows between 10-20% sediment by volume appeared to be hybrid flows having both turbulent and non-turbulent elements. The surfaces of these deposits were flat and featureless. Slurries with sediment concentrations between 25-30% were clearly debris flows. They had distinguishable laminar flow and the deposit surfaces had both compression features and tension cracks.

Tracer techniques for urine volume determination and urine collection and sampling back-up system

NASA Technical Reports Server (NTRS)

Ramirez, R. V.

1971-01-01

The feasibility, functionality, and overall accuracy of the use of lithium were investigated as a chemical tracer in urine for providing a means of indirect determination of total urine volume by the atomic absorption spectrophotometry method. Experiments were conducted to investigate the parameters of instrumentation, tracer concentration, mixing times, and methods for incorporating the tracer material in the urine collection bag, and to refine and optimize the urine tracer technique to comply with the Skylab scheme and operational parameters of + or - 2% of volume error and + or - 1% accuracy of amount of tracer added to each container. In addition, a back-up method for urine collection and sampling system was developed and evaluated. This back-up method incorporates the tracer technique for volume determination in event of failure of the primary urine collection and preservation system. One chemical preservative was selected and evaluated as a contingency chemical preservative for the storage of urine in event of failure of the urine cooling system.

Electrokinetic sample preconcentration and hydrodynamic sample injection for microchip electrophoresis using a pneumatic microvalve.

PubMed

Cong, Yongzheng; Katipamula, Shanta; Geng, Tao; Prost, Spencer A; Tang, Keqi; Kelly, Ryan T

2016-02-01

A microfluidic platform was developed to perform online electrokinetic sample preconcentration and rapid hydrodynamic sample injection for zone electrophoresis using a single microvalve. The polydimethylsiloxane microchip comprises a separation channel, a side channel for sample introduction, and a control channel which is used as a pneumatic microvalve aligned at the intersection of the two flow channels. The closed microvalve, created by multilayer soft lithography, serves as a nanochannel preconcentrator under an applied electric potential, enabling current to pass through while preventing bulk flow. Once analytes are concentrated, the valve is briefly opened and the stacked sample is pressure injected into the separation channel for electrophoretic separation. Fluorescently labeled peptides were enriched by a factor of ∼450 in 230 s. This method enables both rapid analyte concentration and controlled injection volume for high sensitivity, high-resolution CE. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Improved aqueous scrubber for collection of soluble atmospheric trace gases

NASA Technical Reports Server (NTRS)

Cofer, W. R., III; Talbot, R. W.; Collins, V. G.

1985-01-01

A new concentration technique for the extraction and enrichment of water-soluble atmospheric trace gases has been developed. The gas scrubbing technique efficiently extracts soluble gases from a large volume flow rate of air sample into a small volume of refluxed trapping solution. The gas scrubber utilizes a small nebulizing nozzle that mixes the incoming air with an aqueous extracting solution to form an air/droplet mist. The mist provides excellent interfacial surface areas for mass transfer. The resulting mist sprays upward through the reaction chamber until it impinges upon a hydrophobic membrane that virtually blocks the passage of droplets but offers little resistance to the existing gas flow. Droplets containing the scrubbed gases coalesce on the membrane and drip back into the reservoir for further refluxing. After a suitable concentration period, the extracting solution containing the analyte can be withdrawn for analysis. The nebulization-reflex concentration technique is more efficient (maximum flow of gas through the minimum volume of extractant) than conventional bubbler/impinger gas extraction techniques and is offered as an alternative method.

Evaluation of analytical methodology for hydrocarbons in high pressure air and nitrogen systems. [evaluation of methodology

NASA Technical Reports Server (NTRS)

1977-01-01

Samples of liquid oxygen, high pressure nitrogen, low pressure nitrogen, and missile grade air were studied to determine the hydrocarbon concentrations. Concentration of the samples was achieved by adsorption on a molecular sieve and activated charcoal. The trapped hydrocarbons were then desorbed and transferred to an analytical column in a gas chromatograph. The sensitivity of the method depends on the volume of gas passed through the adsorbent tubes. The value of the method was verified through recoverability and reproducibility studies. The use of this method enables LOX, GN2, and missile grade air systems to be routinely monitored to determine low level increases in specific hydrocarbon concentration that could lead to potentially hazardous conditions.

Treatment of carprofen overdose with therapeutic plasma exchange in a dog.

PubMed

Kjaergaard, Astrid B; Davis, Jennifer L; Acierno, Mark J

2018-06-13

To report the use of therapeutic plasma exchange (TPE) in a dog with carprofen toxicosis. A 6-year-old female neutered Bichon Frise weighing 6.9 kg was examined after it had ingested 72 mg/kg carprofen. Mild dehydration without azotemia and with a urine specific gravity of 1.050 was noted at presentation. Treatment consisted of induction of emesis, symptomatic medical therapy, and TPE. The TPE achieved 1.5 plasma volume exchanges over 3 hours. Blood samples and effluent samples were collected every 30 minutes during TPE and additional blood samples were collected 11 and 35 hours after treatment. Carprofen concentrations in these samples were determined by high-pressure liquid chromatography. A 51% reduction in serum carprofen concentration was achieved following TPE. This report describes the successful reduction of plasma carprofen concentration in a dog using TPE. Although recent studies suggest that this particular dog may not have received a toxic dose, a 51% reduction of plasma carprofen concentration was achieved over 180 minutes, and TPE may be beneficial for treatment of dogs that have ingested higher doses. © Veterinary Emergency and Critical Care Society 2018.

Prevalence and concentration of Salmonella on raw shelled peanuts in the United States.

PubMed

Calhoun, Stephen; Post, Laurie; Warren, Benjamin; Thompson, Sterling; Bontempo, Ann Rogers

2013-04-01

Recalls and/or outbreaks associated with Salmonella contamination in peanut-containing products were reported over the past several years. There are very limited data available on the prevalence and concentration of Salmonella on raw shelled peanuts in the United States. The objectives of this study were to estimate the prevalence of Salmonella on raw shelled peanuts in the United States and to estimate that concentration of Salmonella. Samples of Runner- and Virginia-type raw shelled peanuts from the 2008, 2009, and 2010 crop years were proportionately sampled from each growing region, based on 2007 production volume. Of 944 raw shelled peanut samples (375 g each), 22 (2.33%) were positive for Salmonella by the VIDAS Salmonella assay. Salmonella serovars identified in this study included Agona, Anatum, Braenderup, Dessau, Hartford, Meleagridis, Muenchen, Rodepoort, Tennessee, and Tornow. The concentration levels of Salmonella in positive samples, as determined by a most-probable-number assay, were <0.03 to 2.4 MPN/g. These data will be useful when designing and validating processes for the reduction or elimination of Salmonella in peanuts and/or peanut-containing products.

Environmental assessment of a wood-waste-fired industrial watertube boiler. Volume 1. Technical results. Final report, March 1981-March 1984

DOE Office of Scientific and Technical Information (OSTI.GOV)

Castaldini, C.; Waterland, L.R.

1987-03-01

The two-volume report gives results from field tests of a wood-waste-fired industrial watertube boiler. Two series of tests were performed: one firing dry (11% moisture) wood waste, and the other firing green (34% moisture) wood waste. Emission measurements included: continuous monitoring of flue-gas emissions; source-assessment sampling system (SASS) sampling of the flue gas with subsequent laboratory analysis of samples to give total flue-gas organics in two boiling-point ranges, compound category information within these ranges, specific quantitation of the semi-volatile organic priority pollutants, and flue-gas concentrations of 73 trace elements; Method 5 sampling for particulate; controlled condensation system sampling for SO/submore » 2/ and SO/sub 3/; and grab sampling of boiler mechanical collector hopper ash for inorganic composition determinations. Total organic emissions decreased from 60-135 mg/dscm firing dry wood to 2-65 mg/dscm firing green wood, in parallel with corresponding boiler CO emissions.« less

Environmental assessment of a wood-waste-fired industrial watertube boiler. Volume 2. Data supplement. Final report, March 1981-March 1984

DOE Office of Scientific and Technical Information (OSTI.GOV)

Castaldini, C.; Waterland, L.R.

1987-03-01

The two-volume report gives results from field tests of a wood-waste-fired industrial watertube boiler. Two series of tests were performed: one firing dry (11% moisture) wood waste, and the other firing green (34% moisture) wood waste. Emission measurements included: continuous monitoring of flue-gas emissions; source-assessment sampling system (SASS) sampling of the flue-gas with subsequent laboratory analysis of samples to give total flue-gas organics in two boiling-point ranges, compound category information within these ranges, specific quantitation of the semi-volatile organic priority pollutants, and flue gas concentrations of 73 trace elements; Method 5 sampling for particulate; controlled condensation system sampling for SO/submore » 2/ and SO/sub 3/; and grab sampling of boiler mechanical collector hopper ash for inorganic and organic composition determinations. Total organic emissions decreased from 60-135 mg/dscm firing dry wood to 2-65 mg/dscm firing green wood, in parallel with corresponding boiler CO emissions.« less

Radiochemical sampling and analysis of shallow ground water and sediment at the BOMARC Missile Facility, east-central New Jersey, 1999-2000

USGS Publications Warehouse

Szabo, Zoltan; Zapecza, Otto S.; Oden, Jeannette H.; Rice, Donald E.

2005-01-01

A field sampling experiment was designed using low-flow purging with a portable pump and sample-collection equipment for the collection of water and sediment samples from observation wells screened in the Kirkwood-Cohansey aquifer system to determine radionuclide or trace-element concentrations for various size fractions. Selected chemical and physical characteristics were determined for water samples from observation wells that had not been purged for years. The sampling was designed to define any particulate, colloidal, and solution-phase associations of radionuclides or trace elements in ground water by means of filtration and ultrafiltration techniques. Turbidity was monitored and allowed to stabilize before samples were collected by means of the low-flow purging technique rather than by the traditional method of purging a fixed volume of water at high-flow rates from the observation well. A minimum of four water samples was collected from each observation well. The samples of water from each well were collected in the following sequence. (1) A raw unfiltered sample was collected within the first minutes of pumping. (2) A raw unfiltered sample was collected after at least three casing volumes of water were removed and turbidity stabilized. (3) A sample was collected after the water was filtered with a 0.45-micron filter. (4) A sample was collected after the water passed through a 0.45-micron filter and a 0.003-micron tangential-flow ultrafilter in sequence. In some cases, a fifth sample was collected after the water passed through a 0.45-micron filter and a 0.05-micron filter in sequence to test for colloids of 0.003 microns to 0.05 microns in size. The samples were analyzed for the concentration of manmade radionuclides plutonium-238 and -239 plus -240, and americium-241. The samples also were analyzed for concentrations of uranium-234, -235, and -238 to determine whether uranium-234 isotope enrichment (resulting from industrial processing) is present. A subset of samples was analyzed for concentrations of thorium-232, -230, and -228 to determine if thorium-228 isotope enrichment, also likely to result from industrial processing, is present. Concentrations of plutonium isotopes and americium-241 in the water samples were less than 0.1 picocurie per liter, the laboratory reporting level for these manmade radionuclides, with the exception of one americium-241 concentration from a filtered sample. A sequential split sample from the same well did not contain a detectable concentration of americium-241, however. Other filtered and unfiltered samples of water from the same well did not contain quantities of americium-241 nearly as high as 0.1 pCi/L. Therefore, the presence of americium-241 in a quantifiable concentration in water samples from this well could not be confirmed. Neither plutonium nor americium was detected in samples of settled sediment collected from the bottom of the wells. Concentrations of uranium isotopes (maximum of 0.05 and 0.08 picocuries per liter of uranium-238 and uranium-234, respectively) were measurable in unfiltered samples of turbid water from one well and in the settled bottom sediment from 6 wells (maximum concentrations of 0.25 and 0.20 picocuries per gram of uranium-238 and uranium-234, respectively). The uranium-234/uranium-238 isotopic ratio was near 1:1, which indicates natural uranium. The analytical results, therefore, indicate that no manmade radionuclide contamination is present in any of the well-bottom sediments, or unfiltered or filtered water samples from any of the sampled wells. No evidence of manmade radionuclide contamination was observed in the aquifer as settled or suspended particulates, colloids, or in the dissolved phase.

Standardization and performance evaluation of "modified" and "ultrasensitive" versions of the Abbott RealTime HIV-1 assay, adapted to quantify minimal residual viremia.

PubMed

Amendola, Alessandra; Bloisi, Maria; Marsella, Patrizia; Sabatini, Rosella; Bibbò, Angela; Angeletti, Claudio; Capobianchi, Maria Rosaria

2011-09-01

Numerous studies investigating clinical significance of HIV-1 minimal residual viremia (MRV) suggest potential utility of assays more sensitive than those routinely used to monitor viral suppression. However currently available methods, based on different technologies, show great variation in detection limit and input plasma volume, and generally suffer from lack of standardization. In order to establish new tools suitable for routine quantification of minimal residual viremia in patients under virological suppression, some modifications were introduced into standard procedure of the Abbott RealTime HIV-1 assay leading to a "modified" and an "ultrasensitive" protocols. The following modifications were introduced: calibration curve extended towards low HIV-1 RNA concentration; 4 fold increased sample volume by concentrating starting material; reduced volume of internal control; adoption of "open-mode" software for quantification. Analytical performances were evaluated using the HIV-1 RNA Working Reagent 1 for NAT assays (NIBSC). Both tests were applied to clinical samples from virologically suppressed patients. The "modified" and the "ultrasensitive" configurations of the assay reached a limit of detection of 18.8 (95% CI: 11.1-51.0 cp/mL) and 4.8 cp/mL (95% CI: 2.6-9.1 cp/mL), respectively, with high precision and accuracy. In clinical samples from virologically suppressed patients, "modified" and "ultrasensitive" protocols allowed to detect and quantify HIV RNA in 12.7% and 46.6%, respectively, of samples resulted "not-detectable", and in 70.0% and 69.5%, respectively, of samples "detected <40 cp/mL" in the standard assay. The "modified" and "ultrasensitive" assays are precise and accurate, and easily adoptable in routine diagnostic laboratories for measuring MRV. Copyright © 2011 Elsevier B.V. All rights reserved.

A study of uniformity of elements deposition on glass fiber filters after collection of airborne particulate matter (PM-10), using a high-volume sampler.

PubMed

Marrero, Julieta; Rebagliati, Raúl Jiménez; Gómez, Darío; Smichowski, Patricia

2005-12-15

A study was conducted to evaluate the homogeneity of the distribution of metals and metalloids deposited on glass fiber filters collected using a high-volume sampler equipped with a PM-10 sampling head. The airborne particulate matter (APM)-loaded glass fiber filters (with an active surface of about 500cm(2)) were weighed and then each filter was cut in five small discs of 6.5cm of diameter. Each disk was mineralized by acid-assisted microwave (MW) digestion using a mixture of nitric, perchloric and hydrofluoric acids. Analysis was performed by axial view inductively coupled plasma optical emission spectrometry (ICP OES) and the elements considered were: Al, As, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Sb, Ti and V. The validation of the procedure was performed by the analysis of the standard reference material NIST 1648, urban particulate matter. As a way of comparing the possible variability in trace elements distribution in a particular filter, the mean concentration for each element over the five positions (discs) was calculated and each element concentration was normalized to this mean value. Scatter plots of the normalized concentrations were examined for all elements and all sub-samples. We considered that an element was homogeneously distributed if its normalized concentrations in the 45 sub-samples were within +/-15% of the mean value ranging between 0.85 and 1.15. The study demonstrated that the 12 elements tested showed different distribution pattern. Aluminium, Cu and V showed the most homogeneous pattern while Cd and Ni exhibited the largest departures from the mean value in 13 out of the 45 discs analyzed. No preferential deposition was noticed in any sub-sample.

Effects of equipment performance on data quality from the National Atmospheric Deposition Program/National Trends Network and the Mercury Deposition Network

USGS Publications Warehouse

Wetherbee, Gregory A.; Rhodes, Mark F.

2013-01-01

The U.S. Geological Survey Branch of Quality Systems operates the Precipitation Chemistry Quality Assurance project (PCQA) to provide independent, external quality-assurance for the National Atmospheric Deposition Program (NADP). NADP is composed of five monitoring networks that measure the chemical composition of precipitation and ambient air. PCQA and the NADP Program Office completed five short-term studies to investigate the effects of equipment performance with respect to the National Trends Network (NTN) and Mercury Deposition Network (MDN) data quality: sample evaporation from NTN collectors; sample volume and mercury loss from MDN collectors; mercury adsorption to MDN collector glassware, grid-type precipitation sensors for precipitation collectors, and the effects of an NTN collector wind shield on sample catch efficiency. Sample-volume evaporation from an NTN Aerochem Metrics (ACM) collector ranged between 1.1–33 percent with a median of 4.7 percent. The results suggest that weekly NTN sample evaporation is small relative to sample volume. MDN sample evaporation occurs predominantly in western and southern regions of the United States (U.S.) and more frequently with modified ACM collectors than with N-CON Systems Inc. collectors due to differences in airflow through the collectors. Variations in mercury concentrations, measured to be as high as 47.5 percent per week with a median of 5 percent, are associated with MDN sample-volume loss. Small amounts of mercury are also lost from MDN samples by adsorption to collector glassware irrespective of collector type. MDN 11-grid sensors were found to open collectors sooner, keep them open longer, and cause fewer lid cycles than NTN 7-grid sensors. Wind shielding an NTN ACM collector resulted in collection of larger quantities of precipitation while also preserving sample integrity.

A diurnal component to the variation in sieve tube amino acid content in wheat.

PubMed

Gattolin, Stefano; Newbury, H John; Bale, Jeffrey S; Tseng, Hua-Ming; Barrett, David A; Pritchard, Jeremy

2008-06-01

We have used high-sensitivity capillary electrophoresis coupled to a laser-induced fluorescence detection method to quantify 16 amino acids in wheat (Triticum aestivum) sieve tube (ST) samples as small as 2 nL collected by severing the stylets of feeding aphids. The sensitivity of the method was sufficient to determine a quantitative amino acid profile of individual STs without the need to bulk samples to produce larger volumes for analysis. This allowed the observation of the full range of variation that exists in individual STs. Some of the total concentrations of amino acids recorded are higher than those reported previously. The results obtained show variation in the concentrations of phenylalanine (Phe), histidine/valine (His/Val), leucine/isoleucine (Leu/Ile), arginine, asparagine, glutamine, tyrosine (Tyr), and lysine (Lys) across the ST samples. These could not be explained by plant-to-plant variation. Statistical analyses revealed five analytes (Tyr, Lys, Phe, His/Val, and Leu/Ile) that showed striking covariation in their concentrations across ST samples. A regression analysis revealed a significant relationship between the concentrations of Tyr, Lys, Phe, Leu/Ile, His/Val, asparagine, arginine, and proline and the time of collection of ST samples, with these amino acids increasing in concentration during the afternoon. This increase was confirmed to occur in individual STs by analyzing samples obtained from stylet bundles exuding for many hours. Finally, an apparent relationship between the exudation rate of ST sap and its total amino acid concentration was observed: samples containing higher total amino acid concentrations were observed to exude from the severed stylet bundles more slowly.

40 CFR 60.316 - Test methods and procedures.

Code of Federal Regulations, 2010 CFR

2010-07-01

... Section 60.316 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS... for the measurement of VOC concentration. (3) Method 1 for sample and velocity traverses. (4) Method 2... smaller volumes, when necessitated by process variables or other factors, may be approved by the...

Use of marker ion and cationic surfactant plastic membrane electrode for potentiometric titration of cationic polyelectrolytes.

PubMed

Masadome, Takashi; Imato, Toshihiko

2003-07-04

A plasticized poly (vinyl chloride) (PVC) membrane electrode sensitive to stearyltrimethylammonium (STA) ion is applied to the determination of cationic polyelectrolytes such as poly (diallyldimethylammonium chloride) (Cat-floc) by potentiometric titration, using a potassium poly (vinyl sulfate) (PVSK) solution as a titrant. The end-point of the titration is detected as the potential change of the plasticized PVC membrane electrode caused by decrease in the concentration of STA ion added to the sample solution as a marker ion due to the ion association reaction between the STA ion and PVSK. The effects of the concentration of STA ion, coexisting electrolytes in the sample solution and pH of the sample on the degree of the potential change at the end-point were examined. A linear relationship between the concentration of cationic polyelectrolyte and the end-point volume of the titrant exists in the concentration range from 2x10(-5) to 4x10(-4) N for Cat-floc, glycol chitosan, and methylglycol chitosan.

Fate of pharmaceutical and trace organic compounds in three septic system plumes, Ontario, Canada.

PubMed

Carrara, Cherilyn; Ptacek, Carol J; Robertson, William D; Blowes, David W; Moncur, Michael C; Sverko, Ed; Backus, Sean

2008-04-15

Three high volume septic systems in Ontario, Canada, were examined to assess the potential for onsite wastewatertreatment systems to release pharmaceutical compounds to the environment and to evaluate the mobility of these compounds in receiving aquifers. Wastewater samples were collected from the septic tanks, and groundwater samples were collected below and down gradient of the infiltration beds and analyzed for a suite of commonly used pharmaceutical and trace organic compounds. The septic tank samples contained elevated concentrations of several pharmaceutical compounds. Ten of the 12 compounds analyzed were detected in groundwater at one or more sites at concentrations in the low ng L(-1) to low microg L(-1) range. Large differences among the sites were observed in both the number of detections and the concentrations of the pharmaceutical compounds. Of the compounds analyzed, ibuprofen, gemfibrozil, and naproxen were observed to be transported atthe highest concentrations and greatest distances from the infiltration source areas, particularly in anoxic zones of the plumes.

Ambient air concentrations of PCDDs, PCDFs, coplanar PCBs, and PAHs at the Mississippi Sandhill Crane National Wildlife Refuge, Jackson County, Mississippi

USGS Publications Warehouse

White, D.H.; Hardy, J.W.

1994-01-01

Our objective was to determine the levels of selected airborne contaminants in ambient air at the Mississippi Sandhill Crane National Wildlife Refuge, Mississippi, that might be affecting the health of endangered cranes living there. Two high-volume air samplers were operated at separate locations on the Refuge during May?September 1991. The sampling media were micro-quartz filters in combination with polyurethane foam plugs. Composite bimonthly samples from each station were analyzed for polychlorinated dibenzo-p-dioxins (PCDDs), dibenzofurans (PCDFs), coplanar polychlorinated biphenyls (PCBs), and polycyclic aromatic hydrocarbons (PAHs). Overall, residue concentrations were low. The toxic PCDD isomer 2,3,7,8-tetra-CDD was not detected, nor was penta-CDD. There was no difference (P>0.05) in residue concentrations between stations or over time and meteorological parameters were not correlated with residue concentrations. Because contaminant levels and patterns may differ seasonally, we recommend that air samples collected during winter months also be analyzed for these same chemical groups.

Dehydration, hemodynamics and fluid volume optimization after induction of general anesthesia.

PubMed

Li, Yuhong; He, Rui; Ying, Xiaojiang; Hahn, Robert G

2014-01-01

Fluid volume optimization guided by stroke volume measurements reduces complications of colorectal and high-risk surgeries. We studied whether dehydration or a strong hemodynamic response to general anesthesia increases the probability of fluid responsiveness before surgery begins. Cardiac output, stroke volume, central venous pressure and arterial pressures were measured in 111 patients before general anesthesia (baseline), after induction and stepwise after three bolus infusions of 3 ml/kg of 6% hydroxyethyl starch 130/0.4 (n=86) or Ringer's lactate (n=25). A subgroup of 30 patients who received starch were preloaded with 500 ml of Ringer's lactate. Blood volume changes were estimated from the hemoglobin concentration and dehydration was estimated from evidence of renal water conservation in urine samples. Induction of anesthesia decreased the stroke volume to 62% of baseline (mean); administration of fluids restored this value to 84% (starch) and 68% (Ringer's). The optimized stroke volume index was clustered around 35-40 ml/m2/beat. Additional fluid boluses increased the stroke volume by ≥10% (a sign of fluid responsiveness) in patients with dehydration, as suggested by a low cardiac index and central venous pressure at baseline and by high urinary osmolality, creatinine concentration and specific gravity. Preloading and the hemodynamic response to induction did not correlate with fluid responsiveness. The blood volume expanded 2.3 (starch) and 1.8 (Ringer's) times over the infused volume. Fluid volume optimization did not induce a hyperkinetic state but ameliorated the decrease in stroke volume caused by anesthesia. Dehydration, but not the hemodynamic response to the induction, was correlated with fluid responsiveness.

Pollutant deposition via dew in urban and rural environment, Cracow, Poland

NASA Astrophysics Data System (ADS)

Muskała, Piotr; Sobik, Mieczysław; Błaś, Marek; Polkowska, Żaneta; Bokwa, Anita

2015-01-01

This study is a comparative analysis of dew in rural and urban environment. Dew samples were collected between May and October, 2009 in two reference stations in southern Poland: Cracow and Gaik-Brzezowa. The investigation included comparison of volume and chemistry of the collected samples. Due to its formation mechanisms, dew is a good indicator of air pollution. Following parameters were analyzed in 159 collected samples: pH, electric conductivity, concentration of formaldehyde and phenols, concentration of NH4+, Ca2 +, K+, Na+, and Mg2 + cations and NO2-, NO3-, SO42 -, Cl-, F-, and PO43 - anions. The frequency of dew was approximately the same, both in urban and rural conditions reaching 43% of the measurement period. Dew intensity, expressed by volume, was on average two times larger in rural environment than in urban conditions. Urban landuse was recognized as the main factor reducing dew intensity in the urban station in comparison to the rural. Furthermore, the intensity of dew depended on synoptic scale air circulation at both measurement sites. As expected, samples collected in Cracow were much more polluted than the ones from Gaik-Brzezowa. The average TIC (Total Ionic Content) parameter was approximately 50% higher at the urban station. The pH in the rural station was more acidic. NO3- anions and Ca2 + cations were predominant in both measurement sites, however the participation of Ca2 + in Cracow was higher. NO3- indicates pollutions emitted by transport and industrial sources. The concentration of the analytes in both stations, as the volume, depended on air circulation direction. For Gaik-Brzezowa the highest TIC was observed mainly within southern circulation, while for Cracow the highest TIC was noted within both northern and southern. In general the rural station represented background pollution for the whole region and the pollution in Cracow was more dependent on local urban sources as transport or industry.

An assessment of the variability in performance of wet atmospheric deposition samplers

USGS Publications Warehouse

Graham, R.C.; Robertson, J.K.; Obal, John

1987-01-01

The variability in performance of two brands of wet/dry atmospheric deposition samplers were compared for 1 year at a sincle site. A total of nine samplers were used. Samples were collected weekly and analyzed for pH, specific conductance, common chemical constituents, and sample volume. Additionally, data on the duration of each sampler opening were recorded using a microdatalogger. These data disprove the common perception that samplers remain open throughout a precipitation event. The sensitivity of sampler sensors within the range tested did not have a defineable impact on sample collection. The nonnormal distribution within the data set necessitated application of the nonparametric Friedman Test to assess comparability of sample chemical composition and volume between and within sampler brands. Statistically significant differences existed for most comparisons, however the test did not permit quantification of their magnitudes. Differences in analyte concentrations between samplers were small. (USGS)

Freeze-Drying as Sample Preparation for Micellar Electrokinetic Capillary Chromatography – Electrochemical Separations of Neurochemicals in Drosophila Brains

PubMed Central

Berglund, E. Carina; Kuklinski, Nicholas J.; Karagündüz, Ekin; Ucar, Kubra; Hanrieder, Jörg; Ewing, Andrew G.

2013-01-01

Micellar electrokinetic capillary chromatography with electrochemical detection has been used to quantify biogenic amines in freeze-dried Drosophila melanogaster brains. Freeze drying samples offers a way to preserve the biological sample while making dissection of these tiny samples easier and faster. Fly samples were extracted in cold acetone and dried in a rotary evaporator. Extraction and drying times were optimized in order to avoid contamination by red-pigment from the fly eyes and still have intact brain structures. Single freeze-dried fly-brain samples were found to produce representative electropherograms as a single hand-dissected brain sample. Utilizing the faster dissection time that freeze drying affords, the number of brains in a fixed homogenate volume can be increased to concentrate the sample. Thus, concentrated brain samples containing five or fifteen preserved brains were analyzed for their neurotransmitter content, and five analytes; dopamine N-acetyloctopamine, Nacetylserotonin, N-acetyltyramine, N-acetyldopamine were found to correspond well with previously reported values. PMID:23387977

Apparatus and process for microbial detection and enumeration

NASA Technical Reports Server (NTRS)

Wilkins, J. R.; Grana, D. (Inventor)

1982-01-01

An apparatus and process for detecting and enumerating specific microorganisms from large volume samples containing small numbers of the microorganisms is presented. The large volume samples are filtered through a membrane filter to concentrate the microorganisms. The filter is positioned between two absorbent pads and previously moistened with a growth medium for the microorganisms. A pair of electrodes are disposed against the filter and the pad electrode filter assembly is retained within a petri dish by retainer ring. The cover is positioned on base of petri dish and sealed at the edges by a parafilm seal prior to being electrically connected via connectors to a strip chart recorder for detecting and enumerating the microorganisms collected on filter.

Selenium analysis by an integrated microwave digestion-needle trap device with hydride sorption on carbon nanotubes and electrothermal atomic absorption spectrometry determination

NASA Astrophysics Data System (ADS)

Maratta Martínez, Ariel; Vázquez, Sandra; Lara, Rodolfo; Martínez, Luis Dante; Pacheco, Pablo

2018-02-01

An integrated microwave assisted digestion (MW-AD) - needle trap device (NTD) for selenium determination in grape pomace samples is presented. The NTD was filled with oxidized multiwall carbon nanotubes (oxMWCNTS) where Se hydrides were preconcentrated. Determination was carried out by flow injection-electrothermal atomic absorption spectrometry (FI-ETAAS). The variables affecting the system were established by a multivariate design (Plackett Burman), indicating that the following variables significantly affect the system: sample amount, HNO3 digestion solution concentration, NaBH4 volume and elution volume. A Box-Behnken design was implemented to determine the optimized values of these variables. The system improved Se atomization in the graphite furnace, since only trapped hydrides reached the graphite furnace, and the pyrolysis stage was eliminated according to the aqueous matrix of the eluate. Under optimized conditions the system reached a limit of quantification of 0.11 μg kg- 1, a detection limit of 0.032 μg kg- 1, a relative standard deviation of 4% and a preconcentration factor (PF) of 100, reaching a throughput sample of 5 samples per hour. Sample analysis show Se concentrations between 0.34 ± 0.03 μg kg- 1 to 0.48 ± 0.03 μg kg- 1 in grape pomace. This system provides minimal reagents and sample consumption, eliminates discontinuous stages between samples processing reaching a simpler and faster Se analysis.

Sample preconcentration with chemical derivatization in capillary electrophoresis. Capillary as preconcentrator, microreactor and chiral selector for high-throughput metabolite screening.

PubMed

Ptolemy, Adam S; Britz-McKibbin, Philip

2006-02-17

New strategies for integrating sample pretreatment with chemical analyses under a single format is required for rapid, sensitive and enantioselective analyses of low abundance metabolites in complex biological samples. Capillary electrophoresis (CE) offers a unique environment for controlling analyte/reagent band dispersion and electromigration properties using discontinuous electrolyte systems. Recent work in our laboratory towards developing a high-throughput CE platform for low abundance metabolites via on-line sample preconcentration with chemical derivatization (SPCD) is primarily examined in this review, as there have been surprisingly only a few strategies reported in the literature to date. In-capillary sample preconcentration serves to enhance concentration sensitivity via electrokinetic focusing of long sample injection volumes for lower detection limits, whereas chemical derivatization by zone passing is used to expand detectability and selectivity, notably for enantiomeric resolution of metabolites lacking intrinsic chromophores using nanolitre volumes of reagent. Together, on-line SPCD-CE can provide over a 100-fold improvement in concentration sensitivity, shorter total analysis times, reduced sample handling and improved reliability for a variety of amino acid and amino sugar metabolites, which is also amenable to automated high-throughput screening. This review will highlight basic method development and optimization parameters relevant to SPCD-CE, including applications to bacterial metabolite flux and biomarker analyses. Insight into the mechanism of analyte focusing and labeling by SPCD-CE is also discussed, as well as future directions for continued research.

The effect of membrane filtration on dissolved trace element concentrations

USGS Publications Warehouse

Horowitz, A.J.; Lum, K.R.; Garbarino, J.R.; Hall, G.E.M.; Lemieux, C.; Demas, C.R.

1996-01-01

The almost universally accepted operational definition for dissolved constituents is based on processing whole-water samples through a 0.45-??m membrane filter. Results from field and laboratory experiments indicate that a number of factors associated with filtration, other than just pore size (e.g., diameter, manufacturer, volume of sample processed, amount of suspended sediment in the sample), can produce substantial variations in the 'dissolved' concentrations of such elements as Fe, Al, Cu, Zn, Pb, Co, and Ni. These variations result from the inclusion/exclusion of colloidally- associated trace elements. Thus, 'dissolved' concentrations quantitated by analyzing filtrates generated by processing whole-water through similar pore- sized membrane filters may not be equal/comparable. As such, simple filtration through a 0.45-??m membrane filter may no longer represent an acceptable operational definition for dissolved chemical constituents. This conclusion may have important implications for environmental studies and regulatory agencies.

Method development for the analysis of N-nitrosodimethylamine and other N-nitrosamines in drinking water at low nanogram/liter concentrations using solid-phase extraction and gas chromatography with chemical ionization tandem mass spectrometry.

PubMed

Munch, Jean W; Bassett, Margarita V

2006-01-01

N-nitrosodimethylamine (NDMA) is a probable human carcinogen of concern that has been identified as a drinking water contaminant. U.S. Environmental Protection Agency Method 521 has been developed for the analysis of NDMA and 6 additional N-nitrosamines in drinking water at low ng/L concentrations. The method uses solid-phase extraction with coconut charcoal as the sorbent and dichloromethane as the eluent to concentrate 0.50 L water samples to 1 mL. The extracts are analyzed by gas chromatography-chemical ionization tandem mass spectrometry using large-volume injection. Method performance was evaluated in 2 laboratories. Typical analyte recoveries of 87-104% were demonstrated for fortified reagent water samples, and recoveries of 77-106% were demonstrated for fortified drinking water samples. All relative standard deviations on replicate analyses were < 11%.

A rapid high-performance liquid-chromatographic method for simultaneously determining the concentrations of TFM and Bayer 73 in water during lampricide treatments

USGS Publications Warehouse

Dawson, V.K.

1982-01-01

The high-performance liquid-chromatography (HPLC) procedure requires only minutes per sample, is specific, and is relatively sensitive (limit of detection 18 disposable cartridge. The cartridge adsorbs and retains both the lampricides and the internal standard. The quantitative elution of the three chemicals from the cartridge with a small volume of methanol effectively concentrates the sample and provides sample cleanup. The methanol extract is then analyzed directly by HPLC on an MCH 10 reverse phase column by using a methanol:0.01 mol/L acetate buffer (87:13, v:v) as the mobile phase at 2 mL/min and detected by ultraviolet spectrophotometry at 330 (or 254) nm. A microprocessor data system further facilitates the procedure by quantifying off-scale peaks and yielding results directly in units of concentration (mg/L).

Transient Method for Determining Indoor Chemical Concentrations Based on SPME: Model Development and Calibration.

PubMed

Cao, Jianping; Xiong, Jianyin; Wang, Lixin; Xu, Ying; Zhang, Yinping

2016-09-06

Solid-phase microextraction (SPME) is regarded as a nonexhaustive sampling technique with a smaller extraction volume and a shorter extraction time than traditional sampling techniques and is hence widely used. The SPME sampling process is affected by the convection or diffusion effect along the coating surface, but this factor has seldom been studied. This paper derives an analytical model to characterize SPME sampling for semivolatile organic compounds (SVOCs) as well as for volatile organic compounds (VOCs) by considering the surface mass transfer process. Using this model, the chemical concentrations in a sample matrix can be conveniently calculated. In addition, the model can be used to determine the characteristic parameters (partition coefficient and diffusion coefficient) for typical SPME chemical samplings (SPME calibration). Experiments using SPME samplings of two typical SVOCs, dibutyl phthalate (DBP) in sealed chamber and di(2-ethylhexyl) phthalate (DEHP) in ventilated chamber, were performed to measure the two characteristic parameters. The experimental results demonstrated the effectiveness of the model and calibration method. Experimental data from the literature (VOCs sampled by SPME) were used to further validate the model. This study should prove useful for relatively rapid quantification of concentrations of different chemicals in various circumstances with SPME.

A new method for depth profiling reconstruction in confocal microscopy

NASA Astrophysics Data System (ADS)

Esposito, Rosario; Scherillo, Giuseppe; Mensitieri, Giuseppe

2018-05-01

Confocal microscopy is commonly used to reconstruct depth profiles of chemical species in multicomponent systems and to image nuclear and cellular details in human tissues via image intensity measurements of optical sections. However, the performance of this technique is reduced by inherent effects related to wave diffraction phenomena, refractive index mismatch and finite beam spot size. All these effects distort the optical wave and cause an image to be captured of a small volume around the desired illuminated focal point within the specimen rather than an image of the focal point itself. The size of this small volume increases with depth, thus causing a further loss of resolution and distortion of the profile. Recently, we proposed a theoretical model that accounts for the above wave distortion and allows for a correct reconstruction of the depth profiles for homogeneous samples. In this paper, this theoretical approach has been adapted for describing the profiles measured from non-homogeneous distributions of emitters inside the investigated samples. The intensity image is built by summing the intensities collected from each of the emitters planes belonging to the illuminated volume, weighed by the emitters concentration. The true distribution of the emitters concentration is recovered by a new approach that implements this theoretical model in a numerical algorithm based on the Maximum Entropy Method. Comparisons with experimental data and numerical simulations show that this new approach is able to recover the real unknown concentration distribution from experimental profiles with an accuracy better than 3%.

Grey matter, an endophenotype for schizophrenia? A voxel-based morphometry study in siblings of patients with schizophrenia

PubMed Central

van der Velde, Jorien; Gromann, Paula M.; Swart, Marte; de Haan, Lieuwe; Wiersma, Durk; Bruggeman, Richard; Krabbendam, Lydia; Aleman, André

2015-01-01

Background Grey matter, both volume and concentration, has been proposed as an endophenotype for schizophrenia given a number of reports of grey matter abnormalities in relatives of patients with schizophrenia. However, previous studies on grey matter abnormalities in relatives have produced inconsistent results. The aim of the present study was to examine grey matter differences between controls and siblings of patients with schizophrenia and to examine whether the age, genetic loading or subclinical psychotic symptoms of selected individuals could explain the previously reported inconsistencies. Methods We compared the grey matter volume and grey matter concentration of healthy siblings of patients with schizophrenia and healthy controls matched for age, sex and education using voxel-based morphometry (VBM). Furthermore, we selected subsamples based on age (< 30 yr), genetic loading and subclinical psychotic symptoms to examine whether this would lead to different results. Results We included 89 siblings and 69 controls in our study. The results showed that siblings and controls did not differ significantly on grey matter volume or concentration. Furthermore, specifically selecting participants based on age, genetic loading or subclinical psychotic symptoms did not alter these findings. Limitations The main limitation was that subdividing the sample resulted in smaller samples for the subanalyses. Furthermore, we used MRI data from 2 different scanner sites. Conclusion These results indicate that grey matter measured through VBM might not be a suitable endophenotype for schizophrenia. PMID:25768029

Concentration Measurements of Suspended Load using ADV with Influence of the Particle Size

NASA Astrophysics Data System (ADS)

Schwarzwälder, Kordula

2017-04-01

ADV backscatter data can be used under certain conditions to gain information about the concentrations of suspended loads. This was shown in many studies before (Fugate and Friedrichs 2002; Chanson et al 2008; Ha et al. 2009). This paper reports on a pre-study to investigate the influence of particle size on concentration measurements for suspended sediment load with ADV. The study was conducted in a flume in the Oskar-von-Miller-Institute using fresh water from a river including the natural suspended load. The ADV used in the experiments was a Vectrino Profiler (Nortek). In addition water samples were taken for TSS and TOC. For the measurements a surge was generated in the flume to ensure that also particles of larger size will be present in the water phase. The measurements and samples were taken during the whole surge event. Therefore we were able to find a good correlation between the backscatter data of the ADV and the TSS as well as TOC results. For the decreasing part of the flow event the concentration of TOC in the suspended load of the water phase is decreasing much slower than the TSS and results in a damped decrease of the backscatter values. This means that the results for concentration measurements might be slightly influenced by the size of the particles. Further evaluations of measurements conducted with a LISST SL (Sequoia) will be investigated to show the trend of the particle sizes during this process and fortify this result. David C. Fugate, Carl T. Friedrichs, Determining concentration and fall velocity of estuarine particle populations using ADV, OBS and LISST, Continental Shelf Research, Volume 22, Issues 11-13, 2002 H.K. Ha, W.-Y. Hsu, J.P.-Y. Maa, Y.Y. Shao, C.W. Holland, Using ADV backscatter strength for measuring suspended cohesive sediment concentration, Continental Shelf Research, Volume 29, Issue 10, 2009 Hubert Chanson, Maiko Takeuchi, Mark Trevethan, Using turbidity and acoustic backscatter intensity as surrogate measures of suspended sediment concentration in a small subtropical estuary, Journal of Environmental Management, Volume 88, Issue 4, 2008

Taking alcohol by deception: an analysis of ethanol concentration of "paraga" an alcoholic herbal mixture in Nigeria

PubMed Central

2012-01-01

Background Alcohol related road traffic injuries are on the rise in Nigeria. A sizable proportion of the alcohol intake is disguised as herbal medicines which are commonly available at motor parks in most urban centres. This study aims to determine the ethanol concentration of the herbal preparations and the vendors' knowledge about their preparation and use. Twenty-eight samples of the paraga mixtures were obtained for analysis from 22 paraga vendors. The vendors were interviewed in the motor parks using a semi-structured questionnaire. Results All the paraga outlets were located in or near motor parks. Commercial motor drivers and motorcyclists accounted for most customers. There were no formal recipes, production involved no calibrations or weighing and thus the components and concentration of different batches varied. The alcohol by volume (ABV) of the samples ranged between 1.20% and 20.84%. Nine samples were weaker than beers (Alcohol By Volume (ABV) of 1-3.1%). Ten were equivalent to beer (ABV:3-8%) and the rest were equivalent to wine (ABV:8-12%) or stronger (ABV: 18-20%). Conclusions Paraga should be classified as alcoholic beverages, and its sale restricted as such. The production should come under scrutiny, because the haphazard ways they are prepared may pose other health risks apart from those due to their alcoholic contents. PMID:22394987

Taking alcohol by deception: an analysis of ethanol concentration of "paraga" an alcoholic herbal mixture in Nigeria.

PubMed

Kehinde, Oluwadiya S; Adegoke, Akinola E

2012-03-06

Alcohol related road traffic injuries are on the rise in Nigeria. A sizable proportion of the alcohol intake is disguised as herbal medicines which are commonly available at motor parks in most urban centres. This study aims to determine the ethanol concentration of the herbal preparations and the vendors' knowledge about their preparation and use. Twenty-eight samples of the paraga mixtures were obtained for analysis from 22 paraga vendors. The vendors were interviewed in the motor parks using a semi-structured questionnaire. All the paraga outlets were located in or near motor parks. Commercial motor drivers and motorcyclists accounted for most customers. There were no formal recipes, production involved no calibrations or weighing and thus the components and concentration of different batches varied. The alcohol by volume (ABV) of the samples ranged between 1.20% and 20.84%. Nine samples were weaker than beers (Alcohol By Volume (ABV) of 1-3.1%). Ten were equivalent to beer (ABV:3-8%) and the rest were equivalent to wine (ABV:8-12%) or stronger (ABV: 18-20%). Paraga should be classified as alcoholic beverages, and its sale restricted as such. The production should come under scrutiny, because the haphazard ways they are prepared may pose other health risks apart from those due to their alcoholic contents.

A Modified LC/MS/MS Method with Enhanced Sensitivity for the Determination of Scopolamine in Human Plasma

NASA Technical Reports Server (NTRS)

Wang, Zuwei; Vaksman, Zalman; Putcha, Lakshmi

2008-01-01

Intranasal scopolamine is a choice drug for the treatment of motion sickness during space flight because of its quick onset of action, short half-life and favorable sideeffects profile. The dose administered usually ranges between 0.1 and 0.4 mg. Such small doses make it difficult to detect concentrations of scopolamine in biological fluids using existing sensitive LC/MS/MS method, especially when the biological sample volumes are limited. To measure scopolamine in human plasma to facilitate pharmacokinetic evaluation of the drug, we developed a sensitive LC/MS/MS method using 96 well micro elution plates for solid phase extraction (SPE) of scopolamine in human plasma. Human plasma (100-250 micro L) were loaded onto Waters Oasis HLB 96 well micro elution plate and eluted with 50 L of organic solvent without evaporation and reconstitution. HPLC separation of the eluted sample was performed using an Agilent Zorbax SB-CN column (50 x 2.1 mm) at a flow rate of 0.2 mL/min for 3 minutes. The mobile phase for separation was 80:20 (v/v) methanol: ammonium acetate (30 mM) in water. Concentrations of scopolamine were determined using a Micromass Quattro Micro(TM) mass spectrometer with electrospray ionization (ESI). ESI mass spectra were acquired in positive ion mode with multiple reaction monitoring for the determination of scopolamine m/z = 304.2 right arrow 138.1 and internal standard hyoscyamine m/z = 290.2 right arrow 124.1. The method is rapid, reproducible, specific and has the following parameters: scopolamine and the IS are eluted at about 1.1 and 1.7 min respectively. The linear range is 25-10000 pg/mL for scopolamine in human plasma with correlation coefficients greater than 0.99 and CV less than 0.5%. The intra-day and inter-day CVs are less than 15% for quality control samples with concentrations of 75,300, and 750 pg/mL of scopolamine in human plasma. SPE using 96 well micro elution plates allows rapid sample preparation and enhanced sensitivity for the LC/MS/MS determination of scopolamine in a small volume of biological samples. The new method is also cost effective since it uses a small volume of organic solvents compared to the methods using SPE cartridges or regular 96 well SPE plates. This method can be successfully used for bioavailability and pharmacokinetic evaluations of scopolamine, especially when volumes of biological samples are limited. Further investigation to use automated SPE system with 96 well micro elution plates is planned.

Water-quality assessment of stormwater runoff from a heavily used urban highway bridge in Miami, Florida

USGS Publications Warehouse

McKenzie, Donald J.; Irwin, G.A.

1983-01-01

Runoff from a heavily-traveled, 1.43-acre bridge section of Interstate-95 in Miami, Florida, was comprehensively monitored for both quality and quantity during five selected storms between November 1979 and May 1981. For most water-quality parameters, 6 to 11 samples were collected during each of the 5 runoff events. Concentrations of most parameters in the runoff were quite variable both during individual storm events and among the five storm events; however, the ranges in parameter concentration were about the same magnitude report for numerous other highway and urban drainages. Data were normalized to estimate the average, discharge-weighted parameter loads per storm per acre of bridge surface and results suggested that the most significant factor influencing stormwater loads was parameter concentration. Rainfall intensity and runoff volume, however, influenced rates of loading. The total number of antecedent dry days and traffic volume did not appear to be conspicously related to either runoff concentrations or loads. (USGS)

Urinary levoglucosan as a biomarker for woodsmoke exposure in wildland firefighters.

PubMed

Naeher, Luke P; Barr, Dana Boyd; Adetona, Olorunfemi; Simpson, Christopher D

2013-01-01

Levoglucosan, a sugar anhydride and a combustion breakdown product of cellulose is a dominant organic constituent of particles in woodsmoke. After exposure, levoglucosan is excreted unmetabolized in urine. Urinary levoglucosan was assessed as a biomarker of occupational woodsmoke exposure among wildland firefighters. Urine samples were collected from wildland firefighters before and after their work-shifts on days when they worked at prescribed burns. A total of 97 pairs of pre- and post-shift urine samples were collected from 19 firefighters over 10 prescribed burn shifts. The urine samples were analyzed to determine whether there was an increase in the concentration of levoglucosan from pre- to post-shift after the firefighters had worked at the prescribed burns. Overall, there was an increase in both the urinary volume-based and creatinine corrected levoglucosan concentrations from pre- to post-shift (P < 0.05). However, the direction of change in the concentrations was not consistent. There were increases in urinary levoglucosan concentration from pre- to post-shift in 63% of the person-day samples, and in only 58% of the person-day samples for the creatinine corrected concentrations. Although there was an overall increase in urinary concentrations of levoglucosan, results suggest that other sources apart from woodsmoke affected the urinary levels of this biomarker in wildland firefighters. Therefore, urinary levoglucosan may not be effective as a biomarker of woodsmoke exposure in this setting.

Tangential flow ultrafiltration for detection of white spot syndrome virus (WSSV) in shrimp pond water.

PubMed

Alavandi, S V; Ananda Bharathi, R; Satheesh Kumar, S; Dineshkumar, N; Saravanakumar, C; Joseph Sahaya Rajan, J

2015-06-15

Water represents the most important component in the white spot syndrome virus (WSSV) transmission pathway in aquaculture, yet there is very little information. Detection of viruses in water is a challenge, since their counts will often be too low to be detected by available methods such as polymerase chain reaction (PCR). In order to overcome this difficulty, viruses in water have to be concentrated from large volumes of water prior to detection. In this study, a total of 19 water samples from aquaculture ecosystem comprising 3 creeks, 10 shrimp culture ponds, 3 shrimp broodstock tanks and 2 larval rearing tanks of shrimp hatcheries and a sample from a hatchery effluent treatment tank were subjected to concentration of viruses by ultrafiltration (UF) using tangential flow filtration (TFF). Twenty to 100l of water from these sources was concentrated to a final volume of 100mL (200-1000 fold). The efficiency of recovery of WSSV by TFF ranged from 7.5 to 89.61%. WSSV could be successfully detected by PCR in the viral concentrates obtained from water samples of three shrimp culture ponds, one each of the shrimp broodstock tank, larval rearing tank, and the shrimp hatchery effluent treatment tank with WSSV copy numbers ranging from 6 to 157mL(-1) by quantitative real time PCR. The ultrafiltration virus concentration technique enables efficient detection of shrimp viral pathogens in water from aquaculture facilities. It could be used as an important tool to understand the efficacy of biosecurity protocols adopted in the aquaculture facility and to carry out epidemiological investigations of aquatic viral pathogens. Copyright © 2015 Elsevier B.V. All rights reserved.

Radiolytic Hydrogen Production in the South Pacific Subseafloor Basaltic Aquifer

NASA Astrophysics Data System (ADS)

Dzaugis, M. E.; Spivack, A. J.; Dunlea, A. G.; Murray, R. W.; D'Hondt, S.

2015-12-01

Hydrogen (H2) is produced in geological settings by dissociation of water due to radiation from natural radioactive decay of uranium (238U, 235U), thorium (232Th) and potassium (40K). To quantify the potential significance of radiolytic H2 as an electron donor for microbes within the South Pacific subseafloor basaltic aquifer, we calculate radiolytic H2 production rates in basement fractures utilizing measured radionuclide concentrations in 42 basalt samples from IODP Expedition 329. The samples are from three sites with very different basement ages and a wide range of alteration types. Major and trace element concentrations vary by up to an order of magnitude from sample to sample. Comparison of our samples to each other and to previous studies of fresh East Pacific Rise basalt suggests that between-sample variation in radionuclide concentrations is primarily due to differences in initial (pre-alteration) concentrations (which can vary between eruptive events), rather than to alteration type or extent. Local maxima in radionuclide (U, Th, and K) concentrations produce 'hotspots' of radiolytic H2 production; calculated radiolytic rates differ by up to a factor of 80 from sample to sample. Fracture width also greatly influences H2 production. Due to the low penetration distance of alpha radiation, microfractures are 'hotpots' for radiolytic H2 production. For example, radiolytic H2 production rates normalized to water volume are 170 times higher in 1μm-wide fractures than in 10cm-wide fractures.

Experimentally validated mathematical model of analyte uptake by permeation passive samplers.

PubMed

Salim, F; Ioannidis, M; Górecki, T

2017-11-15

A mathematical model describing the sampling process in a permeation-based passive sampler was developed and evaluated numerically. The model was applied to the Waterloo Membrane Sampler (WMS), which employs a polydimethylsiloxane (PDMS) membrane as a permeation barrier, and an adsorbent as a receiving phase. Samplers of this kind are used for sampling volatile organic compounds (VOC) from air and soil gas. The model predicts the spatio-temporal variation of sorbed and free analyte concentrations within the sampler components (membrane, sorbent bed and dead volume), from which the uptake rate throughout the sampling process can be determined. A gradual decline in the uptake rate during the sampling process is predicted, which is more pronounced when sampling higher concentrations. Decline of the uptake rate can be attributed to diminishing analyte concentration gradient within the membrane, which results from resistance to mass transfer and the development of analyte concentration gradients within the sorbent bed. The effects of changing the sampler component dimensions on the rate of this decline in the uptake rate can be predicted from the model. Performance of the model was evaluated experimentally for sampling of toluene vapors under controlled conditions. The model predictions proved close to the experimental values. The model provides a valuable tool to predict changes in the uptake rate during sampling, to assign suitable exposure times at different analyte concentration levels, and to optimize the dimensions of the sampler in a manner that minimizes these changes during the sampling period.

Collection of Pyrethroids in Water and Sediment Matrices: Development and Validation of a Standard Operating Procedure

USGS Publications Warehouse

Hladik, Michelle; Orlando, James L.; Kuivila, Kathryn

2009-01-01

Loss of pyrethroid insecticides onto surfaces during sample collection can confound the interpretation of analytical and toxicity test results. Sample collection devices, container materials, and water matrix composition have a significant influence on the association of pyrethroids to container walls, which can be as high as 50 percent. Any sample collection method involving transfer through multiple containers or pieces of equipment increases the potential for pyrethroid loss. This loose 'surface-association' with container walls can be reversed through agitation. When sampling water matrices with pumps or autosamplers, no pyrethroids were lost as long as the water was moving continuously through the system. When collecting water matrices in containers, the material with the least amount of pyrethroid sorption is as follows: glass less than (<) plastic less than (<) Teflon. Additionally, pyrethroids were easier to re-suspend from the glass container walls. Since the amount of surface-association is proportional to the ratio of volume-to-contact-area of the sample, taking larger-volume field samples (greater than 3 liters) reduced pyrethroid losses to less than 10 percent. The amount of surface-association cannot be predicted easily because of the dependence on water matrix composition; samples with higher dissolved organic carbon or suspended-sediment concentrations were observed to have lower percent loss. Sediment samples were not affected by glass-container sorption (the only containers tested). Standardized sample-collection protocols are critical to yield accurate pyrethroid concentrations for assessment of potential effects, and have been summarized in an accompanying standard operating procedure.

National Water Quality Laboratory, 1995 services catalog

USGS Publications Warehouse

Timme, P.J.

1995-01-01

This Services Catalog contains information about field supplies and analytical services available from the National Water Quality Laboratory in Denver, Colo., and field supplies available from the Quality Water Service Unit in Ocala, Fla., to members of the U.S. Geological Survey. To assist personnel in the selection of analytical services, this catalog lists sample volume, required containers, applicable concentration range, detection level, precision of analysis, and preservation requirements for samples.

High sensitive analysis of steroids in doping control using gas chromatography/time-of-flight mass-spectrometry.

PubMed

Revelsky, A I; Samokhin, A S; Virus, E D; Rodchenkov, G M; Revelsky, I A

2011-04-01

The method of high sensitive gas chromatographic/time-of-flight mass-spectrometric (GC/TOF-MS) analysis of steroids was developed. Low-resolution TOF-MS instrument (with fast spectral acquisition rate) was used. This method is based on the formation of the silyl derivatives of steroids; exchange of the reagent mixture (pyridine and N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA)) for tert-butylmethylether; offline large sample volume injection of this solution based on sorption concentration of the respective derivatives from the vapour-gas mixture flow formed from the solution and inert gas flows; and entire analytes solvent-free concentrate transfer into the injector of the gas chromatograph. Detection limits for 100 µl sample solution volume were 0.5-2 pg/µl (depending on the component). Application of TOF-MS model 'TruTOF' (Leco, St Joseph, MO, USA) coupled with gas chromatograph and ChromaTOF software (Leco, St Joseph, MO, USA) allowed extraction of the full mass spectra and resolving coeluted peaks. Due to use of the proposed method (10 µl sample aliquot) and GC/TOF-MS, two times more steroid-like compounds were registered in the urine extract in comparison with the injection of 1 µl of the same sample solution. Copyright © 2010 John Wiley & Sons, Ltd.

Measuring Blood Glucose Concentrations in Photometric Glucometers Requiring Very Small Sample Volumes.

PubMed

Demitri, Nevine; Zoubir, Abdelhak M

2017-01-01

Glucometers present an important self-monitoring tool for diabetes patients and, therefore, must exhibit high accuracy as well as good usability features. Based on an invasive photometric measurement principle that drastically reduces the volume of the blood sample needed from the patient, we present a framework that is capable of dealing with small blood samples, while maintaining the required accuracy. The framework consists of two major parts: 1) image segmentation; and 2) convergence detection. Step 1 is based on iterative mode-seeking methods to estimate the intensity value of the region of interest. We present several variations of these methods and give theoretical proofs of their convergence. Our approach is able to deal with changes in the number and position of clusters without any prior knowledge. Furthermore, we propose a method based on sparse approximation to decrease the computational load, while maintaining accuracy. Step 2 is achieved by employing temporal tracking and prediction, herewith decreasing the measurement time, and, thus, improving usability. Our framework is tested on several real datasets with different characteristics. We show that we are able to estimate the underlying glucose concentration from much smaller blood samples than is currently state of the art with sufficient accuracy according to the most recent ISO standards and reduce measurement time significantly compared to state-of-the-art methods.

Evaluation of Bio-VOC Sampler for Analysis of Volatile Organic Compounds in Exhaled Breath

PubMed Central

Kwak, Jae; Fan, Maomian; Harshman, Sean W.; Garrison, Catherine E.; Dershem, Victoria L.; Phillips, Jeffrey B.; Grigsby, Claude C.; Ott, Darrin K.

2014-01-01

Monitoring volatile organic compounds (VOCs) from exhaled breath has been used to determine exposures of humans to chemicals. Prior to analysis of VOCs, breath samples are often collected with canisters or bags and concentrated. The Bio-VOC breath sampler, a commercial sampling device, has been recently introduced to the market with growing use. The main advantage for this sampler is to collect the last portion of exhaled breath, which is more likely to represent the air deep in the lungs. However, information about the Bio-VOC sampler is somewhat limited. Therefore, we have thoroughly evaluated the sampler here. We determined the volume of the breath air collected in the sampler was approximately 88 mL. When sampling was repeated multiple times, with the succeeding exhalations applied to a single sorbent tube, we observed linear relationships between the normalized peak intensity and the number of repeated collections with the sampler in many of the breath VOCs detected. No moisture effect was observed on the Tenax sorbent tubes used. However, due to the limitation in the collection volume, the use of the Bio-VOC sampler is recommended only for detection of VOCs present at high concentrations unless repeated collections of breath samples on the sampler are conducted. PMID:25532709

Determination of a wide range of volatile organic compounds in ambient air using multisorbent adsorption/thermal desorption and gas chromatography/mass spectrometry

USGS Publications Warehouse

Pankow, J.F.; Luo, W.; Isabelle, L.M.; Bender, D.A.; Baker, R.J.

1998-01-01

Adsorption/thermal desorption with multisorbent air-sampling cartridges was developed for the determination of 87 method analytes including halogenated alkanes, halogenated alkenes, ethers, alcohols, nitriles, esters, ketones, aromatics, a disulfide, and a furan. The volatilities of the compounds ranged from that of dichlorofluoromethane (CFC12) to that of 1,2,3- trichlorobenzene. The eight most volatile compounds were determined using a 1.5-L air sample and a sample cartridge containing 50 mg of Carbotrap B and 280 mg of Carboxen 1000; the remaining 79 compounds were determined using a 5-L air sample and a cartridge containing 180 mg of Carbotrap B and 70 mg of Carboxen 1000. Analysis and detection were by gas chromatography/mass spectrometry. The minimum detectable level (MDL) concentration values ranged from 0.01 parts per billion by volume (ppbv) for chlorobenzene to 0.4 ppbv for bromomethane; most of the MDL values were in the range 0.02-0.06 ppbv. No breakthrough was detected with the prescribed sample volumes. Analyte stability on the cartridges was very good. Excellent recoveries were obtained with independent check standards. Travel spike recoveries ranged from 90 to 110% for 72 of the 87 compounds. The recoveries were less than 70% for bromomethane and chloroethene and for a few compounds such as methyl acetate that are subject to losses by hydrolysis; the lowest travel spike recovery was obtained for bromomethane (62%). Blank values for all compounds were either below detection or very low. Ambient atmospheric sampling was conducted in New Jersey from April to December, 1997. Three sites characterized by low, moderate, and high densities of urbanization/traffic were sampled. The median detected concentrations of the compounds were either similar at all three sites (as with the chlorofluorocarbon compounds) or increased with the density of urbanization/traffic (as with dichloromethane, MTBE, benzene, and toluene). For toluene, the median detected concentrations were 0.23, 0.42, and 0.70 ppbv at the three sites. Analytical precision was measured using duplicate sampling. As expected, the precision deteriorated with decreasing concentration. At concentrations greater than 0.2 ppbv, most duplicates differed by less than 20%; below the MDL values, the differences between the duplicates were larger, but they were still typically less than 40%.

The impact of health maintenance organization penetration on the use of hospitals that serve minority communities.

PubMed

Gaskin, D J

1997-12-01

Health maintenance organization (HMO) penetration has made hospital markets more price competitive. Hospitals in minority communities may be at a competitive disadvantage because they serve patients who are, on average, sicker and more likely to be uninsured or underinsured. This study estimated the impact of HMO penetration on the use of hospitals in minority communities during 1987 to 1992. Using a sample of 1,413 short-term general hospitals from the 85 largest metropolitan statistical areas, the determinants of hospitals' patient volumes were estimated. Hospitals located in predominately nonwhite neighborhoods were designated minority hospitals, and other hospitals were designated nonminority hospitals. Using regression analysis, the impact of HMO penetration and concentration on hospitals' patient volumes were estimated. By interacting the HMO penetration and concentration variables with a minority hospital indicator variable, HMOs' impact on minority hospitals was calculated. Health maintenance organization penetration was correlated with lower patient volumes in minority hospitals and higher patient volumes in nonminority hospitals. Competition in HMO markets was correlated with lower patient volumes for all hospitals. This effect was stronger for minority hospitals. These findings suggest that minority hospitals may be at risk of losing patients as HMO penetration increases.

Sampling procedures for inventory of commercial volume tree species in Amazon Forest.

PubMed

Netto, Sylvio P; Pelissari, Allan L; Cysneiros, Vinicius C; Bonazza, Marcelo; Sanquetta, Carlos R

2017-01-01

The spatial distribution of tropical tree species can affect the consistency of the estimators in commercial forest inventories, therefore, appropriate sampling procedures are required to survey species with different spatial patterns in the Amazon Forest. For this, the present study aims to evaluate the conventional sampling procedures and introduce the adaptive cluster sampling for volumetric inventories of Amazonian tree species, considering the hypotheses that the density, the spatial distribution and the zero-plots affect the consistency of the estimators, and that the adaptive cluster sampling allows to obtain more accurate volumetric estimation. We use data from a census carried out in Jamari National Forest, Brazil, where trees with diameters equal to or higher than 40 cm were measured in 1,355 plots. Species with different spatial patterns were selected and sampled with simple random sampling, systematic sampling, linear cluster sampling and adaptive cluster sampling, whereby the accuracy of the volumetric estimation and presence of zero-plots were evaluated. The sampling procedures applied to species were affected by the low density of trees and the large number of zero-plots, wherein the adaptive clusters allowed concentrating the sampling effort in plots with trees and, thus, agglutinating more representative samples to estimate the commercial volume.

Methods for the preparation and analysis of solids and suspended solids for methylmercury

USGS Publications Warehouse

DeWild, John F.; Olund, Shane D.; Olson, Mark L.; Tate, Michael T.

2004-01-01

This report presents the methods and method performance data for the determination of methylmercury concentrations in solids and suspended solids. Using the methods outlined here, the U.S. Geological Survey's Wisconsin District Mercury Laboratory can consistently detect methylmercury in solids and suspended solids at environmentally relevant concentrations. Solids can be analyzed wet or freeze dried with a minimum detection limit of 0.08 ng/g (as-processed). Suspended solids must first be isolated from aqueous matrices by filtration. The minimum detection limit for suspended solids is 0.01 ng per filter resulting in a minimum reporting limit ranging from 0.2 ng/L for a 0.05 L filtered volume to 0.01 ng/L for a 1.0 L filtered volume. Maximum concentrations for both matrices can be extended to cover nearly any amount of methylmercury by limiting sample size.

Carbon - Bulk Density Relationships for Highly Weathered Soils of the Americas

NASA Astrophysics Data System (ADS)

Nave, L. E.

2014-12-01

Soils are dynamic natural bodies composed of mineral and organic materials. As a result of this mixed composition, essential properties of soils such as their apparent density, organic and mineral contents are typically correlated. Negative relationships between bulk density (Db) and organic matter concentration provide well-known examples across a broad range of soils, and such quantitative relationships among soil properties are useful for a variety of applications. First, gap-filling or data interpolation often are necessary to develop large soil carbon (C) datasets; furthermore, limitations of access to analytical instruments may preclude C determinations for every soil sample. In such cases, equations to derive soil C concentrations from basic measures of soil mass, volume, and density offer significant potential for purposes of soil C stock estimation. To facilitate estimation of soil C stocks on highly weathered soils of the Americas, I used observations from the International Soil Carbon Network (ISCN) database to develop carbon - bulk density prediction equations for Oxisols and Ultisols. Within a small sample set of georeferenced Oxisols (n=89), 29% of the variation in A horizon C concentrations can be predicted from Db. Including the A-horizon sand content improves predictive capacity to 35%. B horizon C concentrations (n=285) were best predicted by Db and clay content, but were more variable than A-horizons (only 10% of variation explained by linear regression). Among Ultisols, a larger sample set allowed investigation of specific horizons of interest. For example, C concentrations of plowed A (Ap) horizons are predictable based on Db, sand and silt contents (n=804, r2=0.38); gleyed argillic (Btg) horizon concentrations are predictable from Db, sand and clay contents (n=190, r2=0.23). Because soil C stock estimates are more sensitive to variation in soil mass and volume determinations than to variation in C concentration, prediction equations such as these may be used on carefully collected samples to constrain soil C stocks. The geo-referenced ISCN database allows users the opportunity to derive similar predictive relationships among measured soil parameters; continued input of new datasets from highly weathered soils of the Americas will improve the precision of these prediction equations.

Use of continuous and grab sample data for calculating total maximum daily load (TMDL) in agricultural watersheds.

PubMed

Gulati, Shelly; Stubblefield, Ashley A; Hanlon, Jeremy S; Spier, Chelsea L; Stringfellow, William T

2014-03-01

Measuring the discharge of diffuse pollution from agricultural watersheds presents unique challenges. Flows in agricultural watersheds, particularly in Mediterranean climates, can be predominately irrigation runoff and exhibit large diurnal fluctuation in both volume and concentration. Flow and pollutant concentrations in these smaller watersheds dominated by human activity do not conform to a normal distribution and it is not clear if parametric methods are appropriate or accurate for load calculations. The objective of this study was to compare the accuracy of five load estimation methods to calculate pollutant loads from agricultural watersheds. Calculation of loads using results from discrete (grab) samples was compared with the true-load computed using in situ continuous monitoring measurements. A new method is introduced that uses a non-parametric measure of central tendency (the median) to calculate loads (median-load). The median-load method was compared to more commonly used parametric estimation methods which rely on using the mean as a measure of central tendency (mean-load and daily-load), a method that utilizes the total flow volume (volume-load), and a method that uses measure of flow at the time of sampling (instantaneous-load). Using measurements from ten watersheds in the San Joaquin Valley of California, the average percent error compared to the true-load for total dissolved solids (TDS) was 7.3% for the median-load, 6.9% for the mean-load, 6.9% for the volume-load, 16.9% for the instantaneous-load, and 18.7% for the daily-load methods of calculation. The results of this study show that parametric methods are surprisingly accurate, even for data that have starkly non-normal distributions and are highly skewed. Copyright © 2013 Elsevier Ltd. All rights reserved.

Free-volume characteristics of epoxies

NASA Technical Reports Server (NTRS)

Singh, Jag J.; Eftekhari, Abe; Shultz, William J.; St.clair, Terry L.

1992-01-01

Positron annihilation spectroscopy was used to measure free-volume characteristics of selected epoxies. Fluorene resins, a new family of high-temperature thermosetting resins, were selected as the test medium. Experimental results indicate that the free-volume cell size V sub f varies with the molecular weight between the cross-links M sub c according to an equation of the form V sub f = AM sub c sup B, where A and B are structural constants. In two of the samples, the concentration of bulky fluorene groups was increased in the network backbone by replacement of some of the conventional bisphenol A epoxy resin with fluorene-derived epoxy resin. This resulted in an increase in their glass transition temperature for a given level of cross-linking. It was found that in these samples, the Doppler broadening of the annihilation peak decreases with the increasing fluorene content, presumably due to enhanced damping of the chain motions.

A portable molecular-sieve-based CO2 sampling system for radiocarbon measurements

NASA Astrophysics Data System (ADS)

Palonen, V.

2015-12-01

We have developed a field-capable sampling system for the collection of CO2 samples for radiocarbon-concentration measurements. Most target systems in environmental research are limited in volume and CO2 concentration, making conventional flask sampling hard or impossible for radiocarbon studies. The present system captures the CO2 selectively to cartridges containing 13X molecular sieve material. The sampling does not introduce significant under-pressures or significant losses of moisture to the target system, making it suitable for most environmental targets. The system also incorporates a significantly larger sieve container for the removal of CO2 from chambers prior to the CO2 build-up phase and sampling. In addition, both the CO2 and H2O content of the sample gas are measured continuously. This enables in situ estimation of the amount of collected CO2 and the determination of CO2 flux to a chamber. The portable sampling system is described in detail and tests for the reliability of the method are presented.

A portable molecular-sieve-based CO2 sampling system for radiocarbon measurements.

PubMed

Palonen, V

2015-12-01

We have developed a field-capable sampling system for the collection of CO2 samples for radiocarbon-concentration measurements. Most target systems in environmental research are limited in volume and CO2 concentration, making conventional flask sampling hard or impossible for radiocarbon studies. The present system captures the CO2 selectively to cartridges containing 13X molecular sieve material. The sampling does not introduce significant under-pressures or significant losses of moisture to the target system, making it suitable for most environmental targets. The system also incorporates a significantly larger sieve container for the removal of CO2 from chambers prior to the CO2 build-up phase and sampling. In addition, both the CO2 and H2O content of the sample gas are measured continuously. This enables in situ estimation of the amount of collected CO2 and the determination of CO2 flux to a chamber. The portable sampling system is described in detail and tests for the reliability of the method are presented.

Characterization and cooled storage of semen from corn snakes (Elaphe guttata).

PubMed

Fahrig, Brooke M; Mitchell, Mark A; Eilts, Bruce E; Paccamonti, Dale L

2007-03-01

The phylogenetic order Squamata has many representatives that could benefit from the use of semen preservation as a tool for assisting conservation. To date, few studies have been made evaluating the potential for collecting and preserving semen from snakes. The objectives of this study were to characterize semen parameters of the corn snake (Elaphe guttata), including appearance, volume, concentration, sperm motility, and sperm morphology, and to determine the longevity of corn snake sperm motility stored at 4 degrees C. Single semen samples were collected from 22 adult corn snakes. The appearance of the corn snake semen was generally cloudy, and the color was white to tan. Corn snake spermatozoa initially exhibited a median motility of 92.5%. Corn snakes were found to produce small-volume ejaculates (median 0.01 ml). However, the overall concentration of the snake ejaculate was high (chi = 852 x 10(6) +/- 585 x 10(6) spermatozoa/ml). Morphologically, a mean of 75.7 +/- 9.3% of the sperm cells in an ejaculate were normal. Snake ejaculate with a white appearance had significantly higher sperm concentrations (chi = 1,859 x 10(6) +/- 1,008 x 106 sperm cells/ml; F = 15.74, P = 0.001) than tan ejaculates (chi = 601 x 10(6) +/- 439 x 106 sperm cells/ml). Sperm motility decreased significantly in samples that were stored at 4 degrees C for greater than 48 hr in a refrigerator or Equitainer I. This is the first study to characterize semen volume, appearance, and concentration; sperm motility; and sperm morphology in captive corn snakes. The information derived from this study can be used to develop a model for a collection, cooled storage, and shipping program for semen from endangered or threatened captive and wild snakes.

Discrimination of microbiological samples using femtosecond laser-induced breakdown spectroscopy

NASA Astrophysics Data System (ADS)

Baudelet, Matthieu; Yu, Jin; Bossu, Myriam; Jovelet, Julien; Wolf, Jean-Pierre; Amodeo, Tanguy; Fréjafon, Emeric; Laloi, Patrick

2006-10-01

Using femtosecond laser-induced breakdown spectroscopy, the authors have analyzed five different species of bacterium. Line emissions from six trace mineral elements, Na, Mg, P, K, Ca, and Fe, have been clearly detected. Their intensities correspond to relative concentrations of these elements contained in the analyzed samples. The authors demonstrate that the concentration profile of trace elements allows unambiguous discrimination of different bacteria. Quantitative differentiation has been made by representing bacteria in a six-dimension hyperspace with each of its axis representing a detected trace element. In such hyperspace, representative points of different species of bacterium are gathered in different and distinct volumes.

Particulate exhaust emissions from an experimental combustor. [gas turbine engine

NASA Technical Reports Server (NTRS)

Norgren, C. T.; Ingebo, R. D.

1975-01-01

The concentration of dry particulates (carbon) in the exhaust of an experimental gas turbine combustor was measured at simulated takeoff operating conditions and correlated with the standard smoke-number measurement. Carbon was determined quantitatively from a sample collected on a fiberglass filter by converting the carbon in the smoke sample to carbon dioxide and then measuring the volume of carbon dioxide formed by gas chromatography. At a smoke of 25 (threshold of visibility of the smoke plume for large turbojets) the carbon concentration was 2.8 mg carbon/cu m exhaust gas, which is equivalent to an emission index of 0.17 g carbon/kg fuel.

Comparison of two filtration-elution procedures to improve the standard methods ISO 10705-1 & 2 for bacteriophage detection in groundwater, surface water and finished water samples.

PubMed

Helmi, K; Jacob, P; Charni-Ben-Tabassi, N; Delabre, K; Arnal, C

2011-09-01

To select a reliable method for bacteriophage concentration prior detection by culture from surface water, groundwater and drinking water to enhance the sensitivity of the standard methods ISO 10705-1 & 2. Artificially contaminated (groundwater and drinking water) and naturally contaminated (surface water) 1-litre samples were processed for bacteriophages detection. The spiked samples were inoculated with about 150 PFU of F-specific RNA bacteriophages and somatic coliphages using wastewater. Bacteriophage detection in the water samples was achieved using the standard method without and with a concentration step (electropositive Anodisc membrane or a pretreated electronegative Micro Filtration membrane, MF). For artificially contaminated matrices (drinking and ground waters), recovery rates using the concentration step were superior to 70% whilst analyses without concentration step mainly led to false negative results. Besides, the MF membrane presented higher performances compared with the Anodisc membrane. The concentration of a large volume of water (up to one litre) on a filter membrane avoids false negative results obtained by direct analysis as it allows detecting low number of bacteriophages in water samples. The addition of concentration step before applying the standard method could be useful to enhance the reliability of bacteriophages monitoring in water samples as bio-indicators to highlight faecal pollution. © No claim to French Government works. Letters in Applied Microbiology © 2011 The Society for Applied Microbiology.

Chemical Composition of Rainwater in Córdoba City, Argentina

NASA Astrophysics Data System (ADS)

López, M. L.; Asar, M. L.; Ceppi, S.; Bürgesser, R. E.; Avila, E.

2013-05-01

Sampling and chemical analysis of rainwater has proved to be a useful technique for studying its chemical composition and provides a greater understanding of local and regional dispersion of pollutants and their potential impacts to ecosystems through deposition processes. Samples of rainwater were collected during 2009-2012, in Córdoba city, Argentina. Two kind of sampling were performed: event-specific and sequential. The objective of the first of these was to determine the chemical concentration of the total rain, while the objective of the second one was to analyze the variability of the chemical concentration during an individual rain event. The total volume of each sample was divided in halves. One half was filtered through 0.45 μm membrane filter. After this, all the samples were reduced by evaporation to a final volume of 10 ml. The non-filtered samples were acidified and digested in accordance to the method 3050B of the Environmental Protection Agency (EPA) for acid digestion of sediments. Multi-elemental standard solutions in different concentrations were prepared by adequate dilutions. Gallium was added as an internal standard in all standard solutions and samples. Exactly 5 μL of these solutions were deposited on acrylic supports. When these droplets were dried, Synchrotron Radiation Total Reflection X-Ray Fluorescence technique was used for determining the chemical elements. Spectra were analyzed with the AXIL package for spectrum analysis. Due to the intrinsic characteristics of the total reflection technique, the background of the measurements is significantly reduced and there are no matrix effects, therefore quantification can be obtained from the linear correlation between fluorescence intensity and the concentration of the element of interest. The elements quantified were S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, and Pb. For all of them a calibration curve was performed in order to quantify their concentrations on the samples. The results show that the average pH in city rainwater was pH=6.5; the elements found in the samples were S, Ca, Cu, Cr, Sr, P, Fe, Mn, Pb, K, Ti, V, Zn and the average concentrations of these elements were below the limits established by World Health Organization for drinking water, and show a high natural variability. The temporal evolution of inorganic ion concentration during rain events was analyzed and the scavenging coefficients were calculated and compared with data from literature. A comparison was made between the rainwater chemical composition and chemical composition in the aerosols scavenging during the rain. This study is the first in Córdoba city to analyze the chemical composition of rainwater and constitute a base for future comparison of variability in pH and elemental composition.

CO2 volume fluxes outgassing from champagne glasses: the impact of champagne ageing.

PubMed

Liger-Belair, Gérard; Villaume, Sandra; Cilindre, Clara; Jeandet, Philippe

2010-02-15

It was demonstrated that CO(2) volume fluxes outgassing from a flute poured with a young champagne (elaborated in 2007) are much higher than those outgassing from the same flute poured with an older champagne (elaborated in the early 1990s). The difference in dissolved-CO(2) concentrations between the two types of champagne samples was found to be a crucial parameter responsible for differences in CO(2) volume fluxes outgassing from one champagne to another. Nevertheless, it was shown that, for a given identical dissolved-CO(2) concentration in both champagne types, the CO(2) volume flux outgassing from the flute poured with the old champagne is, in average, significantly lower than that outgassing from the flute poured with the young one. Therefore, CO(2) seems to "escape" more easily from the young champagne than from the older one. The diffusion coefficient of CO(2) in both champagne types was pointed as a key parameter to thoroughly determine in the future, in order to unravel our experimental observation. Copyright 2009 Elsevier B.V. All rights reserved.

A compact tritium enrichment unit for large sample volumes with automated re-filling and higher enrichment factor.

PubMed

Kumar, B; Han, L-F; Wassenaar, L I; Klaus, P M; Kainz, G G; Hillegonds, D; Brummer, D; Ahmad, M; Belachew, D L; Araguás, L; Aggarwal, P

2016-12-01

Tritium ( 3 H) in natural waters is a powerful tracer of hydrological processes, but its low concentrations require electrolytic enrichment before precise measurements can be made with a liquid scintillation counter. Here, we describe a newly developed, compact tritium enrichment unit which can be used to enrich up to 2L of a water sample. This allows a high enrichment factor (>100) for measuring low 3 H contents of <0.05TU. The TEU uses a small cell (250mL) with automated re-filling and a CO 2 bubbling technique to neutralize the high alkalinity of enriched samples. The enriched residual sample is retrieved from the cell under vacuum by cryogenic distillation at -20°C and the tritium enrichment factor for each sample is accurately determined by measuring pre- and post- enrichment 2 H concentrations with laser spectrometry. Copyright © 2016. Published by Elsevier Ltd.

Sperm quality in New Zealand: Is the downward trend continuing?

PubMed

Birdsall, Mary A; Peek, John; Valiapan, Sumithra

2015-10-16

To investigate whether the decline in sperm concentration in New Zealand sperm donors observed from 1987 to 2007 continued in the period 2008-2014. A retrospective study from 2008 to 2014. The first semen sample of 285 men presenting as sperm donors in Auckland and Wellington was analysed for sperm concentration, seminal fluid volume and the percentage of motile sperm. These results were compared to results from 1987 to 2007 from the same clinics. The decline in semen volume and sperm concentration observed between 1987 and 2007 did not continue in 2008-2014. Sperm concentration decreased from 1987 until some time between 1997 and 2001, and has remained stable at an average of 62x106/ml between 2001 and 2014. Sperm motility declined significantly (8%) in the period 2008-2014, but there was no significant change over the total period studied, between 1987 and 2014. After a decline between 1987 and sometime during 1997-2001, the sperm concentration in men presenting as donors remained unchanged between 2002 and 2014, suggesting semen quality has not changed in New Zealand men over the last decade.

Simultaneous extraction and quantification of albendazole and triclabendazole using vortex-assisted hollow-fiber liquid-phase microextraction combined with high-performance liquid chromatography.

PubMed

Asadi, Mohammad; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh

2016-06-01

A novel, simple, and rapid vortex-assisted hollow-fiber liquid-phase microextraction method was developed for the simultaneous extraction of albendazole and triclabendazole from various matrices before their determination by high-performance liquid chromatography with fluorescence detection. Several factors influencing the microextraction efficiency including sample pH, nature and volume of extraction solvent, ionic strength, vortex time, and sample volume were investigated and optimized. Under the optimal conditions, the limits of detection were 0.08 and 0.12 μg/L for albendazole and triclabendazole, respectively. The calibration curves were linear in the concentration ranges of 0.3-50.0 and 0.4-50.0 μg/L with the coefficients of determination of 0.9999 and 0.9995 for albendazole and triclabendazole, respectively. The interday and intraday relative standard deviations for albendazole and triclabendazole at three concentration levels (1.0, 10.0, and 30.0 μg/L) were in the range of 6.0-11.0 and 5.0-7.9%, respectively. The developed method was successfully applied to determine albendazole and triclabendazole in water, milk, honey, and urine samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Breakthrough during air sampling with polyurethane foam: What do PUF 2/PUF 1 ratios mean?

PubMed

Bidleman, Terry F; Tysklind, Mats

2018-02-01

Frontal chromatography theory is applied to describe movement of gaseous semivolatile organic compounds (SVOCs) through a column of polyurethane foam (PUF). Collected mass fractions (F C ) are predicted for sample volume/breakthrough volume ratios (τ = V S /V B ) up to 6.0 and PUF bed theoretical plate numbers (N) from 2 to 16. The predictions assume constant air concentrations and temperatures. Extension of the calculations is done to relate the collection efficiency of a 2-PUF train (F C1+2 ) to the PUF 2/PUF 1 ratio. F C1+2 exceeds 0.9 for PUF 2/PUF 1 ≤ 0.5 and lengths of PUF commonly used in air samplers. As the PUF 2/PUF 1 ratio approaches unity, confidence in these predictions is limited by the analytical ability to distinguish residues on the two PUFs. Field data should not be arbitrarily discarded because some analytes broke through to the backup PUF trap. The fractional collection efficiencies can be used to estimate air concentrations from quantities retained on the PUF trap when sampling is not quantitative. Copyright © 2017 Elsevier Ltd. All rights reserved.

Denuder/filter sampling of organic acids and organosulfates at urban and boreal forest sites: Gas/particle distribution and possible sampling artifacts

NASA Astrophysics Data System (ADS)

Kristensen, Kasper; Bilde, Merete; Aalto, Pasi P.; Petäjä, Tuukka; Glasius, Marianne

2016-04-01

Carboxylic acids and organosulfates comprise an important fraction of atmospheric secondary organic aerosols formed from both anthropogenic and biogenic precursors. The partitioning of these compounds between the gas and particle phase is still unclear and further research is warranted to better understand the abundance and effect of organic acids and organosulfates on the formation and properties of atmospheric aerosols. This work compares atmospheric aerosols collected at an urban and a boreal forest site using two side-by-side sampling systems; a high volume sampler (HVS) and a low volume (LVS) denuder/filter sampling system allowing for separate collection of gas- and particle-phase organics. All particle filters and denuder samples were collected at H.C. Andersen Boulevard (HCAB), Copenhagen, Denmark in the summer of 2010, and at the remote boreal forest site at Hyytiälä forestry field station in Finland in the summer of 2012. The chemical composition of gas- and particle-phase secondary organic aerosol was investigated by ultra-high performance liquid chromatography/electrospray ionization quadrupole time-of-flight mass spectrometry (UPLC/ESI-Q-TOFMS), with a focus on carboxylic acids and organosulfates. Results show gas-phase concentrations higher than those observed in the particle phase by a factor of 5-6 in HCAB 2010 and 50-80 in Hyytiälä 2012. Although abundant in the particle phase, no organosulfates were detected in the gas phase at either site. Through a comparison of samples collected by the HVS and the LVS denuder/filter sampling system we evaluate the potential artifacts associated with sampling of atmospheric aerosols. Such comparison shows that particle phase concentrations of semi-volatile organic acids obtained from the filters collected by HVS are more than two times higher than concentrations obtained from filters collected using LVS denuder/filter system. In most cases, higher concentrations of organosulfates are observed in particles collected by HVS compared to samples collected by LVS denuder/filter sampling system. The present study shows that volatile organics may absorb onto filter materials in the HVS (and similar sampling systems without denuder) and furthermore undergo subsequent on-filter oxidation and sulfation resulting in formation of both organic acids and organosulfates.

Redefining the stormwater first flush phenomenon.

PubMed

Bach, Peter M; McCarthy, David T; Deletic, Ana

2010-04-01

The first flush in urban runoff has been an important, yet disputed phenomenon amongst many researchers. The vast differences in the evidence could be solely due to limitations of the first flush current definition and the approach used for its assessment. There is a need for revisiting the first flush theory in the light of its practical applications to urban drainage management practices. We propose that a catchment's first flush behaviour is to be quantified by the runoff volume required to reduce a catchment's stormwater pollutant concentrations to background levels. The proposed method for assessment of this runoff volume starts by finding the average catchment pollutant concentrations for a given increment of discharged volume using a number of event pollutographs. Non-parametric statistics are then used to establish the characteristic pollutograph by pooling statistically indifferent runoff increments (known as slices) together. This allows the identification of the catchment's initial and background pollutant concentrations and for quantification of the first flush volume and its strength. The novel technique was used on seven catchments around Melbourne, Australia, with promising results. Sensitivity to the chosen increment of runoff (for which mean concentrations are calculated) indicated that when dealing with discrete flow-weighted water quality data, a suitable slice size should closely match the flow-weighting of samples. The overall sensitivity to runoff increment and level of significance was found to be negligible. Further research is needed to fully develop this method. Copyright (c) 2010 Elsevier Ltd. All rights reserved.

Effects of breathing pattern and inspired air conditions on breath condensate volume, pH, nitrite, and protein concentrations

PubMed Central

McCafferty, J; Bradshaw, T; Tate, S; Greening, A; Innes, J

2004-01-01

Background: The effects of breathing pattern and inspired air conditions on the volume and content of exhaled breath condensate (EBC) were investigated. Methods: Total exhaled water (TEW), EBC volume, pH, nitrite and protein concentrations were measured in three groups of 10 healthy subjects breathing into a condenser at different target minute ventilations (Vm), tidal volumes (Vt), and inspired air conditions. Results: The volumes of both TEW and EBC increased significantly with Vm. For Vm 7.5, 15 and 22.5 l/min, mean (SD) EBC was 627 (258) µl, 1019 (313) µl, and 1358 (364) µl, respectively (p<0.001) and TEW was 1879 (378) µl, 2986 (496) µl, and 4679 (700) µl, respectively (p<0.001). TEW was significantly higher than EBC, reflecting a condenser efficiency of 40% at a target Vm of 7.5 l/min which reduced to 29% at Vm 22.5 l/min. Lower Vt gave less TEW than higher Vt (26.6 v 30.7 µl/l, mean difference 4.1 (95% CI 2.6 to 5.6), p<0.001) and a smaller EBC volume (4.3 v 7.6 µl/l, mean difference 3.4 (95% CI 2.3 to 4.5), p<0.001). Cooler and drier inspired air yielded less water vapour and less breath condensate than standard conditions (p<0.05). Changes in the breathing pattern had no effect on EBC protein and nitrite concentrations and pH. Conclusion: These results show that condensate volume can be increased by using high Vt and increased Vm without compromising the dilution of the sample. PMID:15282391

Headspace concentrations of explosive vapors in containers designed for canine testing and training: theory, experiment, and canine trials.

PubMed

Lotspeich, Erica; Kitts, Kelley; Goodpaster, John

2012-07-10

It is a common misconception that the amount of explosive is the chief contributor to the quantity of vapor that is available to trained canines. In fact, this quantity (known as odor availability) depends not only on the amount of explosive material, but also the container volume, explosive vapor pressure and temperature. In order to better understand odor availability, headspace experiments were conducted and the results were compared to theory. The vapor-phase concentrations of three liquid explosives (nitromethane, nitroethane and nitropropane) were predicted using the Ideal Gas Law for containers of various volumes that are in use for canine testing. These predictions were verified through experiments that varied the amount of sample, the container size, and the temperature. These results demonstrated that the amount of sample that is needed to saturate different sized containers is small, predictable and agrees well with theory. In general, and as expected, once the headspace of a container is saturated, any subsequent increase in sample volume will not result in the release of more vapors. The ability of canines to recognize and alert to differing amounts of nitromethane has also been studied. In particular, it was found that the response of trained canines is independent of the amount of nitromethane present, provided it is a sufficient quantity to saturate the container in which it is held. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Phelan, J.M.

A high volume sampling system was developed for the collection of volcanic plume aerosols from an aircraft sampling platform. Concentrations of up to 30 elements on particles were determined simultaneously with gas-phase concentrations of S, Cl, and Br in the quiescent plumes of five active volcanoes: Mount St. Helens, US; Arenal and Poas, Costa Rica; Colima and El Chichon, Mexico. Volatile and chalcophilic elements were found to be highly enriched, relative to average crustal and bulk pyroclastic material, in the quiescent plumes of all volcanoes studied. Enriched volatile elements were found to be primarily associated with fine (less than ormore » equal to 3-..mu..m diam) particles, those expected to have the longest residence times in the atmosphere. Samples were also collected using the aircraft sampling system in background, mid-tropospheric air. Analysis of these samples revealed that many of the same elements that are enriched in volcanic plumes are also enriched in clean, relatively remote aerosols collected in the free troposphere (5-7 km). Concentrations of sulfates made in the North American free troposphere (280 ng/m/sup 3/) approach those measured at remote background sites.« less

At the forefront: evidence of the applicability of using environmental DNA to quantify the abundance of fish populations in natural lentic waters with additional sampling considerations

USGS Publications Warehouse

Klobucar, Stephen L.; Rodgers, Torrey W.; Budy, Phaedra

2017-01-01

Environmental DNA (eDNA) sampling has proven to be a valuable tool for detecting species in aquatic ecosystems. Within this rapidly evolving field, a promising application is the ability to obtain quantitative estimates of relative species abundance based on eDNA concentration rather than traditionally labor-intensive methods. We investigated the relationship between eDNA concentration and Arctic char (Salvelinus alpinus) abundance in five well-studied natural lakes; additionally, we examined the effects of different temporal (e.g., season) and spatial (e.g., depth) scales on eDNA concentration. Concentrations of eDNA were linearly correlated with char population estimates ( = 0.78) and exponentially correlated with char densities ( = 0.96 by area; 0.82 by volume). Across lakes, eDNA concentrations were greater and more homogeneous in the water column during mixis; however, when stratified, eDNA concentrations were greater in the hypolimnion. Overall, our findings demonstrate that eDNA techniques can produce effective estimates of relative fish abundance in natural lakes. These findings can guide future studies to improve and expand eDNA methods while informing research and management using rapid and minimally invasive sampling.

"Center punch" and "whole spot" bioanalysis of apixaban in human dried blood spot samples by UHPLC-MS/MS.

PubMed

Zheng, Naiyu; Yuan, Long; Ji, Qin C; Mangus, Heidi; Song, Yan; Frost, Charles; Zeng, Jianing; Aubry, Anne-Françoise; Arnold, Mark E

2015-04-15

Apixaban (Eliquis™) was developed by Bristol-Myers Squibb (BMS) and Pfizer to use as an antithrombotic/anticoagulant agent and has been recently approved for the prevention of stroke and systemic embolism in patients with nonvalvular atrial fibrillation. A clinical study of apixaban, sponsored by BMS and Pfizer, included a pilot exploratory portion to evaluate the potential for future drug concentration monitoring using dried blood spot (DBS) sample collection. For DBS sample collection, a fixed blood volume was dispensed onto a DBS card by either regular volumetric pipette (venous blood collection) or capillary dispenser (finger prick blood collection). A 96-well semi-automated liquid-liquid extraction sample preparation procedure was developed to provide clean extracts for UHPLC-MS/MS quantitation. Assays using both partial-spot center punch and whole spot punch were developed and validated. The linear dynamic ranges for all the analyses were from 0.5 to 500 ng/mL. The coefficient of determination (r(2)) values was >0.9944 for all the validation runs. For the center punch approach, the intra-assay precision (%CV) was within 4.4% and inter-assay precision was within 2.6%. The assay accuracy, expressed as %Dev., was within ± 5.4% of the nominal concentrations. One accuracy and precision run was performed using the whole spot approach, the intra-assay precision (%CV) was within 7.1% and the accuracy was within ± 8.0% of the nominal concentrations. In contrast to the center punch approach, the whole spot approach eliminated the effect of hematocrit and high lipids on the analysis of apixaban in human DBS when an accurate sample blood volume was collected on DBS cards. Copyright © 2015 Elsevier B.V. All rights reserved.

Detection methods for human enteric viruses in representative foods.

PubMed

Leggitt, P R; Jaykus, L A

2000-12-01

Although viral foodborne disease is a significant problem, foods are rarely tested for viral contamination, and when done, testing is limited to shellfish commodities. In this work, we report a method to extract and detect human enteric viruses from alternative food commodities using an elution-concentration approach followed by detection using reverse transcription-polymerase chain reaction (RT-PCR). Fifty-gram lettuce or hamburger samples were artificially inoculated with poliovirus type 1 (PV1), hepatitis A virus (HAV), or the Norwalk virus and processed by the sequential steps of homogenization, filtration, Freon extraction (hamburger), and polyethylene glycol (PEG) precipitation. To reduce volumes further and remove RT-PCR inhibitors, a secondary PEG precipitation was necessary, resulting in an overall 10- to 20-fold sample size reduction from 50 g to 3 to 5 ml. Virus recoveries in secondary PEG concentrates ranged from 10 to 70% for PV1 and 2 to 4% for HAV as evaluated by mammalian cell culture infectivity assay. Total RNA from PEG concentrates was extracted to a small volume (30 to 40 microl) and subjected to RT-PCR amplification of viral RNA sequences. Detection limit studies indicated that viral RNA was consistently detected by RT-PCR at initial inoculum levels > or =102 PFU/50-g food sample for PV1 and > or =10(3) PFU/50-g food sample for HAV. In similar studies with the Norwalk virus, detection at inoculum levels > or =1.5 X 10(3) PCR-amplifiable units/50-g sample for both food products was possible. All RT-PCR amplicons were confirmed by subsequent Southern hybridization. The procedure reported represents progress toward the development of methods to detect human enteric viral contamination in foods other than shellfish.

Concentration of infectious aquatic rhabdoviruses from freshwater and seawater using ultrafiltration.

PubMed

Grant, Amelia A M; Jakob, Eva; Richard, Jon; Garver, Kyle A

2011-12-01

Infectious hematopoietic necrosis virus (IHNV), viral hemorrhagic septicemia virus, and spring viremia of carp virus were concentrated and detected from freshwater and seawater samples by using hollow-fiber ultrafiltration. Within 60 min, virus in a 50-L freshwater or saltwater sample was concentrated more than 70-fold, and virus retention efficiencies were consistently greater than 88%. Retention efficiency was highly dependent upon concentrations of column blocking and sample stabilization solutions. A large column with a surface area of 1.15 m2 and a filtration capacity of 5-200 L exhibited optimal viral retention when blocked with 2% fetal bovine serum (FBS) and when the samples were supplemented with 0.1% FBS. Conversely, a small column with 100-fold less surface area and a filtering capacity of 0.5-2.0 L was optimized when blocked with 1% FBS and when the samples were supplemented with 0.1% FBS. The optimized ultrafiltration procedure was further validated with water from a tank that contained IHNV-exposed juvenile sockeye salmon Oncorhynchus nerka, resulting in an average virus retention efficiency of 91.6 +/- 4.1% (mean +/- SE). Virus quantification of concentrated samples demonstrated that IHNV shedding in sockeye salmon preceded mortality; shedding of the virus was observed to increase significantly as early as 7 d postchallenge and peaked at day 14, when virus levels reached 4.87 x 10(3) plaque-forming units/mL. We conclude that ultrafiltration is a reliable and effective method for concentrating viable aquatic rhabdoviruses from large volumes of water and has application for the analysis of environmental water samples.

Altered tryptophan catabolite concentrations in major depressive disorder and associated changes in hippocampal subfield volumes.

PubMed

Doolin, Kelly; Allers, Kelly A; Pleiner, Sina; Liesener, Andre; Farrell, Chloe; Tozzi, Leonardo; O'Hanlon, Erik; Roddy, Darren; Frodl, Thomas; Harkin, Andrew; O'Keane, Veronica

2018-05-19

Tryptophan depletion is a well-replicated biological finding in Major Depressive Disorder (MDD). The kynurenine pathway (KP) and its rate-limiting tryptophan degrading enzyme, indolamine 2,3 dioxygenase (IDO), have been implicated in the pathogenesis of depression. IDO expression is driven by inflammatory cytokines, providing a putative link between inflammation and neuropathology. This study examined circulating concentrations of C-reactive protein (CRP), plasma tryptophan, kynurenine (KYN), kynurenic acid (KYNA) and quinolinic acid (QUIN) and whole blood mRNA expression of IDO in patients with major depressive disorder (MDD) compared with healthy controls (HC). A diagnosis of major depression was made according to DSM-IV. Depression severity was assessed using the Hamilton depression (HAM-D) rating scale. 74 MDD patients, 39 with a first presentation of MDD (fpMDD) and 35 with chronic or recurrent episodes (rMDD), and 37 HC were recruited to the study. Whole blood and plasma samples were collected. Expression of markers in whole blood were measured by PCR, circulating CRP by ELISA and KP metabolites by LC-MS/MS. Hippocampal cornu ammonis (CA) and subiculum volumes were determined by MRI and calculated using FreeSurfer. Tryptophan concentrations were significantly reduced in MDD compared to HC. There was a positive correlation between QUIN and both CRP concentrations and whole blood IDO1 in MDD. KYNA concentrations were reduced in MDD patients presenting with a first episode (fpMDD) compared to those presenting with recurrent depression (rMDD) and HC. By contrast QUIN concentrations were elevated in rMDD compared to fpMDD and HC. KYNA/QUIN was reduced in MDD and rMDD but not fpMDD compared to HC. Hippocampal subfield volumes were smaller in MDD patients than HC for CA1 (left only), CA2/3 (left and right) and CA4 (right only). CRP and CA1 volumes were negatively correlated bilaterally in MDD patients. KYNA and subiculum volume were positively correlated bilaterally. This study found evidence of KP metabolism imbalance in MDD patients in addition to tryptophan reduction and mild immune activation. Relationships between CRP and KYNA with some hippocampal subfield volumes in MDD patients suggest that this inflammatory signature may be associated with reduced hippocampal subfield volumes in depression. Copyright © 2018 Elsevier Ltd. All rights reserved.

Colorimetric-Solid Phase Extraction Technology for Water Quality Monitoring: Evaluation of C-SPE and Debubbling Methods in Microgravity

NASA Technical Reports Server (NTRS)

Hazen-Bosveld, April; Lipert, Robert J.; Nordling, John; Shih, Chien-Ju; Siperko, Lorraine; Porter, Marc D.; Gazda, Daniel B.; Rutz, Jeff A.; Straub, John E.; Schultz, John R.;

Exploring Nectar Biology To Learn about Pollinators.

ERIC Educational Resources Information Center

LaBare, Kelly M.; Broyles, Steven B.; Klotz, R. Lawrence

2000-01-01

Discusses the importance of studying nectar biology. Describes how to extract nectar from various flowers, measure nectar volume, determine sugar concentration, and determine caloric value per nectar sample. These data are then related to hummingbird energetics to determine how many flowers are required to supply the pollinator with its caloric…

Precipitation and streamwater chemistry in an undisturbed watershed in southeast Alaska.

Treesearch

John D. Stednick

1981-01-01

Water chemistry samples have been taken from streamflow since 1976 and precipitation since 1978 in Indian River, an undisturbed watershed on Chichagof Island in Southeast Alaska. Volume weighted concentrations of total nitrogen, ammonium nitrogen, nitrate nitrogen, total phosphorus, orthophosphate, sulfate sulfur, chloride, bicarbonate, silica, calcium, magnesium,...

40 CFR 63.11646 - What are my compliance requirements?

Code of Federal Regulations, 2012 CFR

2012-07-01

... with Method 29 must collect a minimum sample volume of 0.85 dry standard cubic meters (30 dry standard... weight measurement device, mass flow meter, or densitometer and volumetric flow meter to measure ore...) Measure the weight of concentrate (produced by electrowinning, Merrill Crowe process, gravity feed, or...

40 CFR 63.11646 - What are my compliance requirements?

Code of Federal Regulations, 2014 CFR

2014-07-01

... with Method 29 must collect a minimum sample volume of 0.85 dry standard cubic meters (30 dry standard... weight measurement device, mass flow meter, or densitometer and volumetric flow meter to measure ore...) Measure the weight of concentrate (produced by electrowinning, Merrill Crowe process, gravity feed, or...

40 CFR 63.11646 - What are my compliance requirements?

Code of Federal Regulations, 2011 CFR

2011-07-01

... with Method 29 must collect a minimum sample volume of 0.85 dry standard cubic meters (30 dry standard... weight measurement device, mass flow meter, or densitometer and volumetric flow meter to measure ore...) Measure the weight of concentrate (produced by electrowinning, Merrill Crowe process, gravity feed, or...

40 CFR 63.11646 - What are my compliance requirements?

Code of Federal Regulations, 2013 CFR

2013-07-01

... with Method 29 must collect a minimum sample volume of 0.85 dry standard cubic meters (30 dry standard... weight measurement device, mass flow meter, or densitometer and volumetric flow meter to measure ore...) Measure the weight of concentrate (produced by electrowinning, Merrill Crowe process, gravity feed, or...

Human and bovine viruses in urban and rural streams: Hydrologic and season patterns of wastewater influence

USDA-ARS?s Scientific Manuscript database

Viruses are the cause of many waterborne diseases contracted from fecal-contaminated waters. Collection of samples that properly represent virus concentrations throughout relevant hydrologic periods has historically been difficult due to the large water volume collection and filtration required for ...

40 CFR 60.456 - Test methods and procedures.

Code of Federal Regulations, 2010 CFR

2010-07-01

... Section 60.456 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS... § 60.453. (2) Method 25 for the measurement of the VOC concentration in the gas stream vent. (3) Method... sampling times or smaller volumes, when necessitated by process variables or other factors, may be approved...

40 CFR 89.301 - Scope; applicability.

Code of Federal Regulations, 2010 CFR

2010-07-01

... subpart B of part 89. (b) Exhaust gases, either raw or dilute, are sampled while the test engine is operated using an 8-mode test cycle on an engine dynamometer. The exhaust gases receive specific component analysis determining concentration of pollutant, exhaust volume, the fuel flow, and the power output during...

Utilization of long duration high-volume sampling coupled to SPME-GC-MS/MS for the assessment of airborne pesticides variability in an urban area (Strasbourg, France) during agricultural application.

PubMed

Liaud, Céline; Brucher, Michel; Schummer, Claude; Coscollà, Clara; Wolff, Hélène; Schwartz, Jean-Jacques; Yusà, Vicent; Millet, Maurice

2016-10-02

Atmospheric samples have been collected between 14 March and 12 September 2012 on a 2-week basis (15 days of sampling and exchange of traps each 7 days) in Strasbourg (east of France) for the analysis of 43 pesticides. Samples (particle and gas phases) were separately extracted using Accelerated Solvent Extraction (ASE) and pre-concentrated by Solid Phase Micro-Extraction (SPME) before analysis by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). Four SPME consecutive injections at distinct temperatures were made in order to increase the sensitivity of detection for the all monitored pesticides. Currently used detected pesticides can be grouped in four classes; those used in maize crops (acetochlor, benoxacor, dicamba, s-metolachlor, pendimethalin, and bromoxynil), in cereal crops (benoxacor, chlorothalonil, fenpropimorph, and propiconazole), in vineyards (tebuconazole), and as herbicides for orchards, meadows of green spaces (2,4-MCPA, trichlopyr). This is in accordance with the diversity of crops found in the Alsace region and trends observed are in accordance with the period of application of these pesticides. Variations observed permit also to demonstrate that the long time sampling duration used in this study is efficient to visualize temporal variations of airborne pesticides concentrations. Then, long time high-volume sampling could be a simple method permitting atmospheric survey of atmospheric contamination without any long analysis time and consequently low cost.

Sensitive analysis of steroid estrogens and bisphenol a in small volumes of water using isotope-dilution ultra-performance liquid chromatography-tandem mass spectrometry.

PubMed

Chang, Hong; Shen, Xiaoyan; Shao, Bing; Wu, Fengchang

2018-04-01

An isotope-dilution ultra-performance liquid chromatography-electrospray tandem mass spectrometry method combined with dansylation was established to sensitively quantify four steroid estrogens (estrone, 17α-estradiol, 17β-estradiol and 17α-ethynylestradiol) and bisphenol A in sewage influent and effluent. A simple hexane extraction was performed from a small volume (10 mL), followed by dansyl chloride derivatization and purification with a silica cartridge. The method effectively reduced the matrix effects in sample extract and permitted the selective and sensitive determination of target compounds from complicated matrices. The detection limits of the method for steroid estrogens were 0.20-0.90 ng L -1 in influent and 0.10-0.20 ng L -1 in effluent samples. For bisphenol A, the limits detection of the method were 20 and 0.80 for influent and effluent samples, respectively. Recoveries of 85%-96% were observed in all matrices. The method was applied to analyze residual estrogens and bisphenol A in sewage influent and effluent samples from Beijing, China. The concentrations of bisphenol A (636-1200 ng L -1 ) were up to 250 times higher than those of steroid estrogens. Estrone was the dominant estrogen in influent and effluent samples, while similar concentrations of 17α-estradiol and 17β-estradiol were detected in all samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

Modeling the Sensitivity of Field Surveys for Detection of Environmental DNA (eDNA)

PubMed Central

Schultz, Martin T.; Lance, Richard F.

2015-01-01

The environmental DNA (eDNA) method is the practice of collecting environmental samples and analyzing them for the presence of a genetic marker specific to a target species. Little is known about the sensitivity of the eDNA method. Sensitivity is the probability that the target marker will be detected if it is present in the water body. Methods and tools are needed to assess the sensitivity of sampling protocols, design eDNA surveys, and interpret survey results. In this study, the sensitivity of the eDNA method is modeled as a function of ambient target marker concentration. The model accounts for five steps of sample collection and analysis, including: 1) collection of a filtered water sample from the source; 2) extraction of DNA from the filter and isolation in a purified elution; 3) removal of aliquots from the elution for use in the polymerase chain reaction (PCR) assay; 4) PCR; and 5) genetic sequencing. The model is applicable to any target species. For demonstration purposes, the model is parameterized for bighead carp (Hypophthalmichthys nobilis) and silver carp (H. molitrix) assuming sampling protocols used in the Chicago Area Waterway System (CAWS). Simulation results show that eDNA surveys have a high false negative rate at low concentrations of the genetic marker. This is attributed to processing of water samples and division of the extraction elution in preparation for the PCR assay. Increases in field survey sensitivity can be achieved by increasing sample volume, sample number, and PCR replicates. Increasing sample volume yields the greatest increase in sensitivity. It is recommended that investigators estimate and communicate the sensitivity of eDNA surveys to help facilitate interpretation of eDNA survey results. In the absence of such information, it is difficult to evaluate the results of surveys in which no water samples test positive for the target marker. It is also recommended that invasive species managers articulate concentration-based sensitivity objectives for eDNA surveys. In the absence of such information, it is difficult to design appropriate sampling protocols. The model provides insights into how sampling protocols can be designed or modified to achieve these sensitivity objectives. PMID:26509674

Modeling the Sensitivity of Field Surveys for Detection of Environmental DNA (eDNA).

PubMed

Schultz, Martin T; Lance, Richard F

2015-01-01

The environmental DNA (eDNA) method is the practice of collecting environmental samples and analyzing them for the presence of a genetic marker specific to a target species. Little is known about the sensitivity of the eDNA method. Sensitivity is the probability that the target marker will be detected if it is present in the water body. Methods and tools are needed to assess the sensitivity of sampling protocols, design eDNA surveys, and interpret survey results. In this study, the sensitivity of the eDNA method is modeled as a function of ambient target marker concentration. The model accounts for five steps of sample collection and analysis, including: 1) collection of a filtered water sample from the source; 2) extraction of DNA from the filter and isolation in a purified elution; 3) removal of aliquots from the elution for use in the polymerase chain reaction (PCR) assay; 4) PCR; and 5) genetic sequencing. The model is applicable to any target species. For demonstration purposes, the model is parameterized for bighead carp (Hypophthalmichthys nobilis) and silver carp (H. molitrix) assuming sampling protocols used in the Chicago Area Waterway System (CAWS). Simulation results show that eDNA surveys have a high false negative rate at low concentrations of the genetic marker. This is attributed to processing of water samples and division of the extraction elution in preparation for the PCR assay. Increases in field survey sensitivity can be achieved by increasing sample volume, sample number, and PCR replicates. Increasing sample volume yields the greatest increase in sensitivity. It is recommended that investigators estimate and communicate the sensitivity of eDNA surveys to help facilitate interpretation of eDNA survey results. In the absence of such information, it is difficult to evaluate the results of surveys in which no water samples test positive for the target marker. It is also recommended that invasive species managers articulate concentration-based sensitivity objectives for eDNA surveys. In the absence of such information, it is difficult to design appropriate sampling protocols. The model provides insights into how sampling protocols can be designed or modified to achieve these sensitivity objectives.

Dispersive liquid-liquid microextraction based on solidification of floating organic drop for preconcentration and determination of trace amounts of copper by flame atomic absorption spectrometry.

PubMed

Karadaş, Cennet; Kara, Derya

2017-04-01

A novel, simple, rapid, sensitive, inexpensive and environmentally friendly dispersive liquid-liquid microextraction method based on the solidification of a floating organic drop (DLLME-SFO) was developed for the determination of copper by flame atomic absorption spectrometry (FAAS). N-o-Vanillidine-2-amino-p-cresol was used as a chelating ligand and 1-undecanol was selected as an extraction solvent. The main parameters affecting the performance of DLLME-SFO, such as sample pH, volume of extraction solvent, extraction time, concentration of the chelating ligand, salt effect, centrifugation time and sample volume were investigated and optimized. The effect of interfering ions on the recovery of copper was also examined. Under the optimum conditions, the detection limit (3σ) was 0.93μgL -1 for Cu using a sample volume of 20mL, yielding a preconcentration factor of 20. The proposed method was successfully applied to the determination of Cu in tap, river and seawater, rice flour and black tea samples as well as certified reference materials. Copyright © 2016. Published by Elsevier Ltd.

Tank vapor characterization project. Headspace vapor characterization of Hanford waste tank 241-BY-108: Second comparison study results from samples collected on 3/28/96

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thomas, B.L.; Pool, K.H.; Evans, J.C.

1997-01-01

This report describes the analytical results of vapor samples taken from the headspace of waste storage tank 241-BY-108 (Tank BY-108) at the Hanford Site in Washington State. The results described in this report is the second in a series comparing vapor sampling of the tank headspace using the Vapor Sampling System (VSS) and In Situ Vapor Sampling (ISVS) system without high efficiency particulate air (HEPA) prefiltration. The results include air concentrations of water (H{sub 2}O) and ammonia (NH{sub 3}), permanent gases, total non-methane organic compounds (TO-12), and individual organic analytes collected in SUMMA{trademark} canisters and on triple sorbent traps (TSTs).more » Samples were collected by Westinghouse Hanford Company (WHC) and analyzed by Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volume measurements provided by WHC.« less

Apparatus for the field determination of concentration of radioactive constituents in a medium

DOEpatents

Perkins, R.W.; Schilk, A.J.; Warner, R.A.; Wogman, N.A.

1995-08-15

The instant invention is an apparatus for determining the concentration of radioactive constituents in a test sample; such as surface soils, via rapid real-time analyses, and direct readout on location utilizing a probe made up of multiple layers of detection material used in combination with an analyzer and real-time readout unit. This is accomplished by comparing the signal received from the probe, which can discriminate between types of radiation and energies with stored patterns that are based upon experimental results. This comparison can be used in the calibration of a readout display that reads out in real-time the concentrations of constituents per given volume. For example, the concentration of constituents such as Cs-137, Sr-90, U-238 in the soil, and noble gas radionuclides such as Kr-85 in the atmosphere, can be measured in real-time, on location, without the need for laboratory analysis of samples. 14 figs.

Apparatus for the field determination of concentration of radioactive constituents in a medium

DOEpatents

Perkins, Richard W.; Schilk, Alan J.; Warner, Ray A.; Wogman, Ned A.

1995-01-01

The instant invention is an apparatus for determining the concentration of radioactive constituents in a test sample; such as surface soils, via rapid real-time analyses, and direct readout on location utilizing a probe made up of multiple layers of detection material used in combination with an analyzer and real-time readout unit. This is accomplished by comparing the signal received from the probe, which can discriminate between types of radiation and energies with stored patterns that are based upon experimental results. This comparison can be used in the calibration of a readout display that reads out in real-time the concentrations of constituents per given volume. For example, the concentration of constituents such as Cs-137, Sr-90, U-238 in the soil, and noble gas radionuclides such as Kr-85 in the atmosphere, can be measured in real-time, on location, without the need for laboratory analysis of samples.

Optimising the collection of female genital tract fluid for cytokine analysis in pregnant women.

PubMed

Short, C S; Quinlan, R; Bennett, P; Shattock, R J; Taylor, G P

2018-07-01

To better understand the immunology of pregnancy, study of female genital tract fluid (FGF) is desirable. However the optimum method of collection of FGF in pregnant women for immunological methods, specifically cytokine measurement, is unknown. A prospective study of HIV-uninfected pregnant women comparing two methods of FGF collection: polyvinyl acetal sponge collection of cervical fluid (CF) and menstrual cup collection of cervicovaginal fluid (CVF). Samples were collected at 3 time points across the second and third trimesters: 14-21, 22-25 and 26-31 weeks. Multiplex chemi-luminescent assays were used to measure: IFN-γ, IL-1β, IL-2, IL-4, IL-6, IL-8, IL-10, IL-12, IL-13 and TNF-α. Optimal methodology for cytokine normalisation (sample weight, volume and total protein) was explored. All cytokines were measurable in both fluid types. IL-1β, IL-8 and IL-6 were detected at the highest concentrations (ranking order CF > CVF > plasma). CVF collection was simpler, provided the largest volume of sample (median 0.5 g) with the potential for undiluted usage, and allowed for self-insertion. CF cytokine concentrations were intrinsically associated with sample weight and protein concentration however CVF cytokines were independent of these. Both methods of collection are robust for measurement of FGF cytokines during pregnancy. We recommend CVF collection using a menstrual cup as a viable option in pregnant women for high dimensional biological techniques. Copyright © 2018 The Authors. Published by Elsevier B.V. All rights reserved.

Development of new portable miniaturize solid phase microextraction of silver-APDC complex using micropipette tip in-syringe system couple with electrothermal atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Naeemullah; Kazi, Tasneem Gul; Afridi, Hassan Imran; Shah, Faheem; Arain, Sadaf Sadia; Arain, Salma Aslam; Panhwar, Abdul Haleem; Arain, Mariam Shahzadi; Samoon, Muhammad Kashif

2016-02-01

An innovative and simple miniaturized solid phase microextraction (M-SPME) method, was developed for preconcentration and determination of silver(I) in the fresh and waste water samples. For M-SPME, a micropipette tip packed with activated carbon cloth (ACC) as sorbent, in a syringe system. The size, morphology and elemental composition of ACC before and after adsorption of analyte have been characterized by scanning electron microscopy and energy dispersive spectroscopy. The sample solution treated with a complexing reagent, ammonium pyrrolidine dithiocarbamate (APDC), was drawn into the syringe filled with ACC and dispensed manually for 2 to 10 aspirating/dispensing cycle. Then the Ag- complex sorbed on the ACC in micropipette was quantitatively eluted by drawing and dispensing of different concentrations of acids for 2 to 5 aspirating/dispensing cycles. The extracted Ag ions with modifier were injected directly into the electrothermal atomic absorption spectrometry for analysis. The influence of different variables on the extraction efficiency, including the concentration of ligand, pH, sample volume, eluent type, concentration and volume was investigated. Validity and accuracy of the developed method was checked by the standard addition method. Reliability of the proposed methodology was checked by the relative standard deviation (%RSD), which was found to be < 5%. Under the optimized experimental variables, the limits of detection (LOD) and enhancement factors (EF), were obtained to be 0.86 ng L- 1 and 120, respectively. The proposed method was successfully applied for the determination of trace levels of silver ions in fresh and waste water samples.

Determination of ultratrace elements in natural waters by solid-phase extraction and atomic spectrometry methods.

PubMed

Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Frache, Roberto

2003-01-01

A study was carried out on the preconcentration of ultratrace amounts of cadmium, lead, manganese, copper and iron from high-salinity aqueous samples and determination by atomic spectrometry methods. Sample volume, amount of resin, loading flow rate, and elution volume were optimized in order to obtain the simultaneous preconcentration of all the analytes. Quantitative recoveries were obtained by using 200 mg of iminodiacetic resin with a loading flow rate of 2 mL min(-1), elution volume of 3 mL and sample volume of 50-450 mL. Only copper in seawater samples was not completely retained by the resin (60-70% recovery), due to unfavorable competition of iminodiacetic-active groups with organically bound metal.To quantify the metals in the eluates, two atomic spectrometry techniques were compared: electrothermal atomization atomic absorption spectrometry (ETAAS) and inductively coupled plasma-optical emission spectrometry (ICP-OES) with simultaneous CCD detection system. Both techniques are suitable for sample analysis with detection limits of 1.0, 4.7, 3.3, 6.8, and 53 ng L(-1) using ETAAS and 12, 122, 3.4, 17, and 21 ng L(-1) using ICP-OES for Cd, Pb, Mn, Cu, and Fe, respectively. Relative standard deviations of the procedures ranged from 1.7 to 14% at the sub-microg L(-1) concentration level. The accuracy of both methods was verified by analyzing various certified reference materials (river water, estuarine water, coastal and off-shore seawater).

Research to develop guidelines for cathodic protection of concentric neutral cables, volume 3

NASA Astrophysics Data System (ADS)

Hanck, J. A.; Nekoksa, G.

1982-08-01

Data associated with the corrosion of concentric neutral (CN) wires of direct buried primary cables were statistically analyzed, and guidelines for cathodic protection of CN wires for the electric utility industry were developed. The cathodic protection are reported. Field tests conducted at 36 bellholes excavated in California, Oklahoma, and North Carolina are described. Details of the electrochemical, chemical, bacteriological, and sieve analyses of native soil and imported backfill samples are also included.

High level tritiated water monitoring by Bremsstrahlung counting using a silicon drift detector

DOE Office of Scientific and Technical Information (OSTI.GOV)

Niemes, S.; Sturm, M.; Michling, R.

2015-03-15

The β-ray induced X-ray spectrometry (BIXS) is a promising technique to monitor the tritium concentration in a fuel cycle of a fusion reactor. For in-situ measurements of high level tritiated water by Bremsstrahlung counting, the characteristics of a low-noise silicon drift detector (SDD) have been examined at the Tritium Laboratory Karlsruhe (TLK). In static measurements with constant sample volume and tritium concentration, the Bremsstrahlung spectra of tritiated water samples in a concentration range of 0.02 to 15 MBq/ml have been obtained. The volume has been kept constant at 5 cm{sup 3}. The observed spectra are well above the noise threshold.more » In addition to X-rays induced by β-rays, the spectra feature X-ray fluorescence peaks of the surrounding materials. No indications of memory effects have been observed. A linear relation between the X-ray intensity and the tritium concentration was obtained and the lower detection limit of the setup has been determined to 1 MBq ml{sup -1}, assessed by the Curie criterion. In addition, the spectra obtained experimentally could be reproduced with high agreement by Monte-Carlo simulations using the GEANT4-tool-kit. It was found that the present detection system is applicable to non-invasive measurements of high-level tritiated water and the SDD is a convenient tool to detect the low energy Bremsstrahlung X-rays. (authors)« less

Effects of concentrated and dephytinized wheat bran and rice bran addition on bread properties.

PubMed

Özkaya, Berrin; Baumgartner, Burcu; Özkaya, Hazım

2018-02-01

Wheat bran and rice bran were concentrated in terms of dietary fiber and were dephytinized by two different methods (fermentation and hydrothermal). Untreated, concentrated, concentrated-dephytinized by fermentation method, and concentrated-dephytinized by hydrothermal method bran samples were each incorporated into flour at levels of 0, 10, 15, and 20%, and their effects on bread properties were investigated. Unprocessed wheat bran and rice bran addition decreased the volume yield, and the specific volume of the bread depends on the incorporation level. A further decrease was observed with the addition of concentrated bran. However, the dephytinization treatments slightly improved these values. The same pattern was observed for the total number of cells and the total cell area of bread crumbs. Both wheat bran and rice bran were observed to cause a darker crumb color, and the effects of bran samples on crumb color were more pronounced after the dephytinization treatment. The addition of concentrated wheat bran and rice bran significantly increased hardness, as well as decreasing springiness, cohesiveness, and resilience of the bread, depending on the bran levels. Although dephytinization treatments enhanced the textural properties of bread, these results were still inferior to those obtained using bread produced with untreated bran. Regarding the dephytinization treatments, the influence of fermentation treatment on bread properties was slightly beneficial compared to hydrothermal treatment. Consumption of dietary fiber offers a range of health benefits. Cereal bran has great potential as a dietary fiber source. However, this bran's high phytic acid content and adverse effects on bread quality limit that potential. It is possible to obtain high dietary fiber and low phytic acid bran samples through bran concentration and dephytinization treatments. The dephytinization treatment is an effective method for degradation of phytic acid. The negative effects of wheat bran and rice bran on bread quality decreased significantly following the dephytinization treatments. This study demonstrated that fiber-enriched bread with low phytic acid content and acceptable texture can be produced using concentrated and dephytinized bran. © 2017 Wiley Periodicals, Inc.

Detection of an amphiphilic biosample in a paper microchannel based on length.

PubMed

Chen, Yu-Tzu; Yang, Jing-Tang

2015-01-01

We developed a simple method to achieve semiquantitative detection of an amphiphilic biosample through measuring the length of flow on a microfluidic analytical device (μPAD) based on paper. When an amphiphilic sample was dripped into a straight microchannel defined with a printed wax barrier (hydrophobic) on filter paper (hydrophilic), the length of flow was affected by the reciprocal effect between the sample, the filter-paper channel and the wax barrier. The flow length decreased with increasing concentration of an amphiphilic sample because of adsorption of the sample on the hydrophobic barrier. Measurement of the flow length enabled a determination of the concentration of the amphiphilic sample. The several tested samples included surfactants (Tween 20 and Triton X-100), oligonucleotides (DNA), bovine serum albumin (BSA), human albumin, nitrite, glucose and low-density lipoprotein (LDL). The results show that the measurement of the flow length determined directly the concentration of an amphiphilic sample, whereas a non-amphiphilic sample was not amenable to this method. The proposed method features the advantages of small cost, simplicity, convenience, directness, rapidity (<5 min) and requirement of only a small volume (5 μL) of sample, with prospective applications in developing areas and sites near patients for testing at a point of care (POCT).

Rapid concentration of Bacillus and Clostridium spores from large volumes of milk, using continuous flow centrifugation.

PubMed

Agoston, Réka; Soni, Kamlesh A; McElhany, Katherine; Cepeda, Martha L; Zuckerman, Udi; Tzipori, Saul; Mohácsi-Farkas, Csilla; Pillai, Suresh D

2009-03-01

Deliberate or accidental contamination of foods such as milk, soft drinks, and drinking water with infectious agents or toxins is a major concern to health authorities. There is a critical need to develop technologies that can rapidly and efficiently separate and concentrate biothreat agents from food matrices. A key limitation of current centrifugation and filtration technologies is that they are batch processes with extensive hands-on involvement and processing times. The objective of our studies was to evaluate the continuous flow centrifugation (CFC) technique for the rapid separation and concentration of bacterial spores from large volumes of milk. We determined the effectiveness of the CFC technology for concentrating approximately 10(3) bacterial spores in 3.7 liters (1 gal) of whole milk and skim milk, using Bacillus subtilis, Bacillus atrophaeus, and Clostridium sporogenes spores as surrogates for biothreat agents. The spores in the concentrated samples were enumerated by using standard plating techniques. Three independent experiments were performed at 10,000 rpm and 0.7 liters/min flow rate. The mean B. subtilis spore recoveries were 71.3 and 56.5% in skim and whole milk, respectively, and those for B. atrophaeus were 55 and 59.3% in skim and whole milk, respectively. In contrast, mean C. sporogenes spore recoveries were 88.2 and 78.6% in skim and whole milk, respectively. The successful use of CFC to concentrate these bacterial spores from 3.7 liters of milk in 10 min shows promise for rapidly concentrating other spores from large volumes of milk.

Occurrence, distribution, and volume of metals-contaminated sediment of selected streams draining the Tri-State Mining District, Missouri, Oklahoma, and Kansas, 2011–12

USGS Publications Warehouse

Smith, D. Charlie

2016-12-14

Lead and zinc were mined in the Tri-State Mining District (TSMD) of southwest Missouri, northeast Oklahoma, and southeast Kansas for more than 100 years. The effects of mining on the landscape are still evident, nearly 50 years after the last mine ceased operation. The legacies of mining are the mine waste and discharge of groundwater from underground mines. The mine-waste piles and underground mines are continuous sources of trace metals (primarily lead, zinc, and cadmium) to the streams that drain the TSMD. Many previous studies characterized the horizontal extent of mine-waste contamination in streams but little information exists on the depth of mine-waste contamination in these streams. Characterizing the vertical extent of contamination is difficult because of the large amount of coarse-grained material, ranging from coarse gravel to boulders, within channel sediment. The U.S. Geological Survey, in cooperation with U.S. Fish and Wildlife service, collected channel-sediment samples at depth for subsequent analyses that would allow attainment of the following goals: (1) determination of the relation between concentration and depth for lead, zinc and cadmium in channel sediments and flood-plain sediments, and (2) determination of the volume of gravel-bar sediment from the surface to the maximum depth with concentrations of these metals that exceeded sediment-quality guidelines. For the purpose of this report, volume of gravel-bar sediment is considered to be distributed in two forms, gravel bars and the wetted channel, and this study focused on gravel bars. Concentrations of lead, zinc, and cadmium in samples were compared to the consensus probable effects concentration (CPEC) and Tri-State Mining District specific probable effects concentration (TPEC) sediment-quality guidelines.During the study, more than 700 sediment samples were collected from borings at multiple sites, including gravel bars and flood plains, along Center Creek, Turkey Creek, Shoal Creek, Tar Creek, and Spring River in order to characterize the vertical extent of mine waste in select streams in the TSMD. The largest concentrations of lead, zinc, and cadmium in gravel bar-sediment samples generally were detected in Turkey Creek and Tar Creek and the smallest concentrations were detected in Shoal Creek followed by the Spring River. Gravel bar-sediment samples from Turkey Creek exceeded the CPEC for cadmium (minimum of 70 percent of samples), lead (94 percent), and zinc (99 percent) at a slightly higher frequency than similar samples from Tar Creek (69 percent, 88 percent, and 96 percent, respectively). Gravel bar-sediment samples from Turkey Creek also contained the largest concentrations of cadmium (174 milligrams per kilogram [mg/kg]) and lead (7,520 mg/kg) detected; however, the largest zinc concentration (46,600 mg/kg) was detected in a gravel bar-sediment sample from Tar Creek. In contrast, none of the 65 gravel bar-sediment samples from Shoal Creek contained cadmium above the x-ray fluorescence reporting level of 12 mg/kg, and lead and zinc exceeded the CPEC in only 12 percent and 74 percent of samples, respectively. In most cases, concentrations of lead and zinc above the CPEC or TPEC were present at the maximum depth of boring, which indicated that nearly the entire thickness of sediment in the stream has been contaminated by mine wastes. Approximately 284,000 cubic yards of channel sediment from land surface to the maximum depth that exceeded the CPEC and approximately 236,000 cubic yards of channel sediment from land surface to the maximum depth that exceeded the TPEC were estimated along 37.6 of the 55.1 miles of Center Creek, Turkey Creek, Shoal Creek, and Tar Creek examined in this study. Mine-waste contamination reported along additional reaches of these streams is beyond the scope of this study. Flood-plain cores collected in the TSMD generally only had exceedances of the CPEC and TPEC for lead and zinc in the top 1 or 2 feet of soil with a few exceptions, such as cores in low areas near the stream or cores in areas disturbed by past mining.

A Fast, Accurate and Sensitive GC-FID Method for the Analyses of Glycols in Water and Urine

NASA Technical Reports Server (NTRS)

Kuo, C. Mike; Alverson, James T.; Gazda, Daniel B.

2017-01-01

Glycols, specifically ethylene glycol and 1,2-propanediol, are some of the major organic compounds found in the humidity condensate samples collected on the International Space Station. The current analytical method for glycols is a GC/MS method with direct sample injection. This method is simple and fast, but it is not very sensitive. Reporting limits for ethylene glycol and 1,2-propanediol are only 1 ppm. A much more sensitive GC/FID method was developed, in which glycols were derivatized with benzoyl chloride for 10 minutes before being extracted with hexane. Using 1,3-propanediol as an internal standard, the detection limits for the GC/FID method was determined to be 50 ppb and the analysis only takes 7 minutes. Data from the GC/MS and the new GC/FID methods shows excellent agreement with each other. Factors affecting the sensitivity, including sample volume, NaOH concentration and volume, volume of benzoyl chloride, reaction time and temperature, were investigated. Interferences during derivatization and possible method to reduce interferences were also investigated.

Analysis of microdialysate monoamines, including noradrenaline, dopamine and serotonin, using capillary ultra-high performance liquid chromatography and electrochemical detection.

PubMed

Ferry, Barbara; Gifu, Elena-Patricia; Sandu, Ioana; Denoroy, Luc; Parrot, Sandrine

2014-03-01

Electrochemical methods are very often used to detect catecholamine and indolamine neurotransmitters separated by conventional reverse-phase high performance liquid chromatography (HPLC). The present paper presents the development of a chromatographic method to detect monoamines present in low-volume brain dialysis samples using a capillary column filled with sub-2μm particles. Several parameters (repeatability, linearity, accuracy, limit of detection) for this new ultrahigh performance liquid chromatography (UHPLC) method with electrochemical detection were examined after optimization of the analytical conditions. Noradrenaline, adrenaline, serotonin, dopamine and its metabolite 3-methoxytyramine were separated in 1μL of injected sample volume; they were detected above concentrations of 0.5-1nmol/L, with 2.1-9.5% accuracy and intra-assay repeatability equal to or less than 6%. The final method was applied to very low volume dialysates from rat brain containing monoamine traces. The study demonstrates that capillary UHPLC with electrochemical detection is suitable for monitoring dialysate monoamines collected at high sampling rate. Copyright © 2014 Elsevier B.V. All rights reserved.

Sample Processor for Life on Icy Worlds (SPLIce): Design and Test Results

NASA Technical Reports Server (NTRS)

Chinn, Tori N.; Lee, Anthony K.; Boone, Travis D.; Tan, Ming X.; Chin, Matthew M.; McCutcheon, Griffin C.; Horne, Mera F.; Padgen, Michael R.; Blaich, Justin T.; Forgione, Joshua B.;

A Dual Wedge Microneedle for sampling of perilymph solution via round window membrane

PubMed Central

Watanabe, Hirobumi; Cardoso, Luis; Lalwani, Anil K.; Kysar, Jeffrey W.

2017-01-01

Objective Precision medicine for inner-ear disease is hampered by the absence of a methodology to sample inner-ear fluid atraumatically. The round window membrane (RWM) is an attractive portal for accessing cochlear fluids as it heals spontaneously. In this study, we report on the development of a microneedle for perilymph sampling that minimizes size of RWM perforation, facilitates quick aspiration, and provides precise volume control. Methods Considering the mechanical anisotropy of the RWM and hydrodynamics through a microneedle, a 31G stainless steel pipe was machined into wedge-shaped design via electrical discharge machining. Guinea pig RWM was penetrated in vitro, and 1 μ1 of perilymph was sampled and analyzed via UV-vis spectroscopy. Results The prototype wedge shaped needle created oval perforation with minor and major diameter of 143 and 344 μm (n=6). The sampling duration and standard deviation of aspirated volume were seconds and 6.8% respectively. The protein concentration was 1.74 mg/mL. Conclusion The prototype needle facilitated precise perforation of RWMs and rapid aspiration of cochlear fluid with precise volume control. The needle design is promising and requires testing in human cadaveric temporal bone and further optimization to become clinically viable. PMID:26888440

Novel system using microliter order sample volume for measuring arterial radioactivity concentrations in whole blood and plasma for mouse PET dynamic study.

PubMed

Kimura, Yuichi; Seki, Chie; Hashizume, Nobuya; Yamada, Takashi; Wakizaka, Hidekatsu; Nishimoto, Takahiro; Hatano, Kentaro; Kitamura, Keishi; Toyama, Hiroshi; Kanno, Iwao

2013-11-21

This study aimed to develop a new system, named CD-Well, for mouse PET dynamic study. CD-Well allows the determination of time-activity curves (TACs) for arterial whole blood and plasma using 2-3 µL of blood per sample; the minute sample size is ideal for studies in small animals. The system has the following merits: (1) measures volume and radioactivity of whole blood and plasma separately; (2) allows measurements at 10 s intervals to capture initial rapid changes in the TAC; and (3) is compact and easy to handle, minimizes blood loss from sampling, and delay and dispersion of the TAC. CD-Well has 36 U-shaped channels. A drop of blood is sampled into the opening of the channel and stored there. After serial sampling is completed, CD-Well is centrifuged and scanned using a flatbed scanner to define the regions of plasma and blood cells. The length measured is converted to volume because the channels have a precise and uniform cross section. Then, CD-Well is exposed to an imaging plate to measure radioactivity. Finally, radioactivity concentrations are computed. We evaluated the performance of CD-Well in in vitro measurement and in vivo (18)F-fluorodeoxyglucose and [(11)C]2-carbomethoxy-3β-(4-fluorophenyl) tropane studies. In in vitro evaluation, per cent differences (mean±SE) from manual measurement were 4.4±3.6% for whole blood and 4.0±3.5% for plasma across the typical range of radioactivity measured in mouse dynamic study. In in vivo studies, reasonable TACs were obtained. The peaks were captured well, and the time courses coincided well with the TAC derived from PET imaging of the heart chamber. The total blood loss was less than 200 µL, which had no physiological effect on the mice. CD-Well demonstrates satisfactory performance, and is useful for mouse PET dynamic study.

Paper-based microfluidic devices on the crime scene: A simple tool for rapid estimation of post-mortem interval using vitreous humour.

PubMed

Garcia, Paulo T; Gabriel, Ellen F M; Pessôa, Gustavo S; Santos Júnior, Júlio C; Mollo Filho, Pedro C; Guidugli, Ruggero B F; Höehr, Nelci F; Arruda, Marco A Z; Coltro, Wendell K T

2017-06-29

This paper describes for the first time the use of paper-based analytical devices at crime scenes to estimate the post-mortem interval (PMI), based on the colorimetric determination of Fe 2+ in vitreous humour (VH) samples. Experimental parameters such as the paper substrate, the microzone diameter, the sample volume and the 1,10-phenanthroline (o-phen) concentration were optimised in order to ensure the best analytical performance. Grade 1 CHR paper, microzone with diameter of 5 mm, a sample volume of 4 μL and an o-phen concentration of 0.05 mol/L were chosen as the optimum experimental conditions. A good linear response was observed for a concentration range of Fe 2+ between 2 and 10 mg/L and the calculated values for the limit of detection (LOD) and limit of quantification (LOQ) were 0.3 and 0.9 mg/L, respectively. The specificity of the Fe 2+ colorimetric response was tested in the presence of the main interfering agents and no significant differences were found. After selecting the ideal experimental conditions, four HV samples were investigated on paper-based devices. The concentration levels of Fe 2+ achieved for samples #1, #2, #3 and #4 were 0.5 ± 0.1, 0.7 ± 0.1, 1.2 ± 0.1 and 15.1 ± 0.1 mg/L, respectively. These values are in good agreement with those calculated by ICP-MS. It important to note that the concentration levels measured using both techniques are proportional to the PMI. The limitation of the proposed analytical device is that it is restricted to a PMI greater than 1 day. The capability of providing an immediate answer about the PMI on the crime scene without any sophisticated instrumentation is a great achievement in modern instrumentation for forensic chemistry. The strategy proposed in this study could be helpful in many criminal investigations. Copyright © 2017 Elsevier B.V. All rights reserved.

Spatial considerations during cryopreservation of a large volume sample.

PubMed

Kilbride, Peter; Lamb, Stephen; Milne, Stuart; Gibbons, Stephanie; Erro, Eloy; Bundy, James; Selden, Clare; Fuller, Barry; Morris, John

2016-08-01

There have been relatively few studies on the implications of the physical conditions experienced by cells during large volume (litres) cryopreservation - most studies have focused on the problem of cryopreservation of smaller volumes, typically up to 2 ml. This study explores the effects of ice growth by progressive solidification, generally seen during larger scale cryopreservation, on encapsulated liver hepatocyte spheroids, and it develops a method to reliably sample different regions across the frozen cores of samples experiencing progressive solidification. These issues are examined in the context of a Bioartificial Liver Device which requires cryopreservation of a 2 L volume in a strict cylindrical geometry for optimal clinical delivery. Progressive solidification cannot be avoided in this arrangement. In such a system optimal cryoprotectant concentrations and cooling rates are known. However, applying these parameters to a large volume is challenging due to the thermal mass and subsequent thermal lag. The specific impact of this to the cryopreservation outcome is required. Under conditions of progressive solidification, the spatial location of Encapsulated Liver Spheroids had a strong impact on post-thaw recovery. Cells in areas first and last to solidify demonstrated significantly impaired post-thaw function, whereas areas solidifying through the majority of the process exhibited higher post-thaw outcome. It was also found that samples where the ice thawed more rapidly had greater post-thaw viability 24 h post-thaw (75.7 ± 3.9% and 62.0 ± 7.2% respectively). These findings have implications for the cryopreservation of large volumes with a rigid shape and for the cryopreservation of a Bioartificial Liver Device. Copyright © 2016 The Authors. Published by Elsevier Inc. All rights reserved.

Comparison of nitrate, pesticides, and volatile organic compounds in samples from monitoring and public-supply wells, Kirkwood-Cohansey aquifer system, southern New Jersey

USGS Publications Warehouse

Stackelberg, Paul E.; Kauffman, L.J.; Baehr, A.L.; Ayers, M.A.

2000-01-01

The number and total concentration of volatile organic compounds (VOCs) per sample were significantly greater in water from public-supply wells than in water from shallow and moderate-depth monitoring wells in the surficial Kirkwood-Cohansey aquifer system in the Glassboro area of southern New Jersey. In contrast, concentrations of nitrate (as nitrogen) and the number and total concentration of pesticides per sample were statistically similar in samples from shallow and moderate-depth monitoring wells and those from public-supply wells. VOCs in ground water typically are derived from point sources, which commonly exist in urban areas and which result in spatially variable contaminant concentrations near the water table. Because larger volumes of water are withdrawn from public-supply wells than from monitoring wells, their contributing areas are larger and, therefore, they are more likely to intercept water flowing from VOC point sources. Additionally, public-supply wells intercept flow paths that span a large temporal interval. Public-supply wells in the Glassboro study area withdraw water flowing along short paths, which contains VOCs that recently entered the aquifer system, and water flowing along relatively long paths, which contains VOCs that originated from the degradation of parent compounds or that are associated with past land uses. Because the volume of water withdrawn from monitoring wells is small and because shallow monitoring wells are screened near the water table, they generally intercept only relatively short flow paths. Therefore, samples from these wells represent relatively recent, discrete time intervals and contain both fewer VOCs and a lower total VOC concentration than samples from public-supply wells. Nitrate and pesticides in ground water typically are derived from nonpoint sources, which commonly are found in both agricultural and urban areas and typically result in lowlevel, relatively uniform concentrations near the water table. Because nonpoint sources are diffuse and because processes such as degradation or sorption/dispersion do not occur at rates sufficient to prevent detection of these constituents in parts of the aquifer used for domestic and public supply in the study area, concentrations of nitrate and pesticides and numbers of pesticide compounds are likely to be similar in samples from shallow monitoring wells and samples from public-supply wells. Results of a comparison of (1) the general characteristics of, and water-quality data from, public-supply wells in the Glassboro study area to available data from public-supply wells screened in the Kirkwood-Cohansey aquifer system outside the study area, and (2) land-use settings, soil characteristics, and aquifer properties in and outside the study area indicate that the findings of this study likely are applicable to the entire extent of the Kirkwood- Cohansey aquifer system in southern New Jersey.

Combination induction plasma tube and current concentrator for introducing a sample into a plasma

DOEpatents

Hull, Donald E.; Bieniewski, Thomas M.

1988-01-01

An induction plasma tube in combination with a current concentrator. The rent concentrator has a substantially cylindrical body having an open end and a partially closed end which defines an aperture. A first slot extends the longitudinal length of the cylindrical body and a second slot extends radially outward from the aperture. Together the first and second slots form a single L-shaped slot. The current concentrator is disposed within a volume bounded by an induction coil substantially along the axis thereof, and when power is applied to the induction coil a concentrated current is induced within the current concentrator aperture. The concentrator is moveable relative to the coil along the longitudinal axis of the coil to control the amount of current which is concentrated at the aperture.

Isolation of organic acids from large volumes of water by adsorption on macroporous resins

USGS Publications Warehouse

Aiken, George R.; Suffet, I.H.; Malaiyandi, Murugan

1987-01-01

Adsorption on synthetic macroporous resins, such as the Amberlite XAD series and Duolite A-7, is routinely used to isolate and concentrate organic acids from forge volumes of water. Samples as large as 24,500 L have been processed on site by using these resins. Two established extraction schemes using XAD-8 and Duolite A-7 resins are described. The choice of the appropriate resin and extraction scheme is dependent on the organic solutes of interest. The factors that affect resin performance, selectivity, and capacity for a particular solute are solution pH, resin surface area and pore size, and resin composition. The logistical problems of sample handling, filtration, and preservation are also discussed.

TWO-PHASE FORMATION IN SOLUTIONS OF TOBACCO MOSAIC VIRUS AND THE PROBLEM OF LONG-RANGE FORCES

PubMed Central

Oster, Gerald

1950-01-01

In a nearly salt-free medium, a dilute tobacco mosaic virus solution of rod-shaped virus particles of uniform length forms two phases; the bottom optically anisotropic phase has a greater virus concentration than has the top optically isotropic phase. For a sample containing particles of various lengths, the bottom phase contains longer particles than does the top and the concentrations top and bottom are nearly equal. The longer the particles the less the minimum concentration necessary for two-phase formation. Increasing the salt concentration increases the minimum concentration. The formation of two phases is explained in terms of geometrical considerations without recourse to the concept of long-range attractive forces. The minimum concentration for two-phase formation is that concentration at which correlation in orientation between the rod-shaped particles begins to take place. This concentration is determined by the thermodynamically effective size and shape of the particles as obtained from the concentration dependence of the osmotic pressure of the solutions measured by light scattering. The effective volume of the particles is introduced into the theory of Onsager for correlation of orientation of uniform size rods and good agreement with experiment is obtained. The theory is extended to a mixture of non-uniform size rods and to the case in which the salt concentration is varied, and agreement with experiment is obtained. The thermodynamically effective volume of the particles and its dependence on salt concentration are explained in terms of the shape of the particles and the electrostatic repulsion between them. Current theories of the hydration of proteins and of long-range forces are critically discussed. The bottom layer of freshly purified tobacco mosaic virus samples shows Bragg diffraction of visible light. The diffraction data indicate that the virus particles in solution form three-dimensional crystals approximately the size of crystalline inclusion bodies found in the cells of plants suffering from the disease. PMID:15422102

Chapter 3. Determination of semivolatile organic compounds and polycyclic aromatic hydrocarbons in solids by gas chromatography/mass spectrometry

USGS Publications Warehouse

Zaugg, Steven D.; Burkhardt, Mark R.; Burbank, Teresa L.; Olson, Mary C.; Iverson, Jana L.; Schroeder, Michael P.

2006-01-01

A method for the determination of 38 polycyclic aromatic hydrocarbons (PAHs) and semivolatile organic compounds in solid samples is described. Samples are extracted using a pressurized solvent extraction system. The compounds of interest are extracted from the solid sample twice at 13,800 kilopascals; first at 120 degrees Celsius using a water/isopropyl alcohol mixture (50:50, volume-to-volume ratio), and then the sample is extracted at 200 degrees Celsius using a water/isopropyl alcohol mixture (80:20, volume-to-volume ratio). The compounds are isolated using disposable solid-phase extraction (SPE) cartridges containing divinylbenzene-vinylpyrrolidone copolymer resin. The cartridges are dried with nitrogen gas, and then sorbed compounds are eluted from the SPE material using a dichloromethane/diethyl ether mixture (80:20, volume-to-volume ratio) and passed through a sodium sulfate/Florisil SPE cartridge to remove residual water and to further clean up the extract. The concentrated extract is solvent exchanged into ethyl acetate and the solvent volume reduced to 0.5 milliliter. Internal standard compounds are added prior to analysis by capillary-column gas chromatography/mass spectrometry. Comparisons of PAH data for 28 sediment samples extracted by Soxhlet and the accelerated solvent extraction (ASE) method described in this report produced similar results. Extraction of PAH compounds from standard reference material using this method also compared favorably with Soxhlet extraction. The recoveries of PAHs less than molecular weight 202 (pyrene or fluoranthene) are higher by up to 20 percent using this ASE method, whereas the recoveries of PAHs greater than or equal to molecular weight 202 are equivalent. This ASE method of sample extraction of solids has advantages over conventional Soxhlet extraction by increasing automation of the extraction process, reducing extraction time, and using less solvent. Extract cleanup also is greatly simplified because SPE replaces commonly used gel permeation chromatography. The performance of the method (as expressed by mean recoveries and mean precision) was determined using Ottawa sand, a commercially available topsoil, and an environmental stream sediment, fortified at 1.5 and 15 micrograms per compound. Recoveries of PAH and semivolatile compounds in Ottawa sand samples fortified at 1.5 micrograms averaged 88 percent ? 9.4 percent relative standard deviation, and calculated initial method detection limits per compound averaged 14 micrograms per kilogram, assuming a 25-gram sample size. The recovery for 1,2,4-trichlorobenzene is less than 60 percent; thus, the concentration of this compound will always be reported as estimated with the E remark code. The analysis of 25 alkylated PAH homolog groups also can be determined with this method with extra data analysis and review, but because of the lack of authentic reference standard compounds, these results are considered to be semiquantitative. The PAH homolog groups are quantitated using the response factor of a parent PAH method compound, if available. Precision data for the alkylated PAH homologs detected in a marine sediment standard reference material (SRM 1944) also are presented to document and demonstrate method capability.

Variation in aluminum, iron, and particle concentrations in oxic groundwater samples collected by use of tangential-flow ultrafiltration with low-flow sampling

NASA Astrophysics Data System (ADS)

Szabo, Zoltan; Oden, Jeannette H.; Gibs, Jacob; Rice, Donald E.; Ding, Yuan

2002-02-01

Particulates that move with ground water and those that are artificially mobilized during well purging could be incorporated into water samples during collection and could cause trace-element concentrations to vary in unfiltered samples, and possibly in filtered samples (typically 0.45-um (micron) pore size) as well, depending on the particle-size fractions present. Therefore, measured concentrations may not be representative of those in the aquifer. Ground water may contain particles of various sizes and shapes that are broadly classified as colloids, which do not settle from water, and particulates, which do. In order to investigate variations in trace-element concentrations in ground-water samples as a function of particle concentrations and particle-size fractions, the U.S. Geological Survey, in cooperation with the U.S. Air Force, collected samples from five wells completed in the unconfined, oxic Kirkwood-Cohansey aquifer system of the New Jersey Coastal Plain. Samples were collected by purging with a portable pump at low flow (0.2-0.5 liters per minute and minimal drawdown, ideally less than 0.5 foot). Unfiltered samples were collected in the following sequence: (1) within the first few minutes of pumping, (2) after initial turbidity declined and about one to two casing volumes of water had been purged, and (3) after turbidity values had stabilized at less than 1 to 5 Nephelometric Turbidity Units. Filtered samples were split concurrently through (1) a 0.45-um pore size capsule filter, (2) a 0.45-um pore size capsule filter and a 0.0029-um pore size tangential-flow filter in sequence, and (3), in selected cases, a 0.45-um and a 0.05-um pore size capsule filter in sequence. Filtered samples were collected concurrently with the unfiltered sample that was collected when turbidity values stabilized. Quality-assurance samples consisted of sequential duplicates (about 25 percent) and equipment blanks. Concentrations of particles were determined by light scattering.

Survey of polyfluorinated chemicals (PFCs) in the atmosphere over the northeast Atlantic Ocean

NASA Astrophysics Data System (ADS)

Shoeib, Mahiba; Vlahos, Penny; Harner, Tom; Peters, Andrew; Graustein, Margaret; Narayan, Julie

2010-08-01

High volume air sampling in Bermuda, Sable Island (Nova Scotia) and along a cruise track from the Gulf of Mexico to northeast coast of the USA, was carried out to assess air concentrations, particle-gas partitioning and transport of polyfluorinated chemicals (PFCs) in this region. Samples were collected in the summer of 2007. Targeted compounds included the neutral PFCs: fluorotelomer alcohols (FTOHs), perfluoroalkyl sulfonamides (FOSAs) and perfluoroalkyl sulfonamido ethanols (FOSEs). Among the FTOHs, 8:2 FTOH was dominant in all samples. Sum of the concentration of FTOHs (gas+particle phase) were higher in Bermuda (mean, 34 pg m -3) compared to Sable Island (mean, 16 pg m -3). In cruise samples, sum of FTOHs were highly variable (mean, 81 pg m -3) reflecting contributions from land-based sources in the northeast USA with concentrations reaching as high as 156 pg m -3. Among the FOSAs and FOSEs, MeFOSE was dominant in all samples. In Bermuda, levels of MeFOSE were exceptionally high (mean, 62 pg m -3), exceeding the FTOHs. Sable Island samples also exhibited the dominance of MeFOSE but at a lower concentration (mean, 15 pg m -3). MeFOSE air concentrations (pg m -3) in cruise samples ranged from 1.6 to 73 and were not linked to land-based sources. In fact high concentrations of MeFOSE observed in Bermuda were associated with air masses that originated over the Atlantic Ocean. The partitioning to particles for 8:2 FTOH, 10:2 FTOH, MeFOSE and EtFOSE ranged from as high as 15 to 42% for cruise samples to 0.9 to 14% in Bermuda. This study provides key information for validating and developing partitioning and transport models for the PFCs.

Assessment of the Extraction Methods for Monitoring Phthalate Emerging Contaminants in Groundwater and Tap Water

NASA Astrophysics Data System (ADS)

Cotto, I.; Padilla, I. Y.; De Jesús, N. H.; Torres, P. M.

2015-12-01

Trace organic contaminants such as phthalates, among other chemicals of emerging concerns, have not historically been considered as pollutants but are being detected in water, posing a potential risk to public health and the environment. One of the most common phthalates of particular concern is di-(2-ethylhexyl) phthalate (DEHP), a plasticizer normally found in plastics and consumer products, including: cosmetics, pharmaceuticals, medical devices, food packages, water bottles, and wiring cables. DEHP has been associated with preterm birth, a major cause of neonatal mortality and health complications. This study aims at monitoring the presence and concentration of DEHP and other phthalates in groundwater and tap water systems in Puerto Rico, which has one of the highest rates of preterm birth in the U.S. The Environmental Protection Agency (EPA) suggests a liquid-liquid extraction method that uses methylene chloride as the preferred organic solvent for the extractions. This work presents modified EPA methods that reduce the volume of sample and solvent used, lower the time of analysis, increase productivity, and decrease hazards and waste. Distribution coefficient of DEHP between methylene chloride and water are estimated and related to sample extraction efficiency. Research results indicate that DEHP is in fact distributed between water and methylene chloride with a distribution coefficient average value of 1.24. The study concludes that the sample and solvent volumes have influence on the efficiency but have not an effect on the distribution coefficient. The tests show higher extraction efficiencies for lower DEHP concentrations and higher extraction volumes. Results from the water analysis show presence of DEHP in 55% of groundwater and 44% of tap water samples, indicating a potential exposure through water.

Permeable pavement study (Edison)

EPA Pesticide Factsheets

While permeable pavement is increasingly being used to control stormwater runoff, field-based, side-by-side investigations on the effects different pavement types have on nutrient concentrations present in stormwater runoff are limited. In 2009, the U.S. EPA constructed a 0.4-ha parking lot in Edison, New Jersey, that incorporated permeable interlocking concrete pavement (PICP), pervious concrete (PC), and porous asphalt (PA). Each permeable pavement type has four, 54.9-m2, lined sections that direct all infiltrate into 5.7-m3 tanks enabling complete volume collection and sampling. This paper highlights the results from a 12-month period when samples were collected from 13 rainfall/runoff events and analyzed for nitrogen species, orthophosphate, and organic carbon. Differences in infiltrate concentrations among the three permeable pavement types were assessed and compared with concentrations in rainwater samples and impervious asphalt runoff samples, which were collected as controls. Contrary to expectations based on the literature, the PA infiltrate had significantly larger total nitrogen (TN) concentrations than runoff and infiltrate from the other two permeable pavement types, indicating that nitrogen leached from materials in the PA strata. There was no significant difference in TN concentration between runoff and infiltrate from either PICP or PC, but TN in runoff was significantly larger than in the rainwater, suggesting meaningful inter-event dry de

Real-time and integrated measurement of potential human exposure to particle-bound polycyclic aromatic hydrocarbons (PAHs) from aircraft exhaust.

PubMed Central

Childers, J W; Witherspoon, C L; Smith, L B; Pleil, J D

2000-01-01

We used real-time monitors and low-volume air samplers to measure the potential human exposure to airborne polycyclic aromatic hydrocarbon (PAH) concentrations during various flight-related and ground-support activities of C-130H aircraft at an Air National Guard base. We used three types of photoelectric aerosol sensors (PASs) to measure real-time concentrations of particle-bound PAHs in a break room, downwind from a C-130H aircraft during a four-engine run-up test, in a maintenance hangar, in a C-130H aircraft cargo bay during cargo-drop training, downwind from aerospace ground equipment (AGE), and in a C-130H aircraft cargo bay during engine running on/off (ERO) loading and backup exercises. Two low-volume air samplers were collocated with the real-time monitors for all monitoring events except those in the break room and during in-flight activities. Total PAH concentrations in the integrated-air samples followed a general trend: downwind from two AGE units > ERO-loading exercise > four-engine run-up test > maintenance hangar during taxi and takeoff > background measurements in maintenance hangar. Each PAH profile was dominated by naphthalene, the alkyl-substituted naphthalenes, and other PAHs expected to be in the vapor phase. We also found particle-bound PAHs, such as fluoranthene, pyrene, and benzo[a]pyrene in some of the sample extracts. During flight-related exercises, total PAH concentrations in the integrated-air samples were 10-25 times higher than those commonly found in ambient air. Real-time monitor mean responses generally followed the integrated-air sample trends. These monitors provided a semiquantitative temporal profile of ambient PAH concentrations and showed that PAH concentrations can fluctuate rapidly from a baseline level < 20 to > 4,000 ng/m(3) during flight-related activities. Small handheld models of the PAS monitors exhibited potential for assessing incidental personal exposure to particle-bound PAHs in engine exhaust and for serving as a real-time dosimeter to indicate when respiratory protection is advisable. PMID:11017890

Application of Medical Magnetic Resonance Imaging for Particle Concentration Measurement

NASA Astrophysics Data System (ADS)

Borup, Daniel; Elkins, Christopher; Eaton, John

2014-11-01

Particle transport and deposition in internal flows is important in a range of applications such as dust aggregation in turbine engines and aerosolized medicine deposition in human airways. Unlike optical techniques, Magnetic Resonance Imaging (MRI) is well suited for complex applications in which optical access is not possible. Here we present efforts to measure 3D particle concentration distribution using MRI. Glass particles dispersed in water flow reduce MRI signal from a spin-echo or gradient-echo scanning sequence by decreasing spin density and dephasing the spins present in the fluid. A preliminary experiment was conducted with a particle streak injected at the centerline of a turbulent round pipe flow with a U bend. Measurements confirmed that signal strength was related to particle concentration and showed the effects of gravitational settling and turbulent dispersion. Next, measurements of samples in a mixing chamber were taken. Particle volume fraction was varied and sensitivity to particle/fluid velocity was investigated. These results give a relationship between MRI signal, particle volume fraction, MRI sequence echo time, and spin relaxation parameters that can be used to measure local particle volume fraction in other turbulent flows of interest.

The use of multilevel sampling techniques for determining shallow aquifer nitrate profiles.

PubMed

Lasagna, Manuela; De Luca, Domenico Antonio

2016-10-01

Nitrate is a worldwide pollutant in aquifers. Shallow aquifer nitrate concentrations generally display vertical stratification, with a maximum concentration immediately below the water level. The concentration then gradually decreases with depth. Different techniques can be used to highlight this stratification. The paper aims at comparing the advantages and limitations of three open hole multilevel sampling techniques (packer system, dialysis membrane samplers and bailer), chosen on the base of a literary review, to highlight a nitrate vertical stratification under the assumption of (sub)horizontal flow in the aquifer. The sampling systems were employed at three different times of the year in a shallow aquifer piezometer in northern Italy. The optimal purge time, equilibration time and water volume losses during the time in the piezometer were evaluated. Multilevel techniques highlighted a similar vertical nitrate stratification, present throughout the year. Indeed, nitrate concentrations generally decreased with depth downwards, but with significantly different levels in the sampling campaigns. Moreover, the sampling techniques produced different degrees of accuracy. More specifically, the dialysis membrane samplers provided the most accurate hydrochemical profile of the shallow aquifer and they appear to be necessary when the objective is to detect the discontinuities in the nitrate profile. Bailer and packer system showed the same nitrate profile with little differences of concentration. However, the bailer resulted much more easier to use.

Development of a Pipeline for Exploratory Metabolic Profiling of Infant Urine

PubMed Central

Jackson, Frances; Georgakopoulou, Nancy; Kaluarachchi, Manuja; Kyriakides, Michael; Andreas, Nicholas; Przysiezna, Natalia; Hyde, Matthew J.; Modi, Neena; Nicholson, Jeremy K.; Wijeyesekera, Anisha; Holmes, Elaine

2017-01-01

Numerous metabolic profiling pipelines have been developed to characterize the composition of human biofluids and tissues, the vast majority of these being for studies in adults. To accommodate limited sample volume and to take into account the compositional differences between adult and infant biofluids, we developed and optimized sample handling and analytical procedures for studying urine from newborns. A robust pipeline for metabolic profiling using NMR spectroscopy was established, encompassing sample collection, preparation, spectroscopic measurement, and computational analysis. Longitudinal samples were collected from five infants from birth until 14 months of age. Methods of extraction and effects of freezing and sample dilution were assessed, and urinary contaminants from breakdown of polymers in a range of diapers and cotton wool balls were identified and compared, including propylene glycol, acrylic acid, and tert-butanol. Finally, assessment of urinary profiles obtained over the first few weeks of life revealed a dramatic change in composition, with concentrations of phenols, amino acids, and betaine altering systematically over the first few months of life. Therefore, neonatal samples require more stringent standardization of experimental design, sample handling, and analysis compared to that of adult samples to accommodate the variability and limited sample volume. PMID:27476583

Recent Advances in Water Analysis with Gas Chromatograph Mass Spectrometers

NASA Technical Reports Server (NTRS)

MacAskill, John A.; Tsikata, Edem

2014-01-01

We report on progress made in developing a water sampling system for detection and analysis of volatile organic compounds in water with a gas chromatograph mass spectrometer (GCMS). Two approaches are described herein. The first approach uses a custom water pre-concentrator for performing trap and purge of VOCs from water. The second approach uses a custom micro-volume, split-splitless injector that is compatible with air and water. These water sampling systems will enable a single GC-based instrument to analyze air and water samples for VOC content. As reduced mass, volume, and power is crucial for long-duration, manned space-exploration, these water sampling systems will demonstrate the ability of a GCMS to monitor both air and water quality of the astronaut environment, thereby reducing the amount of required instrumentation for long duration habitation. Laboratory prototypes of these water sampling systems have been constructed and tested with a quadrupole ion trap mass spectrometer as well as a thermal conductivity detector. Presented herein are details of these water sampling system with preliminary test results.

Atmospheric Concentrations of Persistent Organic Pollutants in the Southern Ocean

NASA Astrophysics Data System (ADS)

Vlahos, P.; Edson, J.; Cifuentes, A.; McGillis, W. R.; Zappa, C.

2008-12-01

Long-range transport of persistent organic pollutant (POPs) is a global concern. Remote regions such as the Southern Ocean are greatly under-sampled though critical components in understanding POPs cycling. Over 20 high-volume air samples were collected in the Southern Ocean aboard the RV Brown during the GASEX III experiment between Mar 05 to April 9 2008. The relatively stationary platform (51S,38W) enabled the collection of a unique atmospheric time series at this open ocean station. Air sampling was also conducted across transects from Punto Arenas, Chile and to Montevideo, Uruguay. Samples were collected using glass sleeves packed with poly-urethane foam plugs and C-18 resin in order to collect target organic pollutants (per-fluorinated compounds, currently and historically used pesticides) in this under-sampled region. Here we present POPs concentrations and trends over the sampled period and compare variations with air parcel back trajectories to establish potential origins of their long-range transport.

Electrokinetic Sample Preconcentration and Hydrodynamic Sample Injection for Microchip Electrophoresis Using a Pneumatic Microvalve

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cong, Yongzheng; Katipamula, Shanta; Geng, Tao

2016-02-01

A microfluidic platform was developed to perform online electrokinetic sample preconcentration and rapid hydrodynamic sample injection for electrophoresis using a single microvalve. The PDMS microchip consists of a separation channel, a side channel for sample introduction, and a control channel which is used as a pneumatic microvalve aligned at the intersection of the two flow channels. The closed microvalve, created by multilayer soft lithography, can serve as a preconcentrator under an applied electric potential, enabling current to pass through while blocking bulk flow. Once analytes are concentrated, the valve is briefly opened and the stacked sample is pressure injected intomore » the separation channel for electrophoretic separation. Fluorescently labeled peptides were enriched by a factor of ~450 in 230 s. The performance of the platform was validated by the online preconcentration, injection and electrophoretic separation of fluorescently labeled peptides. This method enables both rapid analyte concentration and controlled injection volume for high sensitivity, high resolution capillary electrophoresis.« less

A simplified method to recover urinary vesicles for clinical applications, and sample banking.

PubMed

Musante, Luca; Tataruch, Dorota; Gu, Dongfeng; Benito-Martin, Alberto; Calzaferri, Giulio; Aherne, Sinead; Holthofer, Harry

2014-12-23

Urinary extracellular vesicles provide a novel source for valuable biomarkers for kidney and urogenital diseases: Current isolation protocols include laborious, sequential centrifugation steps which hampers their widespread research and clinical use. Furthermore, large individual urine sample volumes or sizable target cohorts are to be processed (e.g. for biobanking), the storage capacity is an additional problem. Thus, alternative methods are necessary to overcome such limitations. We have developed a practical vesicle isolation technique to yield easily manageable sample volumes in an exceptionally cost efficient way to facilitate their full utilization in less privileged environments and maximize the benefit of biobanking. Urinary vesicles were isolated by hydrostatic dialysis with minimal interference of soluble proteins or vesicle loss. Large volumes of urine were concentrated up to 1/100 of original volume and the dialysis step allowed equalization of urine physico-chemical characteristics. Vesicle fractions were found suitable to any applications, including RNA analysis. In the yield, our hydrostatic filtration dialysis system outperforms the conventional ultracentrifugation-based methods and the labour intensive and potentially hazardous step of ultracentrifugations are eliminated. Likewise, the need for trained laboratory personnel and heavy initial investment is avoided. Thus, our method qualifies as a method for laboratories working with urinary vesicles and biobanking.

A Simplified Method to Recover Urinary Vesicles for Clinical Applications, and Sample Banking

PubMed Central

Musante, Luca; Tataruch, Dorota; Gu, Dongfeng; Benito-Martin, Alberto; Calzaferri, Giulio; Aherne, Sinead; Holthofer, Harry

2014-01-01

Urinary extracellular vesicles provide a novel source for valuable biomarkers for kidney and urogenital diseases: Current isolation protocols include laborious, sequential centrifugation steps which hampers their widespread research and clinical use. Furthermore, large individual urine sample volumes or sizable target cohorts are to be processed (e.g. for biobanking), the storage capacity is an additional problem. Thus, alternative methods are necessary to overcome such limitations. We have developed a practical vesicle isolation technique to yield easily manageable sample volumes in an exceptionally cost efficient way to facilitate their full utilization in less privileged environments and maximize the benefit of biobanking. Urinary vesicles were isolated by hydrostatic dialysis with minimal interference of soluble proteins or vesicle loss. Large volumes of urine were concentrated up to 1/100 of original volume and the dialysis step allowed equalization of urine physico-chemical characteristics. Vesicle fractions were found suitable to any applications, including RNA analysis. In the yield, our hydrostatic filtration dialysis system outperforms the conventional ultracentrifugation-based methods and the labour intensive and potentially hazardous step of ultracentrifugations are eliminated. Likewise, the need for trained laboratory personnel and heavy initial investment is avoided. Thus, our method qualifies as a method for laboratories working with urinary vesicles and biobanking. PMID:25532487

Towards the feasibility of using ultrasound to determine mechanical properties of tissues in a bioreactor.

PubMed

Mansour, Joseph M; Gu, Di-Win Marine; Chung, Chen-Yuan; Heebner, Joseph; Althans, Jake; Abdalian, Sarah; Schluchter, Mark D; Liu, Yiying; Welter, Jean F

2014-10-01

Our ultimate goal is to non-destructively evaluate mechanical properties of tissue-engineered (TE) cartilage using ultrasound (US). We used agarose gels as surrogates for TE cartilage. Previously, we showed that mechanical properties measured using conventional methods were related to those measured using US, which suggested a way to non-destructively predict mechanical properties of samples with known volume fractions. In this study, we sought to determine whether the mechanical properties of samples, with unknown volume fractions could be predicted by US. Aggregate moduli were calculated for hydrogels as a function of SOS, based on concentration and density using a poroelastic model. The data were used to train a statistical model, which we then used to predict volume fractions and mechanical properties of unknown samples. Young's and storage moduli were measured mechanically. The statistical model generally predicted the Young's moduli in compression to within <10% of their mechanically measured value. We defined positive linear correlations between the aggregate modulus predicted from US and both the storage and Young's moduli determined from mechanical tests. Mechanical properties of hydrogels with unknown volume fractions can be predicted successfully from US measurements. This method has the potential to predict mechanical properties of TE cartilage non-destructively in a bioreactor.

Towards the feasibility of using ultrasound to determine mechanical properties of tissues in a bioreactor

PubMed Central

Mansour, Joseph M.; Gu, Di-Win Marine; Chung, Chen-Yuan; Heebner, Joseph; Althans, Jake; Abdalian, Sarah; Schluchter, Mark D.; Liu, Yiying; Welter, Jean F.

2016-01-01

Introduction Our ultimate goal is to non-destructively evaluate mechanical properties of tissue-engineered (TE) cartilage using ultrasound (US). We used agarose gels as surrogates for TE cartilage. Previously, we showed that mechanical properties measured using conventional methods were related to those measured using US, which suggested a way to non-destructively predict mechanical properties of samples with known volume fractions. In this study, we sought to determine whether the mechanical properties of samples, with unknown volume fractions could be predicted by US. Methods Aggregate moduli were calculated for hydrogels as a function of SOS, based on concentration and density using a poroelastic model. The data were used to train a statistical model, which we then used to predict volume fractions and mechanical properties of unknown samples. Young's and storage moduli were measured mechanically. Results The statistical model generally predicted the Young's moduli in compression to within < 10% of their mechanically measured value. We defined positive linear correlations between the aggregate modulus predicted from US and both the storage and Young's moduli determined from mechanical tests. Conclusions Mechanical properties of hydrogels with unknown volume fractions can be predicted successfully from US measurements. This method has the potential to predict mechanical properties of TE cartilage non-destructively in a bioreactor. PMID:25092421

Helium transfer from water into quartz crystals: A new approach for porewater dating [rapid communication

NASA Astrophysics Data System (ADS)

Tolstikhin, I.; Gannibal, M.; Tarakanov, S.; Pevzner, B.; Lehmann, B.; Ihly, B.; Waber, H. N.

2005-09-01

Several important fundamental and applied problems require a quantification of slow rates of groundwater flow. To resolve these problems helium appears to be a promising tracer. In this contribution we discuss a new approach, which gives the helium inventory in a rock - pore water system by using the relevant mineral record, i.e., without extraction and investigation of the porewater samples. Some U- and Th-poor minerals such as quartz (quartz separates from Permo-Carboniferous Formation, sandstone-shale interlayering, Molasses Basin, Northern Switzerland, hereafter PCF, are used in this study) contain excessive helium having migrated into their internal helium-accessible volume (HAV) from the surrounding porewater [I.N. Tolstikhin, B.E. Lehmann, H.H. Loosli, A. Gautschi, Helium and argon isotopes in rocks, minerals and related groundwaters: a case study in Northern Switzerland, Geochim. Cosmochim. Acta 60 (1996) 1497-1514]. These volumes are estimated by using helium as a nano-size penetrating tool, i.e., by saturation of the minerals with helium under controlled pressure-temperature conditions and subsequent measurements of the helium-saturated concentrations. In the quartz separates HAV/total volume ratios vary from 0.017% to 0.16%; along with the measured initial (unsaturated) He concentration the HAV gives the internal helium pressure, the mean value obtained for 7 samples (25 sample aliquots) is P = 0.45 ± 0.15 atm (1 σ). The product of helium pressure and solubility (7.35 × 10 - 3 cc STP He/cc H 2O for the temperature and salinity of PCF aquifers reported in [F.J. Pearson, W. Balderer, H.H. Loosli, B.E. Lehmann, A. Matter, T. Peters, H. Schmassmann, A. Gautschi, Applied Isotope Hydrogeology-A Case Study in Northern Switzerland, Elsevier Amsterdam, 1991, 439 pp.]) is the mineral-derived He concentration in the respective porewater, CPW = 0.0035 ± 0.0017 cc He/cc H 2O. This value is in full accord with measured He concentrations in PCF aquifers, CPCF, varying from 0.0045 to 0.0016 cc He/cc H 2O. This agreement validates the proposed approach and also shows that the mineral-porewater helium-concentration equilibrium has been established. Indeed, estimates of the He-migration rates through our quartz samples show that in ˜6000 years the internal pressure should equilibrate with He-concentration in related porewater of PCF, and this time interval is short compared to independent estimates [I.N. Tolstikhin, B.E. Lehmann, H.H. Loosli, A. Gautschi, Helium and argon isotopes in rocks, minerals and related groundwaters: a case study in Northern Switzerland, Geochim. Cosmochim. Acta 60 (1996) 1497-1514]. The helium inventory in the rock-porewater assemblage shows that helium abundance in pore waters is indeed important. In shale samples (with ˜15% porosity) porewaters contain more helium than the host minerals altogether. Porewater helium-concentration profiles, available from the mineral record, along with helium production rates are input parameters allowing model(s) of helium migration through a hydrological structure to be developed. Quite high helium concentrations in PCF porewaters imply slow removal mechanisms, which will be discussed elsewhere.

Water quality and bathymetry of Sand Lake, Anchorage, Alaska

USGS Publications Warehouse

Donaldson, Donald E.

1976-01-01

Sand Lake, a dimictic lowland lake in Anchorage, Alaska, has recently become as urban lake. Analyses indicate that the lake is oligotrophic, having low dissolved solids and nutrient concentrations. Snowmelt runoff from an adjacent residential area, however, has a dissolved-solids concentration 10 times that of the main body of Sand Lake. Lead concentrations in the runoff exceed known values from other water in the ANchorage area, including water samples taken beneath landfills. The volume of the snowmelt runoff has not been measured. The data presented can be used as a baseline for water-resource management. (Woodard-USGS)

Pilot study on feasibility of application of gas chromatography for the assessment of acrylamide concentration in sewage sludge.

PubMed

Włodarczyk, Elżbieta; Próba, Marta; Wolny, Lidia; Wojtal, Łukasz

2014-01-01

The aim of this study was to determine the possibility of using gas chromatography to measurement of the acrylamide concentration in sewage sludge. Acrylamide, as a toxic substance, is not indifferent to human health, but it is used in the production of plastics, dyes, adhesives, cosmetics, mortar, as well as a coagulant for water treatment, wastewater or sewage sludge conditioning. Determination of acrylamide by gas chromatography was based on standard: EPA Method 8032A "Acrylamid by gas chromatography." It consists of a bromination reaction of the compound in the presence of dibromopropendial derivative, a triple extraction with the ethyl acetate, a concentration of the eluate sample up to the 1 ml volume, and an analysis by the gas chromatography using an electron capture detector (ECD). The acrylamide concentration of was calculated according to the formula presented in the mentioned standard. All samples were performed twice (the difference between the results was not greater than 10%), and the average value of the four samples was 17.64 µg/L(-1). The presence of acrylamide in sewage sludge has been confirmed.

Ion beam promoted lithium absorption in glassy polymeric carbon

NASA Astrophysics Data System (ADS)

Zimmerman, R. L.; Ila, D.; Jenkins, G. M.; Maleki, H.; Poker, D. B.

1995-12-01

Glassy Polymeric Carbon (GPC) samples prepared from a precursor possess accessible pore volume that depends on the heat treatment temperature [G.M. Jenkins and K. Kawamura, Polymeric Carbons - Carbon Fiber, Glass and Char (Cambridge University Press, Cambridge, 1976) p. 140]. We have shown that lithium percolates without diffusion into the accessible pores of GPC samples immersed in a molten lithium salt bath at 700°C [D. Ila, G.M. Jenkins, L.R. Holland, A.L. Evelyn and H. Jena, Vacuum 45 (1994) 451]. Ion bombardment with 10 MeV Au atoms increases the total pore volume available for lithium occupation even for samples normally impermeable to lithium. The lithium concentration depth profile is measured using Li 7(p,2α) nuclear reaction analysis. We will report on lithium percolation into GPC prepared at temperatures between 500°C and 1000°C and activated by a 10 MeV gold ion bombardment.

Determination of low (137)Cs concentration in seawater using ammonium 12-molybdophosphate adsorption and chemical separation method.

PubMed

Park, J H; Chang, B U; Kim, Y J; Seo, J S; Choi, S W; Yun, J Y

2008-12-01

A new method has been developed for analyzing (137)Cs in a small volume of seawater. Ammonium 12-molybdophosphate (AMP) was used two times during pretreatment procedure. The first step was to adsorb (137)Cs in seawater samples into AMP in order to reduce sample volume, and the second was to remove (87)Rb, interference nuclide for beta counting. The AMP adsorbing (137)Cs was dissolved by sodium hydroxide solution, and then (137)Cs was finally formed to be cesium chloroplatinate precipitate by adding 10% hexachloroplatinic acid. The beta rays emitted from (137)Cs were measured with a low background gas-proportional alpha/beta counter. This method was applied to several seawater samples taken in the East Sea of Korea. Compared to the routinely used gamma-spectrometry method, this new AMP method was reliable and suitable for analyzing (137)Cs in deep seawater.

Temporal trends of bulk precipitation and stream water chemistry (1977-1997) in a small forested area, Krusne hory, northern Bohemia, Czech Republic

USGS Publications Warehouse

Peters, N.E.; Cerny, J.; Havel, M.; Krejci, R.

1999-01-01

The Krusne hory (Erzgebirge or Ore Mountains) has been heavily affected by high atmospheric pollutant deposition caused by fossil fuel combustion in an adjacent Tertiary coal basin. Long-term routine sampling of bulk precipitation (1977-1996) and stream water (1977-1998) in a forested area on the south-eastern slope of the mountains were used to evaluate trends and patterns in solute concentration and flux with respect to controlling processes. From 1977 to 1996, the annual volume-weighted Ca2+ and SO42- concentrations decreased in bulk precipitation. However, after 1989, when a pronounced and continuous decrease occurred in coal production, annual volume-weighted concentrations decreased for most solutes, except H+. The concentration decreases were marked, with 1996 levels at or below 50% of those in 1989. The lack of a trend in H+ is attributed to similar decreases in both acid anions and neutralizing base cations. Stream water concentrations of most solutes, i.e. H+, Ca2+, Mg2+, SO42- and NO3-, were highest at the onset of sampling in 1977, decreased markedly from 1977 to 1983 and decreased more gradually from 1983 to 1998. The spruce forest die-back and removal reduced dry deposition of these solutes by reducing the filtering action, which was provided by the forest canopy. A notable decrease in stream water Ca2+ concentrations occurred after 1995 and may be due to the depletion of Ca2+, which was provided by catchment liming in 1986, 1988 and 1989. Solute flux trends in bulk atmospheric deposition and stream water generally were not significant and the lack of trend is attributed to the large interannual variability in precipitation quantity and runoff, respectively. All solutes except Na+ varied seasonally. The average seasonal concentrations varied between the solutes, but for most solutes were highest in winter and spring and lowest in summer, correlating with the seasonal trend and runoff. For Ca2+, Mg2+ and SO42-, the concentration minimum occurs in September and the maximum occurs in February or March, correlating with the seasonal baseflow. These solutes are primarily controlled by the contribution of soil water and groundwater to stream flow. During snowmelt, the meltwater generally causes concentrations to decrease as soil water and groundwater are diluted. For NO3, average minimum concentrations occur in August at the end of the growing season concurrent with the lowest stream flow, and the maximum occurs in February and March with high stream flow during snowmelt. Seasonal stream water NO3- concentration variations are large compared with the long-term decrease.The Krusne hory (Erzgebirge or Ore Mountains) has been heavily affected by high atmospheric pollutant deposition caused by fossil fuel combustion in an adjacent Tertiary coal basin. Long-term routine sampling of bulk precipitation (1977-1996) and stream water (1977-1998) in a forested area on the south-eastern slope of the mountains were used to evaluate trends and patterns in solute concentration and flux with respect to controlling processes. From 1977 to 1996, the annual volume-weighted Ca2+ and SO42- concentrations decreased in bulk precipitation. However, after 1989, when a pronounced and continuous decrease occurred in coal production, annual volume-weighted concentrations decreased for most solutes, except H+. The concentration decreases were marked, with 1996 levels at or below 50% of those in 1989. The lack of a trend in H+ is attributed to similar decreases in both acid anions and neutralizing base cations. Stream water concentrations of most solutes, i.e. H+, Ca2+, Mg2+, SO42- and NO3-, were highest at the onset of sampling in 1977, decreased markedly from 1977 to 1983 and decreased more gradually from 1983 to 1998. The spruce forest die-back and removal reduced dry deposition of these solutes by reducing the filtering action, which was provided by the forest canopy. A notable decrease in stream water Ca2+ concentrations occurred after 1995 an

Use of Enterococcus faecalis and Bacillus atrophaeus as surrogates to establish and maintain laboratory proficiency for concentration of water samples using ultrafiltration.

PubMed

Mapp, Latisha; Klonicki, Patricia; Takundwa, Prisca; Hill, Vincent R; Schneeberger, Chandra; Knee, Jackie; Raynor, Malik; Hwang, Nina; Chambers, Yildiz; Miller, Kenneth; Pope, Misty

2015-11-01

The U.S. Environmental Protection Agency's (EPA) Water Laboratory Alliance (WLA) currently uses ultrafiltration (UF) for concentration of biosafety level 3 (BSL-3) agents from large volumes (up to 100-L) of drinking water prior to analysis. Most UF procedures require comprehensive training and practice to achieve and maintain proficiency. As a result, there was a critical need to develop quality control (QC) criteria. Because select agents are difficult to work with and pose a significant safety hazard, QC criteria were developed using surrogates, including Enterococcus faecalis and Bacillus atrophaeus. This article presents the results from the QC criteria development study and results from a subsequent demonstration exercise in which E. faecalis was used to evaluate proficiency using UF to concentrate large volume drinking water samples. Based on preliminary testing EPA Method 1600 and Standard Methods 9218, for E. faecalis and B. atrophaeus respectively, were selected for use during the QC criteria development study. The QC criteria established for Method 1600 were used to assess laboratory performance during the demonstration exercise. Based on the results of the QC criteria study E. faecalis and B. atrophaeus can be used effectively to demonstrate and maintain proficiency using ultrafiltration. Published by Elsevier B.V.

Hanford atmospheric dispersion data: 1960 through June 1967

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nickola, P.W.; Ramsdell, J.V.; Glantz, C.S.

1983-11-01

This volume presents dispersion and supporting meteorological data from experiments conducted over relatively flat terrain at Hanford, Washington from January 1960 through June 1967. The nature of the experiments, the sampling grids, and the tracer techniques used are described in the narrative portion of the document. Appendices contain the time-integrated concentrations for samplers within the plumes, summaries of the concentration distributions across the plumes, and wind and temperature profile data for each release period. 18 references, 7 figures, 3 tables.

Sediment quantity and quality in three impoundments in Massachusetts

USGS Publications Warehouse

Zimmerman, Marc James; Breault, Robert F.

2003-01-01

As part of a study with an overriding goal of providing information that would assist State and Federal agencies in developing screening protocols for managing sediments impounded behind dams that are potential candidates for removal, the U.S Geological Survey determined sediment quantity and quality at three locations: one on the French River and two on Yokum Brook, a tributary to the west branch of the Westfield River. Data collected with a global positioning system, a geographic information system, and sediment-thickness data aided in the creation of sediment maps and the calculation of sediment volumes at Perryville Pond on the French River in Webster, Massachusetts, and at the Silk Mill and Ballou Dams on Yokum Brook in Becket, Massachusetts. From these data the following sediment volumes were determined: Perryville Pond, 71,000 cubic yards, Silk Mill, 1,600 cubic yards, and Ballou, 800 cubic yards. Sediment characteristics were assessed in terms of grain size and concentrations of potentially hazardous organic compounds and metals. Assessment of the approaches and methods used at study sites indicated that ground-penetrating radar produced data that were extremely difficult and time-consuming to interpret for the three study sites. Because of these difficulties, a steel probe was ultimately used to determine sediment depth and extent for inclusion in the sediment maps. Use of these methods showed that, where sampling sites were accessible, a machine-driven coring device would be preferable to the physically exhausting, manual sediment-coring methods used in this investigation. Enzyme-linked immunosorbent assays were an effective tool for screening large numbers of samples for a range of organic contaminant compounds. An example calculation of the number of samples needed to characterize mean concentrations of contaminants indicated that the number of samples collected for most analytes was adequate; however, additional analyses for lead, copper, silver, arsenic, total petroleum hydrocarbons, and chlordane are needed to meet the criteria determined from the calculations. Particle-size analysis did not reveal a clear spatial distribution pattern at Perryville Pond. On average, less than 65 percent of each sample was greater in size than very fine sand. The sample with the highest percentage of clay-sized particles (24.3 percent) was collected just upstream from the dam and generally had the highest concentrations of contaminants determined here. In contrast, more than 90 percent of the sediment samples in the Becket impoundments had grain sizes larger than very fine sand; as determined by direct observation, rocks, cobbles, and boulders constituted a substantial amount of the material impounded at Becket. In general, the highest percentages of the finest particles, clays, occurred in association with the highest concentrations of contaminants. Enzyme-linked immunosorbent assays of the Perryville samples showed the widespread presence of petroleum hydrocarbons (16 out of 26 samples), polycyclic aromatic hydrocarbons (23 out of 26 samples), and chlordane (18 out of 26 samples); polychlorinated biphenyls were detected in five samples from four locations. Neither petroleum hydrocarbons nor polychlorinated biphenyls were detected at Becket, and chlordane was detected in only one sample. All 14 Becket samples contained polycyclic aromatic hydrocarbons. Replicate quality-control analyses revealed consistent results between paired samples. Samples from throughout Perryville Pond contained a number of metals at potentially toxic concentrations. These metals included arsenic, cadmium, copper, lead, nickel, and zinc. At Becket, no metals were found in elevated concentrations. In general, most of the concentrations of organic compounds and metals detected in Perryville Pond exceeded standards for benthic organisms, but only rarely exceeded standards for human contact. The most highly contaminated samples were

Changes in plasma thrombospondin-1 concentrations following acute intracerebral hemorrhage.

PubMed

Dong, Xiao-Qiao; Yu, Wen-Hua; Zhu, Qiang; Cheng, Zhen-Yu; Chen, Yi-Hua; Lin, Xiao-Feng; Ten, Xian-Lin; Tang, Xiao-Bing; Chen, Juan

2015-10-23

Angiogenesis is a fundamental process for brain development and repair. Thrombospondin-1 is the first identified endogenous angiogenesis inhibitor. Its expression in rat brain is upregulated after intracerebral hemorrhage (ICH). We determined whether plasma thrombospondin-1 concentrations are associated with injury severity and prognosis in ICH patients. This observational, prospective study recruited 110 patients and 110 age- and gender-matched healthy controls. Blood samples were collected from the patients at admission and from the healthy controls at study entry to measure plasma thrombospondin-1 concentrations. The endpoints included 1-week mortality, 6-month mortality, 6-month overall survival and 6-month unfavorable outcome (modified Rankin Scale score >2). Plasma thrombospondin-1 concentrations were markedly higher in patients than in healthy controls. Thrombospondin-1 was an independent predictive factor for all endpoints and plasma thrombospondin-1 concentrations were highly associated with injury severity reflected by hematoma volume and National Institutes of Health Stroke Scale score. Under receiver operating characteristic curves, plasma thrombospondin-1 concentrations had similar predictive values compared with hematoma volume and National Institutes of Health Stroke Scale score. Increased plasma thrombospondin-1 concentrations following ICH are independently associated with injury severity and short-term and long-term clinical outcomes. Copyright © 2015 Elsevier B.V. All rights reserved.

Effect of evaporation and pasteurization in the biochemical and immunological composition of human milk.

PubMed

Braga, Lucylea P M; Palhares, Durval B

2007-01-01

To assess the effects of evaporation and pasteurization of human milk on its biochemical and immunological composition and on its osmolarity. The samples of mature human milk were categorized into four study groups: in natura human milk, pasteurized human milk, human milk evaporated at 70% of the baseline volume and human milk pasteurized and evaporated at 70%, with 12 different samples of milk in each group. The samples were used to determine the concentrations of sodium, potassium, calcium, phosphorus, magnesium, protein, fat, lactose, immunoglobulin A and osmolarity. The pasteurization of human milk did not show statistically significant changes in the concentration of sodium, potassium, calcium, phosphorus, magnesium, protein, fat, lactose, or in osmolarity; however, it showed remarkable reduction in the mean concentration of immunoglobulin A. Evaporation had a mean increase of 38% in the concentration of sodium, potassium, calcium, phosphorus, magnesium, protein, fat and lactose and mean reduction of 45% in the concentration of immunoglobulin A, without significant change in osmolarity in unprocessed milk. By evaporation at 70% of the baseline value of human milk, it is possible to obtain human milk that meets the nutritional requirements recommended for preterm infants, except for calcium and phosphorus.

The role of gray and white matter segmentation in quantitative proton MR spectroscopic imaging.

PubMed

Tal, Assaf; Kirov, Ivan I; Grossman, Robert I; Gonen, Oded

2012-12-01

Since the brain's gray matter (GM) and white matter (WM) metabolite concentrations differ, their partial volumes can vary the voxel's ¹H MR spectroscopy (¹H-MRS) signal, reducing sensitivity to changes. While single-voxel ¹H-MRS cannot differentiate between WM and GM signals, partial volume correction is feasible by MR spectroscopic imaging (MRSI) using segmentation of the MRI acquired for VOI placement. To determine the magnitude of this effect on metabolic quantification, we segmented a 1-mm³ resolution MRI into GM, WM and CSF masks that were co-registered with the MRSI grid to yield their partial volumes in approximately every 1 cm³ spectroscopic voxel. Each voxel then provided one equation with two unknowns: its i- metabolite's GM and WM concentrations C(i) (GM) , C(i) (WM) . With the voxels' GM and WM volumes as independent coefficients, the over-determined system of equations was solved for the global averaged C(i) (GM) and C(i) (WM) . Trading off local concentration differences offers three advantages: (i) higher sensitivity due to combined data from many voxels; (ii) improved specificity to WM versus GM changes; and (iii) reduced susceptibility to partial volume effects. These improvements made no additional demands on the protocol, measurement time or hardware. Applying this approach to 18 volunteered 3D MRSI sets of 480 voxels each yielded N-acetylaspartate, creatine, choline and myo-inositol C(i) (GM) concentrations of 8.5 ± 0.7, 6.9 ± 0.6, 1.2 ± 0.2, 5.3 ± 0.6 mM, respectively, and C(i) (WM) concentrations of 7.7 ± 0.6, 4.9 ± 0.5, 1.4 ± 0.1 and 4.4 ± 0.6mM, respectively. We showed that unaccounted voxel WM or GM partial volume can vary absolute quantification by 5-10% (more for ratios), which can often double the sample size required to establish statistical significance. Copyright © 2012 John Wiley & Sons, Ltd.

Comprehensive Monitoring Program: Final Biota Annual Report for 1989. Volume 2

DTIC Science & Technology

1990-06-01

samples from RMA lakes were highest in largemouth bass, a top predator . Largemouth bass and bluegill exhibited the widest geographic distribution...certification. BCtL = Siss examined with endrin concentrations below lower certified reporting limit of 0.0740 pg/g (MRI) or 0 036 pf (ESE) for aimal tipte and

Proceedings of the Antenna Applications Symposium (32nd) Held in Monticello, Illinois on 16-18 September 2008. Volume 1

DTIC Science & Technology

2008-12-20

Equation 6 for the sample likelihood function gives a “concentrated likelihood function,” which depends on correlation parameters θh and ph. This...step one and estimates correlation parameters using the new data set including all previous sample points and the new data point x. The algorithm...Unclassified b. ABSTRACT Unclassified c. THIS PAGE Unclassified UU 279 19b. TELEPHONE NUMBER (include area code ) N/A

Application of a surfactant-assisted dispersive liquid-liquid microextraction method along with central composite design for micro-volume based spectrophotometric determination of low level of Cr(VI) ions in aquatic samples.

PubMed

Sobhi, Hamid Reza; Azadikhah, Efat; Behbahani, Mohammad; Esrafili, Ali; Ghambarian, Mahnaz

2018-05-09

A fast, simple, low cost surfactant-assisted dispersive liquid-liquid microextraction method along with central composite design for the determination of low level of Cr(VI) ions in several aquatic samples has been developed. Initially, Cr(VI) ions present in the aqueous sample were readily reacted with 1,5‑diphenylcarbazide (DPC) in acidic medium through complexation. Sodium dodecyl sulfate (SDS), as an anionic surfactant, was then employed as an ion-pair agent to convert the cationic complex into the neutral one. Following on, the whole aqueous phase underwent a dispersive liquid-liquid microextraction (DLLME) leading to the transfer of the neutral complex into the fine droplet of organic extraction phase. A micro-volume spectrophotometer was used to determine Cr(VI) concentrations. Under the optimized conditions predicted by the statistical design, the limit of quantification (LOQ) obtained was reported to be 5.0 μg/L, and the calibration curve was linear over the concentration range of 5-100 μg/L. Finally, the method was successfully implemented for the determination of low levels of Cr(VI) ions in various real aquatic samples and the accuracies fell within the range of 83-102%, while the precision varied in the span of 1.7-5.2%. Copyright © 2018. Published by Elsevier B.V.

Determination of nickel in water, food, and biological samples by electrothermal atomic absorption spectrometry after preconcentration on modified carbon nanotubes.

PubMed

Taher, Mohammad Ali; Mazaheri, Lida; Ashkenani, Hamid; Mohadesi, Alireza; Afzali, Daryoush

2014-01-01

A new and sensitive SPE method using modified carbon nanotubes for extraction and preconcentration, and electrothermal atomic absorption spectrometric determination of nickel (Ni) in real samples at ng/L levels was investigated. First, multiwalled carbon nanotubes were oxidized with concentrated HNO3, then modified with 2-(5-bormo-2-pyridylazo)-5-diethylaminophenol reagent. The adsorption was achieved quantitatively on a modified carbon nanotubes column in a pH range of 6.5 to 8.5; the adsorbed Ni(II) ions were then desorbed by passing 5.0 mL of 1 M HNO3. The effects of analytical parameters, including pH of the solution, eluent type and volume, sample volume, flow rate of the eluent, and matrix ions, were investigated for optimization of the presented procedure. The enrichment factor was 180, and the LOD for Ni was 4.9 ng/L. The method was applied to the determination of Ni in water, food, and biological samples, and reproducible results were obtained.

Ultrasensitive Detection of Shigella Species in Blood and Stool.

PubMed

Luo, Jieling; Wang, Jiapeng; Mathew, Anup S; Yau, Siu-Tung

2016-02-16

A modified immunosensing system with voltage-controlled signal amplification was used to detect Shigella in stool and blood matrixes at the single-digit CFU level. Inactivated Shigella was spiked in these matrixes and detected directly. The detection was completed in 78 min. Detection limits of 21 CFU/mL and 18 CFU/mL were achieved in stool and blood, respectively, corresponding to 2-7 CFUs immobilized on the detecting electrode. The outcome of the detection of extremely low bacterium concentration, i.e., below 100 CFU/mL, blood samples show a random nature. An analysis of the detection probabilities indicates the correlation between the sample volume and the success of detection and suggests that sample volume is critical for ultrasensitive detection of bacteria. The calculated detection limit is qualitatively in agreement with the empirically determined detection limit. The demonstrated ultrasensitive detection of Shigella on the single-digit CFU level suggests the feasibility of the direct detection of the bacterium in the samples without performing a culture.

Characteristics of produced water discharged to the Gulf of Mexico hypoxiczone.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Veil, J. A.; Kimmell, T. A.; Rechner, A. C.

2005-08-24

Each summer, an area of low dissolved oxygen (the hypoxic zone) forms in the shallow nearshore Gulf of Mexico waters from the Mississippi River Delta westward to near the Texas/Louisiana border. Most scientists believe that the leading contributor to the hypoxic zone is input of nutrients (primarily nitrogen and phosphorus compounds) from the Mississippi and Atchafalaya Rivers. The nutrients stimulate growth of phytoplankton. As the phytoplankton subsequently die, they fall to the bottom waters where they are decomposed by microorganisms. The decomposition process consumes oxygen in the bottom waters to create hypoxic conditions. Sources other than the two rivers mentionedmore » above may also contribute significant quantities of oxygen-demanding pollutants. One very visible potential source is the hundreds of offshore oil and gas platforms located within or near the hypoxic zone. Many of these platforms discharge varying volumes of produced water. However, only limited data characterizing oxygen demand and nutrient concentration and loading from offshore produced water discharges have been collected. No comprehensive and coordinated oxygen demand data exist for produced water discharges in the Gulf of Mexico. This report describes the results of a program to sample 50 offshore oil and gas platforms located within the Gulf of Mexico hypoxic zone. The program was conducted in response to a requirement in the U.S. Environmental Protection Agency (EPA) general National Pollutant Discharge Elimination System (NPDES) permit for offshore oil and gas discharges. EPA requested information on the amount of oxygen-demanding substances contained in the produced water discharges. This information is needed as inputs to several water quality models that EPA intends to run to estimate the relative contributions of the produced water discharges to the occurrence of the hypoxic zone. Sixteen platforms were sampled 3 times each at approximately one-month intervals to give an estimate of temporal variability. An additional 34 platforms were sampled one time. The 50 sampled platforms were scattered throughout the hypoxic zone to give an estimate of spatial variability. Each platform was sampled for biochemical oxygen demand (BOD), total organic carbon (TOC), nitrogen (ammonia, nitrate, nitrite, and total Kjeldahl nitrogen [TKN]), and phosphorus (total phosphorus and orthophosphate). In addition to these parameters, each sample was monitored for pH, conductivity, salinity, and temperature. The sampling provided average platform concentrations for each parameter. Table ES-1 shows the mean, median, maximum, and minimum for the sampled parameters. For some of the parameters, the mean is considerably larger than the median, suggesting that one or a few data points are much higher than the rest of the points (outliers). Chapter 4 contains an extensive discussion of outliers and shows how the sample results change if outliers are deleted from consideration. A primary goal of this study is to estimate the mass loading (lb/day) of each of the oxygen-demanding pollutants from the 50 platforms sampled in the study. Loading is calculated by multiplying concentrations by the discharge volume and then by a conversion factor to allow units to match. The loadings calculated in this study of 50 platforms represent a produced water discharge volume of about 176,000 bbl/day. The total amount of produced water generated in the hypoxic zone during the year 2003 was estimated as 508,000 bbl/day. This volume is based on reports by operators to the Minerals Management Service each year. It reflects the volume of produced water that is generated from each lease, not the volume that is discharged from each platform. The mass loadings from offshore oil and gas discharges to the entire hypoxic zone were estimated by multiplying the 50-platform loadings by the ratio of total water generated to 50-platform discharge volume. The loadings estimated for the 50 platforms and for the entire hypoxic zone are shown in Table ES-2. These estimates and the sampling data from 50 platforms represent the most complete and comprehensive effort ever undertaken to characterize the amount and potential sources of the oxygen demand in offshore oil and gas produced water discharges.« less

Solid phase extraction of trace amounts of Ag, Cd, Cu, and Zn in environmental samples using magnetic nanoparticles coated by 3-(trimethoxysilyl)-1-propantiol and modified with 2-amino-5-mercapto-1,3,4-thiadiazole and their determination by ICP-OES.

PubMed

Mashhadizadeh, Mohammad Hossein; Karami, Zahra

2011-06-15

A fast, sensitive, and simple method using magnetic nanoparticles (MNPs) coated by 3-(trimethoxysilyl)-1-propantiol and modified with 2-amino-5-mercapto-1,3,4-thiadiazole, as an adsorbent has been successfully developed for extraction, preconcentration, and determination of trace amounts of Ag, Cd, Cu, and Zn from environmental samples. The prepared nanoparticles were characterized by Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). These magnetic nanoparticles can be easily dispersed in aqueous samples and retrieved by the application of external magnetic field via a piece of permanent magnet. The main factors affecting the extraction efficiency such as pH value, sample volume, eluent concentration and volume, ultrasonication time, and coexisting ions have been investigated and established. Under the optimal conditions, high concentration factors (194, 190, 170, and 182) were achieved for Ag, Cd, Cu, and Zn with relative standard deviations of 5.31%, 4.03%, 3.62%, and 4.20%, respectively. The limits of detection for Ag, Cd, Cu, and Zn were as low as 0.12, 0.12, 0.13 and 0.11 ng mL(-1). The prepared sorbent was applied for preconcentration of trace amounts of Ag, Cd, Cu, and Zn in the various water samples with satisfactory results. Copyright © 2011 Elsevier B.V. All rights reserved.

[Evaluation of measurement uncertainty of welding fume in welding workplace of a shipyard].

PubMed

Ren, Jie; Wang, Yanrang

2015-12-01

To evaluate the measurement uncertainty of welding fume in the air of the welding workplace of a shipyard, and to provide quality assurance for measurement. According to GBZ/T 192.1-2007 "Determination of dust in the air of workplace-Part 1: Total dust concentration" and JJF 1059-1999 "Evaluation and expression of measurement uncertainty", the uncertainty for determination of welding fume was evaluated and the measurement results were completely described. The concentration of welding fume was 3.3 mg/m(3), and the expanded uncertainty was 0.24 mg/m(3). The repeatability for determination of dust concentration introduced an uncertainty of 1.9%, the measurement using electronic balance introduced a standard uncertainty of 0.3%, and the measurement of sample quality introduced a standard uncertainty of 3.2%. During the determination of welding fume, the standard uncertainty introduced by the measurement of sample quality is the dominant uncertainty. In the process of sampling and measurement, quality control should be focused on the collection efficiency of dust, air humidity, sample volume, and measuring instruments.

Effect on the structural, DC resistivity and magnetic properties of Zr and Cu co-SubstitutedNi0.5Zn0.5Fe2O4using sol-gel auto-combustion method

NASA Astrophysics Data System (ADS)

Jalaiah, K.; Vijaya Babu, K.; Chandra mouli, K.; Subba Rao, P. S. V.

2018-04-01

The Zr and Cu co-substituted Ni0.5Zn0.5Fe2O4 ferrite nanoparticles have been synthesized by the sol-gel auto combustion method. The XRD patterns confirmed single phase cubic spinel structure for present ferrite systems. The substitution of co-dopants in the spinel structure initially decreases the lattice parameter from x = 0.00 to 0.08 and thereafter increases and the same tendency reflecting in cell volume. The DC resistivity was initially increased later followed the decreasing trend; however the drift mobility of all ferrite samples appears to be in opposite phenomenon to DC resistivity. The saturation magnetization and net magnetic moments of all ferrite samples are decreasing with increasing dopant concentration. The coercive field and Y-K angles are increased with dopant concentration. The initial permeability of all samples is decreased with increasing dopant concentration. The Q-Factor for all samples shows the narrow frequency band with increasing frequency.

Air quality during demolition and recovery activities in post-Katrina New Orleans.

PubMed

Ravikrishna, Raghunathan; Lee, Han-Woong; Mbuligwe, Stephen; Valsaraj, K T; Pardue, John H

2010-07-01

Air samples were collected during demolition and cleanup operations in the Lakeview district of New Orleans, Louisiana, USA, in late 2005 during the period immediately after Hurricane Katrina. Three different high-volume air samples were collected around waste collection areas that were created to temporarily hold the debris from the cleanup of residential properties in the area. Particulate concentrations were elevated and included crystalline fibers associated with asbestos. Metal concentrations on particulate matter resembled those measured in sediments deposited by floodwaters with the exception of Ba, which was elevated at all three locations. The highest organic contaminant concentration measured on particulates was the pesticide Ziram (Zinc, bis[diethylcarbamodithioato-S,S']-, [T-4]-) at 2,200 microg/g of particulate matter during sampling period 2. Ziram is used in latex paint, adhesives, caulking, and wallboard as a preservative. Fungal isolates developed from particulate air samples included species associated with disease including Aspergillus and Penicillium species. These data represent the most comprehensive assessment of demolition activities during the period immediately after Hurricane Katrina. Copyright (c) 2010 SETAC.

Airborne concentrations of benzene for dock workers at the ExxonMobil refinery and chemical plant, Baton Rouge, Louisiana, USA (1977-2005).

PubMed

Widner, Thomas E; Gaffney, Shannon H; Panko, Julie M; Unice, Kenneth M; Burns, Amanda M; Kreider, Marisa; Marshall, J Ralph; Booher, Lindsay E; Gelat, Richard H; Paustenbach, Dennis J

2011-03-01

Benzene is a natural constituent of crude oil and natural gas (0.1-3.0% by volume). Materials that are refined from crude oil and natural gas contain some residual benzene. Few datasets have appeared in the peer-reviewed literature characterizing exposures to benzene at specific refineries or during specific tasks. In this study, historical samples of airborne benzene collected from 1977-2005 at the ExxonMobil Baton Rouge, Louisiana, USA, docks were evaluated. Workers were categorized into 11 job titles, and both non-task (≤180 min sample duration) and task-related (<180 min) benzene concentrations were assessed. Approximately 800 personal air samples (406 non-task and 397 task-related) were analyzed. Non-task samples showed that concentrations varied significantly across job titles and generally resulted from exposures during short-duration tasks such as tank sampling. The contractor - tankerman job title had the highest average concentration [N=38, mean 1.4 parts per million (ppm), standard deviation (SD) 2.6]. Task-related samples indicated that the highest exposures were associated with the disconnection of cargo loading hoses (N=134, mean 11 ppm, SD 32). Non-task samples for specific job categories showed that concentrations have decreased over the past 30 years. Recognizing the potential for benzene exposure, this facility has required workers to use respiratory protective equipment during selected tasks and activities; thus, the concentrations measured were likely greater than those that the employee actually experienced. This study provides a job title- and task-focused analysis of occupational exposure to benzene during dock facility operations that is insightful for understanding the Baton Rouge facility and others similar to it over the past 30 years.

Rapid Microbial Sample Preparation from Blood Using a Novel Concentration Device

PubMed Central

Boardman, Anna K.; Campbell, Jennifer; Wirz, Holger; Sharon, Andre; Sauer-Budge, Alexis F.

2015-01-01

Appropriate care for bacteremic patients is dictated by the amount of time needed for an accurate diagnosis. However, the concentration of microbes in the blood is extremely low in these patients (1–100 CFU/mL), traditionally requiring growth (blood culture) or amplification (e.g., PCR) for detection. Current culture-based methods can take a minimum of two days, while faster methods like PCR require a sample free of inhibitors (i.e., blood components). Though commercial kits exist for the removal of blood from these samples, they typically capture only DNA, thereby necessitating the use of blood culture for antimicrobial testing. Here, we report a novel, scaled-up sample preparation protocol carried out in a new microbial concentration device. The process can efficiently lyse 10 mL of bacteremic blood while maintaining the microorganisms’ viability, giving a 30‑μL final output volume. A suite of six microorganisms (Staphylococcus aureus, Streptococcus pneumoniae, Escherichia coli, Haemophilus influenzae, Pseudomonas aeruginosa, and Candida albicans) at a range of clinically relevant concentrations was tested. All of the microorganisms had recoveries greater than 55% at the highest tested concentration of 100 CFU/mL, with three of them having over 70% recovery. At the lowest tested concentration of 3 CFU/mL, two microorganisms had recoveries of ca. 40–50% while the other four gave recoveries greater than 70%. Using a Taqman assay for methicillin-sensitive S. aureus (MSSA)to prove the feasibility of downstream analysis, we show that our microbial pellets are clean enough for PCR amplification. PCR testing of 56 spiked-positive and negative samples gave a specificity of 0.97 and a sensitivity of 0.96, showing that our sample preparation protocol holds great promise for the rapid diagnosis of bacteremia directly from a primary sample. PMID:25675242

Newborn screening blood spot analysis in the UK: influence of spot size, punch location and haematocrit.

PubMed

Lawson, A J; Bernstone, L; Hall, S K

2016-03-01

In dried blood spot analysis, punch location and variations in applied sample volume and haematocrit can produce different measured concentrations of analytes. We investigated the magnitude of these effects in newborn screening in the UK. Heparinized blood spiked with thyroid stimulating hormone (TSH), phenylalanine, tyrosine, leucine, methionine, octanoyl carnitine (C8), and immunoreactive trypsinogen (IRT) was spotted onto filter paper: (i) at a constant haematocrit of 50% at various volumes, and (ii) at a range of haematocrits using a constant volume. Subpunches (3.2 mm) of the dried blood spots were then analysed. Compared with a central punch from a 50 µL blood spot with 50% haematocrit, 10 µL spots can have significantly lower measured concentrations of all analytes, with decreases of 15% or more observed for leucine, methionine, phenylalanine, and tyrosine. Punching at the edge of a spot can increase measured concentrations up to 35%. Higher haematocrit decreased measured TSH and C8 yet increased amino acids and IRT by 15% compared with 50% haematocrit. Lower haematocrits had the opposite effect, but only with higher concentrations of some analytes. Differences in blood spot size, haematocrit and punch location substantially affect measured concentrations for analytes used in the UK newborn screening programme, and this could affect false positive and negative rates. To minimize analytical bias, these variables should be controlled or adjusted for where possible. © The Author(s) 2015.

Signal Enhancement in HPLC/Micro-Coil NMR Using Automated Column Trapping

PubMed Central

Djukovic, Danijel; Liu, Shuhui; Henry, Ian; Tobias, Brian; Raftery, Daniel

2008-01-01

A new HPLC-NMR system is described that performs analytical separation, pre-concentration, and NMR spectroscopy in rapid succession. The central component of our method is the online pre-concentration sequence that improves the match between post-column analyte peak volume and the micro-coil NMR detection volume. Separated samples are collected on to a C18 guard column with a mobile phase composed of 90% D2O/10% acetonitrile-D3, and back-flashed to the NMR micro-coil probe with 90% acetonitrile-D3/10% D2O. In order to assess the performance of our unit, we separated a standard mixture of 1 mM ibuprofen, naproxen, and phenylbutazone using a commercially available C18 analytical column. The S/N measurements from the NMR acquisitions indicated that we achieved signal enhancement factors up to 10.4 (±1.2)-fold. Furthermore, we observed that pre-concentration factors increased as the injected amount of analyte decreased. The highest concentration enrichment of 14.7 (±2.2)-fold was attained injecting 100 μL solution of 0.2 mM (~4 μg) ibuprofen. PMID:17037915

Assessing Amide Proton Transfer (APT) MRI Contrast Origins in 9 L Gliosarcoma in the Rat Brain Using Proteomic Analysis.

PubMed

Yan, Kun; Fu, Zongming; Yang, Chen; Zhang, Kai; Jiang, Shanshan; Lee, Dong-Hoon; Heo, Hye-Young; Zhang, Yi; Cole, Robert N; Van Eyk, Jennifer E; Zhou, Jinyuan

2015-08-01

To investigate the biochemical origin of the amide photon transfer (APT)-weighted hyperintensity in brain tumors. Seven 9 L gliosarcoma-bearing rats were imaged at 4.7 T. Tumor and normal brain tissue samples of equal volumes were prepared with a coronal rat brain matrix and a tissue biopsy punch. The total tissue protein and the cytosolic subproteome were extracted from both samples. Protein samples were analyzed using two-dimensional gel electrophoresis, and the proteins with significant abundance changes were identified by mass spectrometry. There was a significant increase in the cytosolic protein concentration in the tumor, compared to normal brain regions, but the total protein concentrations were comparable. The protein profiles of the tumor and normal brain tissue differed significantly. Six cytosolic proteins, four endoplasmic reticulum proteins, and five secreted proteins were considerably upregulated in the tumor. Our experiments confirmed an increase in the cytosolic protein concentration in tumors and identified several key proteins that may cause APT-weighted hyperintensity.

Measurement of trace impurities in ultra pure hydrogen and deuterium at the parts-per-billion level using gas chromatography

NASA Astrophysics Data System (ADS)

Ganzha, V.; Ivshin, K.; Kammel, P.; Kravchenko, P.; Kravtsov, P.; Petitjean, C.; Trofimov, V.; Vasilyev, A.; Vorobyov, A.; Vznuzdaev, M.; Wauters, F.

2018-02-01

A series of muon experiments at the Paul Scherrer Institute in Switzerland deploy ultra-pure hydrogen active targets. A new gas impurity analysis technique was developed, based on conventional gas chromatography, with the capability to measure part-per-billion (ppb) traces of nitrogen and oxygen in hydrogen and deuterium. Key ingredients are a cryogenic admixture accumulation, a directly connected sampling system and a dedicated calibration setup. The dependence of the measured concentration on the sample volume was investigated, confirming that all impurities from the sample gas are collected in the accumulation column and measured with the gas chromatograph. The system was calibrated utilizing dynamic dilution of admixtures into the gas flow down to sub-ppb level concentrations. The total amount of impurities accumulated in the purification system during a three month long experimental run was measured and agreed well with the calculated amount based on the measured concentrations in the flow.

The mercury isotope composition of Arctic coastal seawater

NASA Astrophysics Data System (ADS)

Štrok, Marko; Baya, Pascale Anabelle; Hintelmann, Holger

2015-11-01

For the first time, Hg isotope composition of seawater in the Canadian Arctic Archipelago is reported. Hg was pre-concentrated from large volumes of seawater sampling using anion exchange resins onboard the research vessel immediately after collection. Elution of Hg was performed in laboratory followed by isotope composition determination by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). For comparison, seawater from two stations was shipped to the laboratory and processed within it. Results showed negative mass-dependent fractionation in the range from -2.85 to -1.10‰ for δ202Hg, as well as slightly positive mass-independent fractionation of odd Hg isotopes. Positive mass-independent fractionation of 200Hg was also observed. Samples that were pre-concentrated in the laboratory showed different Hg isotope signatures and this is most probably due to the abiotic reduction of Hg in the dark by organic matter during storage and shipment after sampling. This emphasizes the need for immediate onboard pre-concentration.

Phase behaviour of oat β-glucan/sodium caseinate mixtures varying in molecular weight.

PubMed

Agbenorhevi, Jacob K; Kontogiorgos, Vassilis; Kasapis, Stefan

2013-05-01

The isothermal phase behaviour at 5 °C of mixtures of sodium caseinate and oat β-glucan isolates varying in molecular weight (MW) was investigated by means of phase diagram construction, rheometry, fluorescence microscopy and electrophoresis. Phase diagrams indicated that the compatibility of the β-glucan/sodium caseinate system increases as β-glucan MW decreases. Images of mixtures taken at various biopolymer concentrations revealed phase separated domains. Results also revealed that at the state of thermodynamic equilibrium, lower MW samples yielded considerable viscosity in the mixture. At equivalent hydrodynamic volume of β-glucan in the mixtures, samples varying in molecular weight exhibited similar flow behaviour. A deviation dependent on the protein concentration was observed for the high MW sample in the concentrated regime due to the size of β-glucan aggregates formed. Results demonstrate that by controlling the structural features of β-glucan in mixtures with sodium caseinate, informed manipulation of rheological properties in these systems can be achieved. Copyright © 2012 Elsevier Ltd. All rights reserved.

On-line preconcentration and speciation of arsenic by flow injection hydride generation atomic absorption spectrophotometry.

PubMed

Narcise, Cristine Ingrid S; Coo, Lilibeth Dlc; Del Mundo, Florian R

2005-12-15

A flow injection-column preconcentration-hydride generation atomic absorption spectrophotometric (FI-column-HGAAS) method was developed for determining mug/l levels of As(III) and As(V) in water samples, with simultaneous preconcentration and speciation. The speciation scheme involved determining As(V) at neutral pH and As(III+V) at pH 12, with As(III) obtained by difference. The enrichment factor (EF) increased with increase in sample loading volume from 2.5 to 10ml, and for preconcentration using the chloride-form anion exchange column, EFs ranged from 5 to 48 for As(V) and 4 to 24 for As(III+V), with corresponding detection limits of 0.03-0.3 and 0.07-0.3mug/l. Linear concentration range (LCR) also varied with sample loading volume, and for a 5-ml sample was 0.3-5 and 0.2-8mug/l for As(V) and As(III+V), respectively. Sample throughput, which decreased with increase in sample volume, was 8-17 samples/h. For the hydroxide-form column, the EFS for 2.5-10ml samples were 3-23 for As(V) and 2-15 for As(III+V), with corresponding detection limits of 0.07-0.4 and 0.1-0.5mug/l. The LCR for a 5-ml sample was 0.3-10mug/l for As(V) and 0.2-20mug/l for As(III+V). Sample throughput was 10-20 samples/h. The developed method has been effectively applied to tap water and mineral water samples, with recoveries ranging from 90 to 102% for 5-ml samples passed through the two columns.

The effects of training volume and competition on the salivary cortisol concentrations of Olympic weightlifters.

PubMed

Crewther, Blair T; Heke, Taati; Keogh, Justin W L

2011-01-01

This study examined the effects of training volume and competition on the salivary cortisol (Sal-C) concentrations of Olympic weightlifters. Male (n = 5) and female (n = 4) Olympic weightlifters provided saliva samples across a 5-week experimental = period. The first aim was to assess the weekly effects of high (≥ 200 sets) and low (≤ 100 sets) training volume on Sal-C. The second aim was to compare Sal-C concentrations and 1 repetition maximum (1RM) performance during 2 simulated and 2 actual competitions. Performance was assessed using the snatch, clean and jerk, and the Olympic total lift. Data from each competition setting were pooled before analysis. There were no significant weekly changes in Sal-C levels (p > 0.05). The actual competitions produced higher (128-130%) Sal-C concentrations (p < 0.001) and superior 1RM lifts (1.9-2.6%) for the clean and jerk, and the Olympic total, than the simulated competitions (p < 0.05). Individual Sal-C concentrations before the simulated competitions were positively correlated to all of the 1RM lifts (r = 0.48-0.49, p < 0.05). In conclusion, actual competitions produced greater Sal-C responses than simulated competitions, and this appeared to benefit the 1RM performance of Olympic weightlifters. Individuals with higher Sal-C concentrations also tended to exhibit superior 1RM lifts during the simulated competitions. Given these findings, greater emphasis should be placed upon the monitoring of C to establish normative values, training standards and to assist with performance prediction.

Effect of a commercial anion dietary supplement on acid-base balance, urine volume, and urinary ion excretion in male goats fed oat or grass hay diets.

PubMed

Stratton-Phelps, Meri; House, John K

2004-10-01

To determine whether feeding a commercial anionic dietary supplement as a urinary acidifier to male goats may be useful for management of urolithiasis. 8 adult sexually intact male Toggenburg, Saanen, and Nubian goats. Goats were randomly assigned by age-, breed-, and weight-matched pairs to an oat or grass hay diet that was fed for 12 days. On days 13 to 14 (early sample collection time before supplementation), measurements were made of blood and urine sodium, potassium, calcium, magnesium, chloride, phosphorus, and sulfur concentrations; blood and urine pH; urine production; and water consumption. During the next 28 days, the anionic dietary supplement was added to the oat and grass hay diets to achieve a dietary cation-anion difference of 0 mEq/100g of dry matter. Blood and urine samples were analyzed during dietary supplementation on days 12 to 13 (middle sample collection time) and 27 to 28 (late sample collection time). Blood bicarbonate, pH, and urine pH of goats fed grass hay and goats fed oat hay were significantly decreased during the middle and late sample collection times, compared with the early sample collection time. Water consumption and urine production in all goats increased significantly during the late sample collection time, compared with the early sample collection time. The anionic dietary supplement used in our study increases urine volume, alters urine ion concentrations, and is an efficacious urinary acidifier in goats. Goats treated with prolonged anionic dietary supplementation should be monitored for secondary osteoporosis from chronic urinary calcium loss.

A multi-residue method for characterization and determination of atmospheric pesticides measured at two French urban and rural sampling sites.

PubMed

Baraud, Laurent; Tessier, Didier; Aaron, Jean-Jacques; Quisefit, Jean-Paul; Pinart, Johann

2003-12-01

The extensive use of pesticides to protect agricultural crops can result in the transfer of these compounds into the atmosphere and their diffusion towards urban areas. Precise evaluation of the geographic impact of this type of pollution is important environmentally. In this paper, analytical methods for the sampling, characterization, and determination of agricultural pesticides in air were developed; the methods were then applied in the Paris and Champagne regions. Sixteen pesticides belonging to nine chemical families were monitored. Sampling was carried out in urban (Paris) and rural (Aube district) sites, utilizing either a high-volume pump (12.5 m3 h(-1)) (urban site) or a low-volume pump (2.3 m3 h(-1)) for the rural site. Quartz filters and polyurethane foams (PUF) were used for sampling in all cases. After extracting the samples and concentrating the recovered solutions, high-performance liquid chromatography (HPLC) analysis with UV detection was performed. Identification of the pesticides was confirmed by applying to the HPLC measurements a novel UV-detection procedure based on the normalized absorbance variation with wavelength (Noravawa procedure). The presence of metsulfuron methyl, isoproturon, linuron, deltamethrin (and/or malathion), and chlorophenoxy acids (2,4-D and MCPP) was found at the urban sampling site at levels ranging from about 1 to 1130 ng m(-3) of air, depending on the compound and sampling period. On the rural sampling site residues of isoproturon, deltamethrin (and/or malathion), MCPP, and 2,4-D were generally detected at higher levels (19-5130 ng m(-3)) than on the urban site, as expected. The effects of the weather conditions and agricultural activity on the atmospheric concentrations of pesticides are discussed, as are long-range atmospheric transfer processes for these pesticides.

A portable molecular-sieve-based CO{sub 2} sampling system for radiocarbon measurements

DOE Office of Scientific and Technical Information (OSTI.GOV)

Palonen, V., E-mail: vesa.palonen@helsinki.fi

We have developed a field-capable sampling system for the collection of CO{sub 2} samples for radiocarbon-concentration measurements. Most target systems in environmental research are limited in volume and CO{sub 2} concentration, making conventional flask sampling hard or impossible for radiocarbon studies. The present system captures the CO{sub 2} selectively to cartridges containing 13X molecular sieve material. The sampling does not introduce significant under-pressures or significant losses of moisture to the target system, making it suitable for most environmental targets. The system also incorporates a significantly larger sieve container for the removal of CO{sub 2} from chambers prior to the CO{submore » 2} build-up phase and sampling. In addition, both the CO{sub 2} and H{sub 2}O content of the sample gas are measured continuously. This enables in situ estimation of the amount of collected CO{sub 2} and the determination of CO{sub 2} flux to a chamber. The portable sampling system is described in detail and tests for the reliability of the method are presented.« less

Simultaneous LC/MS/MS determination of thiols and disulfides in urine samples based on differential labeling with ferrocene-based maleimides.

PubMed

Seiwert, Bettina; Karst, Uwe

2007-09-15

A method for the simultaneous determination of a series of thiols and disulfides in urine samples has been developed based on the sequential labeling of free and bound thiol functionalities with two ferrocene-based maleimide reagents. The sample is first exposed to N-(2-ferroceneethyl)maleimide, thus leading to the derivatization of free thiol groups in the sample. After quantitative reaction and subsequent reduction of the disulfide-bound thiols by tris(2-carboxyethyl)phosphine, the newly formed thiol functionalities are reacted with ferrocenecarboxylic acid-(2-maleimidoyl)ethylamide. The reaction products are determined by LC/MS/MS in the multiple reaction mode, and precursor ion scan as well as neutral loss scan is applied to detect unknown further thiols. The method was successfully applied to the analysis of free and disulfide-bound thiols in urine samples. Limits of detection are 30 to 110 nM, and the linear range comprises two decades of concentration, thus covering the relevant concentration range of thiols in urine samples. The thiol and disulfide concentrations were referred to the creatinine content to compensate for different sample volumes. As some calibration standards for the disulfides are not commercially available, they were synthesized in an electrochemical flow-through cell. This allowed the synthesis of hetero- and homodimeric disulfides.

Pressurized capillary electrochromatographic analysis of water-soluble vitamins by combining with on-line concentration technique.

PubMed

Jia, Li; Liu, Yaling; Du, Yanyan; Xing, Da

2007-06-22

A pressurized capillary electrochromatography (pCEC) system was developed for the separation of water-soluble vitamins, in which UV absorbance was used as the detection method and a monolithic silica-ODS column as the separation column. The parameters (type and content of organic solvent in the mobile phase, type and concentration of electrolyte, pH of the electrolyte buffer, applied voltage and flow rate) affecting the separation resolution were evaluated. The combination of two on-line concentration techniques, namely, solvent gradient zone sharpening effect and field-enhanced sample stacking, was utilized to improve detection sensitivity, which proved to be beneficial to enhance the detection sensitivity by enabling the injection of large volumes of samples. Coupling electrokinetic injection with the on-line concentration techniques was much more beneficial for the concentration of positively charged vitamins. Comparing with the conventional injection mode, the enhancement in the detection sensitivities of water-soluble vitamins using the on-line concentration technique is in the range of 3 to 35-fold. The developed pCEC method was applied to evaluate water-soluble vitamins in corns.

Quantification of 18F-fluorocholine kinetics in patients with prostate cancer.

PubMed

Verwer, Eline E; Oprea-Lager, Daniela E; van den Eertwegh, Alfons J M; van Moorselaar, Reindert J A; Windhorst, Albert D; Schwarte, Lothar A; Hendrikse, N Harry; Schuit, Robert C; Hoekstra, Otto S; Lammertsma, Adriaan A; Boellaard, Ronald

2015-03-01

Choline kinase is upregulated in prostate cancer, resulting in increased (18)F-fluoromethylcholine uptake. This study used pharmacokinetic modeling to validate the use of simplified methods for quantification of (18)F-fluoromethylcholine uptake in a routine clinical setting. Forty-minute dynamic PET/CT scans were acquired after injection of 204 ± 9 MBq of (18)F-fluoromethylcholine, from 8 patients with histologically proven metastasized prostate cancer. Plasma input functions were obtained using continuous arterial blood-sampling as well as using image-derived methods. Manual arterial blood samples were used for calibration and correction for plasma-to-blood ratio and metabolites. Time-activity curves were derived from volumes of interest in all visually detectable lymph node metastases. (18)F-fluoromethylcholine kinetics were studied by nonlinear regression fitting of several single- and 2-tissue plasma input models to the time-activity curves. Model selection was based on the Akaike information criterion and measures of robustness. In addition, the performance of several simplified methods, such as standardized uptake value (SUV), was assessed. Best fits were obtained using an irreversible compartment model with blood volume parameter. Parent fractions were 0.12 ± 0.4 after 20 min, necessitating individual metabolite corrections. Correspondence between venous and arterial parent fractions was low as determined by the intraclass correlation coefficient (0.61). Results for image-derived input functions that were obtained from volumes of interest in blood-pool structures distant from tissues of high (18)F-fluoromethylcholine uptake yielded good correlation to those for the blood-sampling input functions (R(2) = 0.83). SUV showed poor correlation to parameters derived from full quantitative kinetic analysis (R(2) < 0.34). In contrast, lesion activity concentration normalized to the integral of the blood activity concentration over time (SUVAUC) showed good correlation (R(2) = 0.92 for metabolite-corrected plasma; 0.65 for whole-blood activity concentrations). SUV cannot be used to quantify (18)F-fluoromethylcholine uptake. A clinical compromise could be SUVAUC derived from 2 consecutive static PET scans, one centered on a large blood-pool structure during 0-30 min after injection to obtain the blood activity concentrations and the other a whole-body scan at 30 min after injection to obtain lymph node activity concentrations. © 2015 by the Society of Nuclear Medicine and Molecular Imaging, Inc.

Atmospheric chlorinated polycyclic aromatic hydrocarbons in East Asia.

PubMed

Kakimoto, Kensaku; Nagayoshi, Haruna; Konishi, Yoshimasa; Kajimura, Keiji; Ohura, Takeshi; Hayakawa, Kazuichi; Toriba, Akira

2014-09-01

This study estimates atmospheric concentrations of chlorinated polycyclic aromatic hydrocarbons (ClPAHs) and polycyclic aromatic hydrocarbons (PAHs) in East Asia using a Gas Chromatograph with High Resolution Mass Spectrometer (GC-HRMS). ClPAHs are ubiquitously generated from PAHs through substitution, and some ClPAHs show higher aryl hydrocarbon receptor (AhR)-mediated activities than their parent PAHs. Atmospheric particles were collected using a high-volume air sampler equipped with a quartz-fiber filter. We determined the ClPAH concentrations of atmospheric particles collected in Japan (Sapporo, Sagamihara, Kanazawa, and Kitakyushu), Korea (Busan), and China (Beijing). The concentrations of ClPAHs were highest in the winter Beijing sample, where the total mean concentration was approximately 15-70 times higher than in the winter samples from Japan and Korea. The concentrations of Σ19ClPAHs and Σ9PAHs were significantly correlated in the Kanazawa and the Busan samples. This indicates that within those cities ClPAHs and PAHs share the same origin, implying direct chlorination of parent PAHs. Toxic equivalent concentrations (TEQs) of the total ClPAHs and PAHs were lowest in Kanazawa in the summer, reaching 1.18 and 2610fg-TEQm(-3) respectively, and highest in Beijing in the winter, reaching 627 and 4240000fg-TEQm(-3) respectively. Copyright © 2014 Elsevier Ltd. All rights reserved.

Optics-Integrated Microfluidic Platforms for Biomolecular Analyses

PubMed Central

Bates, Kathleen E.; Lu, Hang

2016-01-01

Compared with conventional optical methods, optics implemented on microfluidic chips provide small, and often much cheaper ways to interrogate biological systems from the level of single molecules up to small model organisms. The optical probing of single molecules has been used to investigate the mechanical properties of individual biological molecules; however, multiplexing of these measurements through microfluidics and nanofluidics confers many analytical advantages. Optics-integrated microfluidic systems can significantly simplify sample processing and allow a more user-friendly experience; alignments of on-chip optical components are predetermined during fabrication and many purely optical techniques are passively controlled. Furthermore, sample loss from complicated preparation and fluid transfer steps can be virtually eliminated, a particularly important attribute for biological molecules at very low concentrations. Excellent fluid handling and high surface area/volume ratios also contribute to faster detection times for low abundance molecules in small sample volumes. Although integration of optical systems with classical microfluidic analysis techniques has been limited, microfluidics offers a ready platform for interrogation of biophysical properties. By exploiting the ease with which fluids and particles can be precisely and dynamically controlled in microfluidic devices, optical sensors capable of unique imaging modes, single molecule manipulation, and detection of minute changes in concentration of an analyte are possible. PMID:27119629

Drop size distributions and related properties of fog for five locations measured from aircraft

NASA Technical Reports Server (NTRS)

Zak, J. Allen

1994-01-01

Fog drop size distributions were collected from aircraft as part of the Synthetic Vision Technology Demonstration Program. Three west coast marine advection fogs, one frontal fog, and a radiation fog were sampled from the top of the cloud to the bottom as the aircraft descended on a 3-degree glideslope. Drop size versus altitude versus concentration are shown in three dimensional plots for each 10-meter altitude interval from 1-minute samples. Also shown are median volume radius and liquid water content. Advection fogs contained the largest drops with median volume radius of 5-8 micrometers, although the drop sizes in the radiation fog were also large just above the runway surface. Liquid water content increased with height, and the total number of drops generally increased with time. Multimodal variations in number density and particle size were noted in most samples where there was a peak concentration of small drops (2-5 micrometers) at low altitudes, midaltitude peak of drops 5-11 micrometers, and high-altitude peak of the larger drops (11-15 micrometers and above). These observations are compared with others and corroborate previous results in fog gross properties, although there is considerable variation with time and altitude even in the same type of fog.

Vortex-assisted surfactant-enhanced emulsification microextraction based on solidification of floating organic drop combined with high performance liquid chromatography for determination of naproxen and nabumetone.

PubMed

Asadi, Mohammad; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh; Abbasi, Bijan

2015-12-18

A novel, rapid, simple and green vortex-assisted surfactant-enhanced emulsification microextraction method based on solidification of floating organic drop was developed for simultaneous separation/preconcentration and determination of ultra trace amounts of naproxen and nabumetone with high performance liquid chromatography-fluorescence detection. Some parameters influencing the extraction efficiency of analytes such as type and volume of extractant, type and concentration of surfactant, sample pH, KCl concentration, sample volume, and vortex time were investigated and optimized. Under optimal conditions, the calibration graph exhibited linearity in the range of 3.0-300.0ngL(-1) for naproxen and 7.0-300.0ngL(-1) for nabumetone with a good coefficient of determination (R(2)>0.999). The limits of detection were 0.9 and 2.1ngL(-1). The relative standard deviations for inter- and intra-day assays were in the range of 5.8-10.1% and 3.8-6.1%, respectively. The method was applied to the determination of naproxen and nabumetone in urine, water, wastewater and milk samples and the accuracy was evaluated through recovery experiments. Copyright © 2015 Elsevier B.V. All rights reserved.

Comparative evaluation of saliva collection methods for proteome analysis.

PubMed

Golatowski, Claas; Salazar, Manuela Gesell; Dhople, Vishnu Mukund; Hammer, Elke; Kocher, Thomas; Jehmlich, Nico; Völker, Uwe

2013-04-18

Saliva collection devices are widely used for large-scale screening approaches. This study was designed to compare the suitability of three different whole-saliva collection approaches for subsequent proteome analyses. From 9 young healthy volunteers (4 women and 5 men) saliva samples were collected either unstimulated by passive drooling or stimulated using a paraffin gum or Salivette® (cotton swab). Saliva volume, protein concentration and salivary protein patterns were analyzed comparatively. Samples collected using paraffin gum showed the highest saliva volume (4.1±1.5 ml) followed by Salivette® collection (1.8±0.4 ml) and drooling (1.0±0.4 ml). Saliva protein concentrations (average 1145 μg/ml) showed no significant differences between the three sampling schemes. Each collection approach facilitated the identification of about 160 proteins (≥2 distinct peptides) per subject, but collection-method dependent variations in protein composition were observed. Passive drooling, paraffin gum and Salivette® each allows similar coverage of the whole saliva proteome, but the specific proteins observed depended on the collection approach. Thus, only one type of collection device should be used for quantitative proteome analysis in one experiment, especially when performing large-scale cross-sectional or multi-centric studies. Copyright © 2013 Elsevier B.V. All rights reserved.

Simultaneous determination of the quantity and isotopic signature of dissolved organic matter from soil water using high-performance liquid chromatography/isotope ratio mass spectrometry.

PubMed

Scheibe, Andrea; Krantz, Lars; Gleixner, Gerd

2012-01-30

We assessed the accuracy and utility of a modified high-performance liquid chromatography/isotope ratio mass spectrometry (HPLC/IRMS) system for measuring the amount and stable carbon isotope signature of dissolved organic matter (DOM) <1 µm. Using a range of standard compounds as well as soil solutions sampled in the field, we compared the results of the HPLC/IRMS analysis with those from other methods for determining carbon and (13)C content. The conversion efficiency of the in-line wet oxidation of the HPLC/IRMS averaged 99.3% for a range of standard compounds. The agreement between HPLC/IRMS and other methods in the amount and isotopic signature of both standard compounds and soil water samples was excellent. For DOM concentrations below 10 mg C L(-1) (250 ng C total) pre-concentration or large volume injections are recommended in order to prevent background interferences. We were able to detect large differences in the (13)C signatures of soil solution DOM sampled in 10 cm depth of plots with either C3 or C4 vegetation and in two different parent materials. These measurements also demonstrated changes in the (13)C signature that demonstrate rapid loss of plant-derived C with depth. Overall the modified HLPC/IRMS system has the advantages of rapid sample preparation, small required sample volume and high sample throughput, while showing comparable performance with other methods for measuring the amount and isotopic signature of DOM. Copyright © 2011 John Wiley & Sons, Ltd.

[Emission Characteristics of VOCs from Typical Restaurants in Beijing].

PubMed

Cui, Tong; Cheng, Jing-chen; He, Wan-qing; Ren, Pei-fang; Nie, Lei; Xu, Dong-yao; Pan, Tao

2015-05-01

Using the EPA method, emission of volatile organic compounds (VOCs) , sampled from barbecue, Chinese and Western fast-food, Sichuan cuisine and Zhejiang cuisine restaurants in Beijing was investigated. VOCs concentrations and components from different cuisines were studied. The results indicated that based on the calibrated baseline ventilation volume, the VOCs emission level from barbecue was the highest, reaching 12.22 mg · m(-3), while those from fast-food of either Chinese or Western, Sichuan cuisine and Zhejiang cuisine were about 4 mg · m(-3). The components of VOCs from barbecue were different from those in the other cuisines, which were mainly propylene, 1-butene, n-butane, etc. The non-barbecue cuisines consisted of high concentration of alcohols, and Western fast-food contained relatively high proportion of aldehydes and ketones organic compounds. According to emission concentration of baseline ventilation volume, barbecue released more pollutants than the non-barbecue cuisines at the same scale. So, barbecue should be supervised and controlled with the top priority.

Deformational behaviour of knee cartilage and changes in serum cartilage oligomeric matrix protein (COMP) after running and drop landing.

PubMed

Niehoff, A; Müller, M; Brüggemann, L; Savage, T; Zaucke, F; Eckstein, F; Müller-Lung, U; Brüggemann, G-P

2011-08-01

To investigate (1) the effect of running and drop landing interventions on knee cartilage deformation and serum cartilage oligomeric matrix protein (COMP) concentration and (2) if the changes in cartilage volume correlate with the changes in serum COMP level. Knee joint cartilage volume and thickness were determined using magnetic resonance imaging (MRI) as well as COMP concentration from serum samples before and after in vivo loading of 14 healthy adults (seven male and seven female). Participants performed different loading interventions of 30 min duration on three different days: (1) 100 vertical drop landings from a 73 cm high platform, (2) running at a velocity of 2.2m/s (3.96 km), and (3) resting on a chair. Blood samples were taken immediately before, immediately after and 0.5h, 1h, 2h and 3h post intervention. Pre- and post-loading coronal and axial gradient echo MR images with fat suppression were used to determine the patellar, tibial and femoral cartilage deformation. Serum COMP levels increased immediately after the running (+30.7%, pre: 7.3U/l, 95% confidence interval (CI): 5.6, 8.9, post: 9.1U/l, 95% CI: 7.2, 11.0, P=0.001) and after drop landing intervention (+32.3%, pre: 6.8U/l, 95% CI: 5.3, 8.4; post: 8.9U/l, 95% CI: 6.8, 10.9, P=0.001). Cartilage deformation was more pronounced after running compared to drop landing intervention, with being significant (volume: P=0.002 and thickness: P=0.001) only in the lateral tibia. We found a significant correlation (r(2)=0.599, P=0.001) between changes in serum COMP (%) and in cartilage volume (%) after the drop landing intervention, but not after running. In vivo exercise interventions differentially regulate serum COMP concentrations and knee cartilage deformations. The relation between changes in COMP and in cartilage volume seems to depend on both mechanical and biochemical factors. Copyright © 2011 Osteoarthritis Research Society International. Published by Elsevier Ltd. All rights reserved.

Comparison of the effects of intravenous administration of isotonic and hypertonic sodium bicarbonate solutions on venous acid-base status in dehydrated calves with strong ion acidosis.

PubMed

Coskun, Alparslan; Sen, Ismail; Guzelbektes, Hasan; Ok, Mahmut; Turgut, Kursat; Canikli, Sebnem

2010-05-15

OBJECTIVE-To compare the effects of IV administration of isotonic (1.3%) and hypertonic (8.4%) sodium bicarbonate (NaHCO(3)) solutions on acid-base status in dehydrated calves with strong ion (metabolic) acidosis. DESIGN-Randomized controlled clinical trial. ANIMALS-50 calves with diarrhea and severe dehydration. PROCEDURES-Calves were randomly assigned to receive isotonic NaHCO(3) solution (65 mL/kg [29.5 mL/lb], IV) over 3 hours (n = 30) or hypertonic NaHCO(3) solution (10 mL/kg [4.5 mL/lb], IV) over 20 minutes (20). Blood samples were collected at 0 hours (immediately prior to solution administration) and at 0.5, 1, 2, and 4 hours after administration began. Samples were submitted for blood gas analysis, serum biochemical analysis, and determination of blood Na(+), K(+), and Cl(-) concentrations and percentage change in plasma volume. RESULTS-Calves that received isotonic NaHCO(3) solution had an increase in venous blood pH, HCO(3) concentration, and base excess; a small, transient increase in Po(2); and no change in Pco(2) within 4 hours after administration began. Calves that received hypertonic NaHCO(3) solution had an immediate increase in venous blood pH, HCO(3) concentration, and base excess; a small, transient increase Pco(2); and no change in Po(2) within 0.5 hours after treatment began. Plasma volume increased to a greater extent following administration of isotonic solution than after administration of hypertonic solution. CONCLUSIONS AND CLINICAL RELEVANCE-IV administration of 8.4% NaHCO(3) solution in small volumes provided fast and effective improvement of severe acid-base abnormalities in calves with severe strong ion acidosis but did not improve hydration status as well as administration of a larger volume of isotonic NaHCO(3) solution.

An experimental correlation approach for predicting thermal conductivity of water-EG based nanofluids of zinc oxide

NASA Astrophysics Data System (ADS)

Ahmadi Nadooshan, Afshin

2017-03-01

In this study, the effects of temperature (20 °C

Effect of ZnO on the Physical Properties and Optical Band Gap of Soda Lime Silicate Glass

PubMed Central

Zaid, Mohd Hafiz Mohd; Matori, Khamirul Amin; Aziz, Sidek Hj. Abdul; Zakaria, Azmi; Ghazali, Mohd Sabri Mohd

2012-01-01

This manuscript reports on the physical properties and optical band gap of five samples of soda lime silicate (SLS) glass combined with zinc oxide (ZnO) that were prepared by a melting and quenching process. To understand the role of ZnO in this glass structure, the density, molar volume and optical band gaps were investigated. The density and absorption spectra in the Ultra-Violet-Visible (UV-Visible) region were recorded at room temperature. The results show that the densities of the glass samples increased as the ZnO weight percentage increased. The molar volume of the glasses shows the same trend as the density: the molar volume increased as the ZnO content increased. The optical band gaps were calculated from the absorption edge, and it was found that the optical band gap decreased from 3.20 to 2.32 eV as the ZnO concentration increased. PMID:22837711

Photosensitizer quantitation in vivo by flourescence microsampling

NASA Astrophysics Data System (ADS)

Pogue, Brian W.; Burke, Gregory C.; Lee, Claudia C.; Hoopes, P. Jack

2000-06-01

Photodynamic therapy can provide a reliable method of tumor destruction when the appropriate dosimetry is applied. Current dosimetry practice involves quantification of the drug and light doses applied to the tumor, but it would be desirable to monitor in vivo light and drug levels to provide the most accurate determination of dosimetry. In vivo measurements can be used to minimize variations in treatment response due to inter-animal variability, by providing animal-specific or patient-specific treatment planning. This study reports on the development of a micro-sampling method to measure fluorescence from tissue, which is not significantly affected by the tissue optical properties. The system measures fluorescence from the surface of a tissue, using a fiber bundle composed of individual 100 micron fibers which ar all spaced apart by 700 microns from one another at the tissue contact end. This design provides sampling of the fluorescence at multiple sites to increase the signal intensity, while maintaining a micro- sampling of the tissue volume just below the surface. The calibration studies here indicate that the 1/e sampling depth is near 60 microns when measured in optical phantoms, which are similar to typical tissue properties. The probe fluorescence signal is independent of blood concentration up to a maximum of 10% blood by volume, which is similar to most tumor tissue. Animal tests indicate that the sensitivity to drug concentration is essentially the same in when measured in murine liver and muscle tissues, both in vivo and ex vivo. These preliminary calibration results suggest that the probe can be used to measure photosensitizer uptake in vivo non- invasively and rapidly via conversion of fluorescence intensity to photosensitizer concentration.

Development of new portable miniaturize solid phase microextraction of silver-APDC complex using micropipette tip in-syringe system couple with electrothermal atomic absorption spectrometry.

PubMed

Naeemullah; Kazi, Tasneem Gul; Afridi, Hassan Imran; Shah, Faheem; Arain, Sadaf Sadia; Arain, Salma Aslam; Panhwar, Abdul Haleem; Arain, Mariam Shahzadi; Samoon, Muhammad Kashif

2016-02-05

An innovative and simple miniaturized solid phase microextraction (M-SPME) method, was developed for preconcentration and determination of silver(I) in the fresh and waste water samples. For M-SPME, a micropipette tip packed with activated carbon cloth (ACC) as sorbent, in a syringe system. The size, morphology and elemental composition of ACC before and after adsorption of analyte have been characterized by scanning electron microscopy and energy dispersive spectroscopy. The sample solution treated with a complexing reagent, ammonium pyrrolidine dithiocarbamate (APDC), was drawn into the syringe filled with ACC and dispensed manually for 2 to 10 aspirating/dispensing cycle. Then the Ag- complex sorbed on the ACC in micropipette was quantitatively eluted by drawing and dispensing of different concentrations of acids for 2 to 5 aspirating/dispensing cycles. The extracted Ag ions with modifier were injected directly into the electrothermal atomic absorption spectrometry for analysis. The influence of different variables on the extraction efficiency, including the concentration of ligand, pH, sample volume, eluent type, concentration and volume was investigated. Validity and accuracy of the developed method was checked by the standard addition method. Reliability of the proposed methodology was checked by the relative standard deviation (%RSD), which was found to be <5%. Under the optimized experimental variables, the limits of detection (LOD) and enhancement factors (EF), were obtained to be 0.86 ng L(-1) and 120, respectively. The proposed method was successfully applied for the determination of trace levels of silver ions in fresh and waste water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of heavy metal ions in vegetable samples using a magnetic metal-organic framework nanocomposite sorbent.

PubMed

Hassanpour, Akbar; Hosseinzadeh-Khanmiri, Rahim; Babazadeh, Mirzaagha; Abolhasani, Jafar; Ghorbani-Kalhor, Ebrahim

2015-01-01

This paper describes the synthesis and application of a novel magnetic metal-organic framework (MOF) [(Fe₃O₄-benzoyl isothiocyanate)/Cu₃(benzene-1,3,5-tricarboxylate)₂] to pre-concentrate trace amounts of Cd(II), Pb(II), Zn(II) and Cr(III) ions and their determination by flame atomic absorption spectrometry. A Box-Behnken design was used to find the parameters affecting the pre-concentration procedure through response surface methodology. Three factors including uptake time, amount of the magnetic sorbent and pH of the sample were selected as affecting factors in the sorption step, and four factors including type, volume and concentration of the eluent as well as the elution time were selected in the elution step for the optimisation study. The opted values were 30 mg, 10.1 min, 5.9, EDTA, 4.0 ml, 0.57 mol l(-1) EDTA solution and 13.0 min for the amount of the magnetic sorbent, uptake time, pH of the sample, type, volume, concentration of the eluent, and elution time, respectively. The limits of detection (LODs) were 0.12, 0.7, 0.16, and 0.4 ng ml(-1) for Cd(II), Pb(II), Zn(II) and Cr(III) ions, respectively. The relative standard deviations (RSDs) of the method were less than 7.2% for five separate batch experiments for the determination of 30 μg l(-1) of Cd(II), Pb(II), Zn(II) and Cr(III) ions. The sorption capacity of the [(Fe₃O₄-benzoyl isothiocyanate)/MOF] was 175 mg g(-1) for Cd(II), 168 mg g(-1) for Pb(II), 210 mg g(-1) for Zn(II) and 196 mg g(-1) for Cr(III). It was found that the magnetic MOF nanocomposite demonstrated a higher capacity compared with Fe₃O₄-benzoyl isothiocyanate. Finally, the magnetic MOF nanocomposite was successfully applied to the rapid extraction of trace amounts of the heavy metal ions from vegetable samples.

Multiple-wavelength spectroscopic quantitation of light-absorbing species in scattering media

DOEpatents

Nathel, Howard; Cartland, Harry E.; Colston, Jr., Billy W.; Everett, Matthew J.; Roe, Jeffery N.

2000-01-01

An oxygen concentration measurement system for blood hemoglobin comprises a multiple-wavelength low-coherence optical light source that is coupled by single mode fibers through a splitter and combiner and focused on both a target tissue sample and a reference mirror. Reflections from both the reference mirror and from the depths of the target tissue sample are carried back and mixed to produce interference fringes in the splitter and combiner. The reference mirror is set such that the distance traversed in the reference path is the same as the distance traversed into and back from the target tissue sample at some depth in the sample that will provide light attenuation information that is dependent on the oxygen in blood hemoglobin in the target tissue sample. Two wavelengths of light are used to obtain concentrations. The method can be used to measure total hemoglobin concentration [Hb.sub.deoxy +Hb.sub.oxy ] or total blood volume in tissue and in conjunction with oxygen saturation measurements from pulse oximetry can be used to absolutely quantify oxyhemoglobin [HbO.sub.2 ] in tissue. The apparatus and method provide a general means for absolute quantitation of an absorber dispersed in a highly scattering medium.

Hydrology and Glacier-Lake-Outburst Floods (1987-2004) and Water Quality (1998-2003) of the Taku River near Juneau, Alaska

USGS Publications Warehouse

Neal, Edward G.

2007-01-01

The Taku River Basin originates in British Columbia, Canada, and drains an area of 6,600 square miles at the U.S. Geological Survey's Taku River gaging station. Several mines operated within the basin prior to 1957, and mineral exploration has resumed signaling potential for future mining developments. The U.S. Geological Survey in cooperation with the Douglas Indian Association, Alaska Department of Environmental Conservation, and the U.S. Environmental Protection Agency conducted a water-quality and flood-hydrology study of the Taku River. Water-quality sampling of the Taku River from 1998 through 2003 established a baseline for assessing potential effects of future mining operations on water quality. The annual mean discharge of the Taku River is 13,700 cubic feet per second. The monthly mean discharge ranges from a minimum of 1,940 cubic feet per second in February to a maximum of 34,400 cubic feet per second in June. Nearly 90 percent of the annual discharge is from May through November. The highest spring discharges are sourced primarily from snowmelt and moderate discharges are sustained throughout the summer by glacial meltwaters. An ice cover usually forms over the Taku River in December persisting through the winter into March and occasionally into April. Glacier-lake-outburst floods originating from two glacier-dammed lakes along the margin of the Tulsequah Glacier in British Columbia, Canada, are the source of the greatest peak discharges on the Taku River. The largest flood during the period of record was 128,000 cubic feet per second on June 25, 2004, resulting from an outburst of Lake No Lake. Lake No Lake is the larger of the two lakes. The outburst-flood contribution to peak discharge was 80,000 cubic feet per second. The volume discharged from Lake No Lake is relatively consistent indicating drainage may be triggered when the lake reaches a critical stage. This suggests prediction of the timing of these outburst floods might be possible if lake-stage data were available. Further increases in the volume of Lake No Lake are unlikely as all tributary glaciers have retreated out of the lake basin. Decreasing outburst-flood volumes from Tulsequah Lake suggests a continued decline in the volume of this lake. Physical and chemical parameters and concentrations of basic water-quality constituents indicate good water quality. Samples collected at the Taku River gaging station contained low concentrations of trace elements in the dissolved phase. Trace elements sampled were within acceptable limits when compared with the Alaska Department of Environmental Conservation aquatic-life criteria for fresh waters. The highest concentrations of total trace elements sampled were collected during glacial-outburst floods and likely are associated with suspended sediments. Total trace-element concentrations generally increase with increasing water discharge, although a high correlation for all constituents sampled does not always exist.

The Development of the improved equipment for the measurement radionuclides of xenon in atmospheric air

NASA Astrophysics Data System (ADS)

Pakhomov, S. A.; Dubasov, Y. V.

2009-04-01

The Radium Khlopin Institute have developed the mobile (vehicle based) equipment attended for the providing of the monitoring of radioactive xenon isotopes in atmospheric air on territories, neighboring with NPP. This equipment comprises the improved sampling installation with sample-processing unit and specialized spectrometer of β-γ-coincidences. The principal specificity of sampling installation is the using of the gas-cooling machine attended for the reaching of the cryogenic temperatures, which works without helium, using for cooling the processed air itself. The capacity of sampling reaches 20 cubic meters per hour with the xenon extraction factor of 75%. The duration of the sampling cycle forms 3 - 7 hours depending of the xenon volume requirements. The sample-processing unit is designed on preparative gas chromatograph scheme. Duration of sample-processing procedure does not exceed one and half hour. The volume of the prepared sample is around half liter, it contains 3 - 7 cubic centimeters of the xenon, depending of sampling cycle time. For measurements of xenon radioisotopes containing in obtained sample, was developed a β-γ-coincidences spectrometer on the base of the "ORTEC" HP Ge detector equipped with scintillation β-detector designed as Marinelli chamber of 700 cm3 volume. This spectrometer allows to reduce the ambient background more than in 20 times, with γ-channel efficiency reduction not more than in 1.5 times. The minimum detectable activity of 133Хе (MDA), evaluated by Currie formula for probability 95 % is 0.05 Bq at the exposition of 20 hours. Spectrometer is also intended for determination of the stable krypton and xenon concentrations in β-chamber by X-ray-fluorescent method. Therefore, in a shield of the spectrometer collimating pinhole is made and 241Am source is installed. To improve the sensitivity of the analysis beryllium window is made in β-chamber wall, adjoining to the HPGe detector. X-ray-fluorescent analysis allows to surely define Xe volumetric concentration of 0.05% in β-cell, that is equivalent less then 0,5 cm3 of Xe. The first approbation of described equipment was fulfilled in St. Petersburg at autumn of 2007 year and have shown that the spectrometer allows to measure 133Xe concentration at the level of 2 mBq/m3, and this value is in a good agreement with the results of other measurements. Described equipment was practically approbated in field conditions on 2008 year during the expeditionary work carryout in Sosnovyi Bor, Udomlya and Polyarnie Zori - the cities of North-West of Russia, which are located in close neighboring with acting NPP.

Solid-contact potentiometric polymer membrane microelectrodes for the detection of silver ions at the femtomole level

PubMed Central

Rubinova, Nastassia; Chumbimuni-Torres, Karin; Bakker, Eric

2010-01-01

In recent years, ion-selective electrodes based on polymer membranes have been shown to exhibit detection limits that are often in the nanomolar concentration range, and thus drastically lower than traditionally accepted. Since potentiometry is less dependent on scaling laws that other established analytical techniques, their performance in confined sample volumes is explored here. Solid-contact silver-selective microelectrodes, with a sodium-selective microelectrode as a reference, were inserted into a micropipette tip used as a 50-μl sample. The observed potential stabilities, reproducibilities and detection limits were attractive and largely matched that for large 100-ml samples. This should pave the way for further experiments to detecting ultra-small total ion concentrations by potentiometry, especially when used as a transducer after an amplification step in bioanalysis. PMID:20543910

Quantification of myo-inositol, 1,5-anhydro-D-sorbitol, and D-chiro-inositol using high-performance liquid chromatography with electrochemical detection in very small volume clinical samples

PubMed Central

Schimpf, Karen J.; Meek, Claudia C.; Leff, Richard D.; Phelps, Dale L.; Schmitz, Daniel J.; Cordle, Christopher T.

2015-01-01

Inositol is a six-carbon sugar alcohol and is one of nine biologically significant isomers of hexahydroxycyclohexane. Myo-inositol is the primary biologically active form and is present in higher concentrations in the fetus and newborn than in adults. It is currently being examined for the prevention of retinopathy of prematurity in newborn preterm infants. A robust method for quantifying myo-inositol (MI), D-chiro-inositol (DCI) and 1,5-anhydro-D-sorbitol (ADS) in very small-volume (25 μL) urine, blood serum and/or plasma samples was developed. Using a multiple-column, multiple mobile phase liquid chromatographic system with electrochemical detection, the method was validated with respect to (a) selectivity, (b) accuracy/recovery, (c) precision/reproducibility, (d) sensitivity, (e) stability and (f) ruggedness. The standard curve was linear and ranged from 0.5 to 30 mg/L for each of the three analytes. Above-mentioned performance measures were within acceptable limits described in the Food and Drug Administration’s Guidance for Industry: Bioanalytical Method Validation. The method was validated using blood serum and plasma collected using four common anticoagulants, and also by quantifying the accuracy and sensitivity of MI measured in simulated urine samples recovered from preterm infant diaper systems. The method performs satisfactorily measuring the three most common inositol isomers on 25 μL clinical samples of serum, plasma milk, and/or urine. Similar performance is seen testing larger volume samples of infant formulas and infant formula ingredients. MI, ADS and DCI may be accurately tested in urine samples collected from five different preterm infant diapers if the urine volume is greater than 2–5 mL. PMID:26010453

Ring-oven based preconcentration technique for microanalysis: simultaneous determination of Na, Fe, and Cu in fuel ethanol by laser induced breakdown spectroscopy.

PubMed

Cortez, Juliana; Pasquini, Celio

2013-02-05

The ring-oven technique, originally applied for classical qualitative analysis in the years 1950s to 1970s, is revisited to be used in a simple though highly efficient and green procedure for analyte preconcentration prior to its determination by the microanalytical techniques presently available. The proposed preconcentration technique is based on the dropwise delivery of a small volume of sample to a filter paper substrate, assisted by a flow-injection-like system. The filter paper is maintained in a small circular heated oven (the ring oven). Drops of the sample solution diffuse by capillarity from the center to a circular area of the paper substrate. After the total sample volume has been delivered, a ring with a sharp (c.a. 350 μm) circular contour, of about 2.0 cm diameter, is formed on the paper to contain most of the analytes originally present in the sample volume. Preconcentration coefficients of the analyte can reach 250-fold (on a m/m basis) for a sample volume as small as 600 μL. The proposed system and procedure have been evaluated to concentrate Na, Fe, and Cu in fuel ethanol, followed by simultaneous direct determination of these species in the ring contour, employing the microanalytical technique of laser induced breakdown spectroscopy (LIBS). Detection limits of 0.7, 0.4, and 0.3 μg mL(-1) and mean recoveries of (109 ± 13)%, (92 ± 18)%, and (98 ± 12)%, for Na, Fe, and Cu, respectively, were obtained in fuel ethanol. It is possible to anticipate the application of the technique, coupled to modern microanalytical and multianalyte techniques, to several analytical problems requiring analyte preconcentration and/or sample stabilization.

Simplification and validation of a large volume polyurethane foam sampler for the analysis of persistent hydrophobic compounds in drinking water.

PubMed

Choi, J W; Lee, J H; Moon, B S; Kannan, K

2008-08-01

The use of a large volume polyurethane foam (PUF) sampler was validated for rapid extraction of persistent organic pollutants (POPs), such as polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), in raw water and treated water from drinking water plants. To validate the recovery of target compounds in the sampling process, a (37)Cl-labeled standard was spiked into the 1st PUF plug prior to filtration. An accelerated solvent extraction method, as a pressurized liquid extractor (PLE), was optimized to extract the PUF plug. For sample preparation, tandem column chromatography (TCC) clean-up was used for rapid analysis. The recoveries of labeled compounds in the analytical method were 80-110% (n = 9). The optimized PUF-PLE-TCC method was applied in the analysis of raw water and treated potable water from seven drinking water plants in South Korea. The sample volume used was between 18 and 102 L for raw water at a flow rate of 0.4-2 L min(-1), 95 and 107 L for treated water at a flow rate of 1.5-2.2 L min(-1). Limit of quantitation (LOQ) was a function of sample volume and it decreased with increasing sample volume. The LOQ of PCDD/Fs in raw waters analyzed by this method was 3-11 times lower than that described using large-size disk-type solid phase extraction (SPE) method. The LOQ of PCDD/F congeners in raw water and treated water were 0.022-3.9 ng L(-1) and 0.018-0.74 ng L(-1), respectively. Octachlorinated dibenzo-p-dioxin (OCDD) was found in some raw water samples, while their concentrations were well below the tentative criterion set by the Japanese Environmental Ministry for drinking water. OCDD was below the LOQ in the treated drinking water.

Nickel and vanadium in air particulates at Dhahran (Saudi Arabia) during and after the Kuwait oil fires

NASA Astrophysics Data System (ADS)

Sadiq, M.; Mian, A. A.

Air particulates, both the total suspended (TSP) and inhalable (PM 10, smaller than 10 microns in size), were collected during and after the Kuwait oil fires (from March 1991 to July 1992) using Hi-Vol samplers. These samples were wet-digested at 120°C in an aqua regia and perchloric acids mixture for 3 h. Air particulate samples collected in 1982 at the same location were prepared similarly. Concentrations of nickel and vanadium were determined in the aliquot samples using an inductively coupled argon plasma analyser (ICAP). The monthly mean concentrations of nickel and vanadium, on volume basis, increased rapidly from March to June and decreased sharply during July-August in 1991. The minimum mean concentrations of these elements were found in the particulate samples collected in December 1991 which gradually increased through May 1992. Like 1991, nickel and vanadium concentrations in the air particulates spiked in June and decreased again in July 1992. This distribution pattern of nickel and vanadium concentrations was similar to that of the predominant wind from the north (Kuwait). In general, concentrations of these elements were higher in the air particulates collected during April-July 1991 as compared with those collected in 1992 during the same period. The TSPs contained higher concentrations of nickel and vanadium than those found in the PM 10 samples. However, this trend was reversed when concentrations of nickel and vanadium, on were expressed on particulate weight basis. The monthly mean concentrations of nickel and vanadium, on weight basis, decreased gradually through 1991 and increased slightly from March to July 1992. Concentrations of these elements were significantly higher in the air particulate samples collected in 1991 than those samples collected during 1982 at the same location. The data of this study suggest a contribution of the Kuwait oil fires in elevating nickel and vanadium concentrations in the air particulates at Dhahran during April-July 1991. Concentrations of these elements were largely below their proposed limits in the ambient air (for nickel-50 μg m -3, air; for vanadium—1 μg m -3 air). It is, therefore, anticipated that concentrations of nickel and vanadium in the air particulate samples were not a health concern during Kuwait oil fires at Dhahran, Saudi Arabia.

Microextraction by packed sorbent: an emerging, selective and high-throughput extraction technique in bioanalysis.

PubMed

Pereira, Jorge; Câmara, José S; Colmsjö, Anders; Abdel-Rehim, Mohamed

2014-06-01

Sample preparation is an important analytical step regarding the isolation and concentration of desired components from complex matrices and greatly influences their reliable and accurate analysis and data quality. It is the most labor-intensive and error-prone process in analytical methodology and, therefore, may influence the analytical performance of the target analytes quantification. Many conventional sample preparation methods are relatively complicated, involving time-consuming procedures and requiring large volumes of organic solvents. Recent trends in sample preparation include miniaturization, automation, high-throughput performance, on-line coupling with analytical instruments and low-cost operation through extremely low volume or no solvent consumption. Micro-extraction techniques, such as micro-extraction by packed sorbent (MEPS), have these advantages over the traditional techniques. This paper gives an overview of MEPS technique, including the role of sample preparation in bioanalysis, the MEPS description namely MEPS formats (on- and off-line), sorbents, experimental and protocols, factors that affect the MEPS performance, and the major advantages and limitations of MEPS compared with other sample preparation techniques. We also summarize MEPS recent applications in bioanalysis. Copyright © 2014 John Wiley & Sons, Ltd.

Determination of polycyclic aromatic hydrocarbons in drinking water samples by solid-phase nanoextraction and high-performance liquid chromatography.

PubMed

Wang, Huiyong; Campiglia, Andres D

2008-11-01

A novel alternative is presented for the extraction and preconcentration of polycyclic aromatic hydrocarbons (PAH) from water samples. The new approachwhich we have named solid-phase nanoextraction (SPNE)takes advantage of the strong affinity that exists between PAH and gold nanoparticles. Carefully optimization of experimental parameters has led to a high-performance liquid chromatography method with excellent analytical figures of merit. Its most striking feature correlates to the small volume of water sample (500 microL) for complete PAH analyses. The limits of detection ranged from 0.9 (anthracene) to 58 ng.L (-1) (fluorene). The relative standard deviations at medium calibration concentrations vary from 3.2 (acenaphthene) to 9.1% (naphthalene). The analytical recoveries from tap water samples of the six regulated PAH varied from 83.3 +/- 2.4 (benzo[ k]fluoranthene) to 95.7 +/- 4.1% (benzo[ g,h,i]perylene). The entire extraction procedure consumes less than 100 microL of organic solvents per sample, which makes it environmentally friendly. The small volume of extracting solution makes SPNE a relatively inexpensive extraction approach.

Simultaneous trace multielement determination by ICP-OES after solid phase extraction with modified octadecyl silica gel.

PubMed

Karbasi, Mohamad-Hadi; Jahanparast, Babak; Shamsipur, Mojtaba; Hassan, Jalal

2009-10-15

Multielement simultaneous determination of 35 trace elements in environmental samples was carried out by inductively coupled plasma emission spectrometry (ICP-OES) after preconcentration with octadecyl silicagel, modified with aurin tricarboxylic acid (Aluminon). Optimal experimental conditions including pH of sample solution, sample volume, sample and eluent flow rate, type, concentration and volume of eluent and foreign ions effect were investigated and established. Trace element ions in aqueous solution were quantitatively adsorbed onto octadecyl silicagel modified with aurin tricarboxylic acid at pH 8.0 with a flow rate of 11.0 mL min(-1). The adsorbed element ions were eluted with 3-5 mL of 0.5 mol L(-1) HNO(3) at a flow rate of 10.0 mL min(-1) and analyzed by ICP-OES simultaneously. The proposed method has at least preconcentration factor of 100 in water samples, which results high sensitive detection of ultra-trace and trace analysis. The present methodology gave recoveries better than 70% and RSD less than 16%.

Short term effects of increasing dietary salt concentrations on urine composition in healthy cats.

PubMed

Paßlack, N; Burmeier, H; Brenten, T; Neumann, K; Zentek, J

2014-09-01

High dietary salt (NaCl) concentrations are assumed to be beneficial in preventing the formation of calcium oxalate (CaOx) uroliths in cats, since increased water intake and urine volume have been observed subsequent to intake. In human beings, dietary NaCl restriction is recommended for the prevention of CaOx urolith formation, since high NaCl intake is associated with increased urinary Ca excretion. The aim of the present study was to clarify the role of dietary NaCl in the formation of CaOx uroliths in cats. Eight cats received four diets that differed in Na and Cl concentrations (0.38-1.43% Na and 0.56-2.52% Cl dry matter, DM). Each feeding period consisted of a 21 day adaptation period, followed by a 7 day sampling period for urine collection. Higher dietary NaCl concentrations were associated with increased urine volume and renal Na excretion. Urinary Ca concentration was constant, but renal Ca excretion increased from 0.62 to 1.05 mg/kg bodyweight (BW)/day with higher dietary NaCl concentrations (P ≤ 0.05). Urinary oxalate (Ox), citrate, P and K concentrations decreased when NaCl intake was high (P ≤ 0.05), and urinary pH was low in all groups (6.33-6.45; P > 0.05). Relative supersaturation of CaOx in the urine was unaffected by dietary NaCl concentrations. In conclusion, the present study demonstrated several beneficial effects of high dietary NaCl intake over a relatively short time period. In particular, urinary Ca concentration remained unchanged because of increased urine volume. Decreased urinary Ox concentrations might help to prevent the formation of CaOx uroliths, but this should be verified in future studies in diseased or predisposed cats. Copyright © 2014 Elsevier Ltd. All rights reserved.

Positron lifetime beam for defect studies in thin epitaxial semiconductor structures

NASA Astrophysics Data System (ADS)

Laakso, A.; Saarinen, K.; Hautojärvi, P.

2001-12-01

Positron annihilation spectroscopies are methods for direct identification of vacancy-type defects by measuring positron lifetime and Doppler broadening of annihilation radiation and providing information about open volume, concentration and atoms surrounding the defect. Both these techniques are easily applied to bulk samples. Only the Doppler broadening spectroscopy can be employed in thin epitaxial samples by utilizing low-energy positron beams. Here we describe the positron lifetime beam which will provide us with a method to measure lifetime in thin semiconductor layers.

Preliminary synchrotron analysis of lead in hair from a lead smelter worker

DOE Office of Scientific and Technical Information (OSTI.GOV)

Martin, R.R.; Kempson, I.M.; Naftel, S.J.

2008-06-09

Synchrotron X-ray fluorescence has been used to study the distribution of lead in a hair sample collected from a lead smelter worker. A mathematical model was used to imitate the transverse scan signal based on the analysis volume and concentration profiles. The results suggest that the Pb originates both from ingestion and environmental exposure, however direct deposition from the environment is the more important source of hair lead. The model could apply equally to any other analysis involving a thin cylindrical sample.

Prediction of Protein Aggregation in High Concentration Protein Solutions Utilizing Protein-Protein Interactions Determined by Low Volume Static Light Scattering.

PubMed

Hofmann, Melanie; Winzer, Matthias; Weber, Christian; Gieseler, Henning

2016-06-01

The development of highly concentrated protein formulations is more demanding than for conventional concentrations due to an elevated protein aggregation tendency. Predictive protein-protein interaction parameters, such as the second virial coefficient B22 or the interaction parameter kD, have already been used to predict aggregation tendency and optimize protein formulations. However, these parameters can only be determined in diluted solutions, up to 20 mg/mL. And their validity at high concentrations is currently controversially discussed. This work presents a μ-scale screening approach which has been adapted to early industrial project needs. The procedure is based on static light scattering to directly determine protein-protein interactions at concentrations up to 100 mg/mL. Three different therapeutic molecules were formulated, varying in pH, salt content, and addition of excipients (e.g., sugars, amino acids, polysorbates, or other macromolecules). Validity of the predicted aggregation tendency was confirmed by stability data of selected formulations. Based on the results obtained, the new prediction method is a promising screening tool for fast and easy formulation development of highly concentrated protein solutions, consuming only microliter of sample volumes. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Ultrasonic-energy enhance the ionic liquid-based dual microextraction to preconcentrate the lead in ground and stored rain water samples as compared to conventional shaking method.

PubMed

Nizamani, Sooraj; Kazi, Tasneem G; Afridi, Hassan I

2018-01-01

An efficient preconcentration technique based on ultrasonic-assisted ionic liquid-based dual microextraction (UA-ILDµE) method has been developed to preconcentrate the lead (Pb +2 ) in ground and stored rain water. In the current proposed method, Pb +2 was complexed with a chelating agent (dithizone), whereas an ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate) was used for extraction purpose. The ultrasonic irradiation and electrical shaking system were applied to enhance the dispersion and extraction of Pb +2 complex in aqueous samples. For second phase, dual microextraction (DµE phase), the enriched Pb +2 complex in ionic liquid, extracted back into the acidic aqueous solution and finally determined by flame atomic absorption spectrometry. Some major analytical parameters that influenced the extraction efficiency of developed method, such as pH, concentration of ligand, volume of ionic liquid and samples, time of shaking in thermostatic electrical shaker and ultrasonic bath, effect of back extracting HNO 3 volume, matrix effect, centrifugation time and rate were optimized. At the sample volume of 25mL, the calculated preconcentration factor was 62.2. The limit of detection of proposed procedure for Pb +2 ions was found to be 0.54μgL -1 . The validation of developed method was performed by the analysis of certified sample of water SRM 1643e and standard addition method in a real water sample. The extraction recovery of Pb +2 was enhanced≥2% with shaking time of 80s in ultrasonic bath as compared to used thermostatic electrical shaker, where for optimum recovery up to 10min was required. The developed procedure was successfully used for the enrichment of Pb +2 in ground and stored rain water (surface water) samples of an endemic region of Pakistan. The resulted data indicated that the ground water samples were highly contaminated with Pb +2 , while some of the surface water samples were also have higher values of Pb +2 than permissible limit of WHO. The concentration of Pb +2 in surface and ground water samples was found in the range of 17.5-24.5 and 25.6-99.1μgL - 1 respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Method of freezing living cells and tissues with improved subsequent survival

DOEpatents

Senkan, Selim M.; Hirsch, Gerald P.

1980-01-01

This invention relates to an improved method for freezing red blood cells, ther living cells, or tissues with improved subsequent survival, wherein constant-volume freezing is utilized that results in significantly improved survival compared with constant-pressure freezing; optimization is attainable through the use of different vessel geometries, cooling baths and warming baths, and sample concentrations.

40 CFR 98.344 - Monitoring and QA/QC requirements.

Code of Federal Regulations, 2012 CFR

2012-07-01

... minutes between samples and determine the methane composition of the landfill gas using one of the methods.... ER30OC09.136 Where: CCH4 = Methane concentration in the landfill gas (volume %) for use in Equation HH-4 of... procedures used to ensure the accuracy of the estimates of disposal quantities and, if applicable, gas flow...

40 CFR 98.344 - Monitoring and QA/QC requirements.

Code of Federal Regulations, 2013 CFR

2013-07-01

... minutes between samples and determine the methane composition of the landfill gas using one of the methods.... ER30OC09.136 Where: CCH4 = Methane concentration in the landfill gas (volume %) for use in Equation HH-4 of... procedures used to ensure the accuracy of the estimates of disposal quantities and, if applicable, gas flow...

Detection of low-concentration host mRNA transcripts in Malawian children at risk for environmental enteropathy

USDA-ARS?s Scientific Manuscript database

Transcriptomic analysis of fecal samples is an emerging method for the diagnosis of gastrointestinal pathology because it is noninvasive and requires minute volumes of analyte; however, detection of mRNA in low copy numbers in human stool is challenging. Our objective was to develop a method for det...

A Literature Review of Concentrations and Size Distributions of Ambient Airborne Pb-Containing Particulate Matter

EPA Science Inventory

The final 2008 lead (Pb) national ambient air quality standards (NAAQS) revision maintains Pb in total suspended particulate matter as the indicator. However, the final rule permits the use of low-volume PM₁₀ (particulate matter sampled with a 50% cut-point of 10 μm) F...

The organic pollutant status of rivers in Bosnia and Herzegovina as determined by a combination of active and passive sampling methods.

PubMed

Harman, Christopher; Grung, Merete; Djedjibegovic, Jasmina; Marjanovic, Aleksandra; Fjeld, Eirik; Braaten, Hans Fredrik Veiteberg; Sober, Miroslav; Larssen, Thorjørn; Ranneklev, Sissel Brit

2018-04-15

There is an overall lack of data concerning the pollution status of Bosnia Herzegovina, which is confounded by fragmented national environmental management. The present study aimed to provide some initial data for concentrations of priority substances in two major Bosnian Rivers, using two types of passive sampler (PS) as well as by using high volume water sampling (HVWS). Overall, concentrations of most persistent organic pollutants (POPs), including polychlorinated biphenyls (PCBs) and legacy pesticides, were shown to be low. However, around the town of Doboj on the Bosna River, concentrations of polycyclic aromatic hydrocarbons (PAH) breached European standards for several compounds and reached 67 ng L -1 for freely dissolved concentrations and 250 ng L -1 for total concentrations. In general, contamination was lower in the Neretva River compared to the Bosna, although for brominated diphenyl ethers (PBDEs), results suggested an active source of PBDEs at one location based on the ratio of congeners 47 and 99. Direct comparisons between the different sampling techniques used are not straightforward, but similar patterns of PAH contamination were shown by HVWS and PS in the Bosna River. There are both scientific and practical considerations when choosing which type of sampling technique to apply, and this should be decided based on the goals of each individual study.

A colorimetric probe based on desensitized ionene-stabilized gold nanoparticles for single-step test for sulfate ions.

PubMed

Arkhipova, Viktoriya V; Apyari, Vladimir V; Dmitrienko, Stanislava G

2015-03-15

Desensitized ionene-stabilized gold nanoparticles have been prepared and applied as a colorimetric probe for the single-step test for sulfate ions at the relatively high concentration level. The approach is based on aggregation of the nanoparticles leading to the change in absorption spectra and color of the solution. These nanoparticles are characterized by the decreased sensitivity due to both electrostatic and steric stabilization, which allows for simple, and rapid direct single-step determination of sulfate at the relatively high concentration level in real water samples without sample pretreatment or dilution. Influence of different factors (the time of interaction, pH, the concentrations of sulfate ions and the nanoparticles) on the aggregation and analytical performance of the procedure was investigated. The method allows for the determination of sulfate ions in the mass range of 0.2-0.4 mg with RSD of 5% from the sample volume of less than 2 mL. It has a sharp dependence of the colorimetric response on the concentration of sulfate, which makes it prospective for indicating deviations of the sulfate concentration regarding some declared value chosen within the above range. The time of the analysis is 2 min. The method was applied to the analysis of mineral water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

A population study of urine glycerol concentrations in elite athletes competing in North America.

PubMed

Kelly, Brian N; Madsen, Myke; Sharpe, Ken; Nair, Vinod; Eichner, Daniel

2013-01-01

Glycerol is an endogenous substance that is on the World Anti-Doping Agency's list of prohibited threshold substances due to its potential use as a plasma volume expansion agent. The WADA has set the threshold for urine glycerol, including measurement uncertainty, at 1.3 mg/mL. Glycerol in circulation largely comes from metabolism of triglycerides in order to meet energy requirements and when the renal threshold is eclipsed, glycerol is excreted into urine. In part due to ethnic differences in postprandial triglyceride concentrations, we investigated urine glycerol concentrations in a population of elite athletes competing in North America and compared the results to those of athletes competing in Europe. 959 urine samples from elite athletes competing in North America collected for anti-doping purposes were analyzed for urine glycerol concentrations by a gas chromatography mass-spectrometry method. Samples were divided into groups according to: Timing (in- or out-of-competition), Class (strength, game, or endurance sports) and Gender. 333 (34.7%) samples had undetectable amounts of glycerol (<1 μg/mL). 861 (89.8%) of the samples had glycerol concentrations ≤20 μg/mL. The highest glycerol concentration observed was 652 μg/mL. Analysis of the data finds the effects of each category to be statistically significant. The largest estimate of the 99.9(th) percentile, from the in-competition, female, strength athlete samples, was 1813 μg/mL with a 95% confidence range from 774 to 4251 μg/mL. This suggests a conservative threshold of 4.3 mg/mL, which would result in a reasonable detection window for urine samples collected in-competition for all genders and sport classes. Copyright © 2013 John Wiley & Sons, Ltd.

Recovery of spiked Δ9-tetrahydrocannabinol in oral fluid from polypropylene containers.

PubMed

Molnar, Anna; Lewis, John; Fu, Shanlin

2013-04-10

Oral fluid is currently used by Australian and international law enforcement agencies and employers to detect recent use of cannabis and other drugs of abuse. The main psychoactive constituent of cannabis, Δ(9)-tetrahydrocannabinol (THC), is highly lipophilic and losses occur when in contact with plastic, possibly due to its adsorption onto the plastic surface. This study aims to investigate factors governing the interaction of THC with plastic and search for ways of overcoming such interaction so to improve THC recovery. As polypropylene is one of the most common types of plastic used in collection devices, it was the focus of this study. All experiments were done by preparing neat oral fluid samples spiked with THC in 2-mL polypropylene centrifuge tubes. Samples were transferred with or without prior addition of Triton(®) X-100 (0.25%) to glass tubes containing d3-THC as internal standard and 0.1M phosphate buffer was then added. Samples were extracted by liquid-liquid extraction using hexane/ethyl acetate (9:1, v/v), dried and analysed by gas chromatography-mass spectrometry (GC-MS) after derivatisation. No significant difference was found in terms of THC loss to plastic when the concentration ranged from 25 to 1000 ng/mL in the same volume of oral fluid. Varying the oral fluid volume (0.5-1.5 mL) while keeping THC at a constant concentration showed an upward trend with more loss associated with lower volumes. The use of Triton(®) X-100 significantly decreased the adherence of THC to the plastic tubes and increased the THC transfer (>96%) at all volumes tested. Degradation of THC during storage was also studied over a 4-week period and it was found that azide did not seem to play a significant role in preserving THC in oral fluid. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

Chemical characterization of ambient aerosol collected during the southwest monsoon and intermonsoon seasons over the Arabian Sea: Labile-Fe(II) and other trace metals

NASA Astrophysics Data System (ADS)

Siefert, Ronald L.; Johansen, Anne M.; Hoffmann, Michael R.

1999-02-01

Atmospheric deposition of iron (Fe) to certain regions of the oceans is an important nutrient source of Fe to the biota, and the ability of the biota to uptake Fe is dependent on the speciation of the Fe. Therefore understanding the speciation of Fe in the atmosphere is critical to understanding the role of Fe as a nutrient source in surface ocean waters. Labile ferrous iron (Fe(II)) concentrations as well as total concentrations for Fe and other important trace metals, cations, and anions were determined over the Arabian Sea for two nonconsecutive months during 1995. Ambient aerosol samples were collected during the Indian Ocean intermonsoon and southwest monsoon seasons over the Arabian Sea. Sampling took place aboard the German research vessel Meteor in the months of May (leg M32/3; intermonsoon) and July/August (leg M32/5; southwest monsoon). Both cruise tracks followed the 65th east meridian, traveling for 30 days each (from north to south during leg M32/3 and from south to north during leg M32/5). A high-volume dichotomous virtual impactor with an aerodynamic cutoff size of 3 μm was used to collect the fine and coarse aerosol fractions for metal analysis. A low volume collector was used to collect aerosol samples for anion and cation analysis. The analysis for labile-Fe(II) was done immediately after sample collection to minimize any possible Fe redox reactions which might occur during sample storage. The analytical procedure involved filter extraction in a formate/formic acid buffered solution at pH 4.2 followed by colorimetric quantification of soluble Fe(II). Metals, anions, and cations were analyzed after the cruise. Total atmospheric aqueous-labile-Fe(II) concentrations during the intermonsoon were between 4.75 and <0.4 ng m-3, of which most (>80%) was present in the fine fraction (<3.0 μm). During the southwest monsoon, atmospheric aqueous-labile-Fe(II) concentrations were consistently below the detection limit (<0.34 to <0.089 ng m-3, depending on the volume of air sampled). Air mass back trajectories (5 day, three dimensional) showed that air masses sampled during the southwest monsoon had advected over the open Indian Ocean, while air masses sampled during the intermonsoon had advected over northeast Africa, the Saudi Arabian peninsula, and southern Asia. These calculations were consistent with the results of the statistical analysis performed on the data set which showed that the variance due to crustal species during the intermonsoon samples was greater than the variance due to crustal species during the southwest monsoon. The factor scores for the crustal components were also greater when the back trajectories had advected over the nearby continental masses. Principal component analysis was also performed with the intermonsoon samples where aqueous labile Fe(II) was above the detection limit. Aqueous labile Fe(II) did not correlate well with other species indicating possible atmospheric processing of the iron during advection.

Determination of mercury in agroindustrial samples by flow-injection cold vapor atomic absorption spectrometry using ion exchange and reductive elution.

PubMed

Gomes Neto, J A; Zara, L F; Rocha, J C; Santos, A; Dakuzaku, C S; Nóbrega, J A

2000-03-06

A flow-injection system with a Chelite-S(R) cationic resin packed minicolumn is proposed for the determination of trace levels of mercury in agroindustrial samples by cold vapor atomic absorption spectrometry. Improved sensitivity and selectivity are attained since mercuric ions are on-line concentrated whereas other potential interferents are discarded. With on-line reductive elution procedure, concentrated hydrochloric acid could be replaced by 10% w/v SnCl(2), in 6 M HCl as eluent. The reversed-intermittent stream either carries the atomic mercury to the flow cell in the forward direction or removes the residue from reactor/gas-liquid separator to a discarding flask in the opposite direction. Concentration and volume of reagent, acidity, flow rates, commutation times and potential interfering species were investigated. For 120 s preconcentration time, the proposed system handles about 25 samples h(-1) (50.0-500 ng l(-1)), consuming about 10 ml sample and 5 mg SnCl(2) per determination. The detection limit is 0.8 ng l(-1) and the relative standard deviation (RSD) (n=12) of a 76.7 ng l(-1) sample is about 5%. Results are in agreement with certified value of standard materials at 95% confidence level and good recoveries (97-128%) of spiked samples were found.

Air Quality measurements near the Gulf of Mexico Deep Water Horizon Oil Spill site in July 2010

NASA Astrophysics Data System (ADS)

Schade, G. W.; Rasmussen, R.; Conlee, D.; Seroka, G.; Delao, D.

2010-12-01

Eight whole air samples were acquired within several kilometers of the Deepwater Horizon well head location between 5 and 13 July 2010. A Teflon coated pump was used to pressurize 0.8 L volume stainless steel canisters to approximately 2 bar. Various amounts of oil were visible on the water surface during most sampling times, and some samples were accompanied by strong hydrocarbon smells. The air samples were analyzed over the next two months using high sensitivity GC-FID and GC-MS methods for C1-C30 hydrocarbons and selected hetero-atomic compounds. Highest concentrations reached several ppm for total hydrocarbons, comparable to concentrations in highway road tunnels. None of the samples showed elevated concentrations suggestive of hazardous concentrations, or near OSHA PEL or NIOSH REL levels. Consistent with studies of seawater methane concentrations at different depths, atmospheric methane mixing ratios were close to background abundances at 1.75-1.78 ppm, suggesting that the spill’s methane emissions had not reached the surface at that time. Non-methane hydrocarbons presented a highly complex mixture (100+ species) of dominantly alkanes, as expected. Linear alkanes were detected at elevated mixing ratios from C4 up to C30, and were dominated by nonane (C9). Aromatic hydrocarbons showed a pattern suggestive of a significant retention by seawater of benzene and toluene, the compounds with the highest water solubilities. While benzene was hardly and toluene only slightly elevated, lower solubility compounds such as the xylenes and naphthalene were clearly elevated. Data will be presented relative to an upwind sample taken on 5 July.

Quantitative detection of glucose level based on radiofrequency patch biosensor combined with volume-fixed structures.

PubMed

Qiang, Tian; Wang, Cong; Kim, Nam-Young

2017-12-15

A concept for characterizing a radiofrequency (RF) patch biosensor combined with volume-fixed structures is presented for timely monitoring of an individual's glucose levels based on frequency variation. Two types of patch biosensors-separately integrated with a backside slot (0.53μL) and a front-side tank (0.70μL) structure-were developed to achieve precise and efficient detection while excluding the effects of interference due to the liquidity, shape, and thickness of the tested glucose sample. A glucose test analyte at different concentrations (50-600mg/dL) was dropped into the volume-fixed structures. It fully interacted with the RF patch electromagnetic field, effectively and sensitively changing the resonance frequency and magnitude of the reflection coefficient. Measurement results based on the resonance frequency showed high sensitivity up to 1.13MHz and 1.97MHz per mg/dL, and low detection limits of 26.54mg/dL and 15.22mg/dL, for the two types of patch biosensors, respectively, as well as a short response time of less than 1s. Excellent reusability of the proposed biosensors was verified through three sets of measurements for each individual glucose sample. Regression analysis revealed a good linear correlation between glucose concentrations and the resonance frequency shift. Moreover, to facilitate a multi-parameter-sensitive detection of glucose, the magnitude of the reflection coefficient was also tested, and it showed a good linear correlation with the glucose concentration. Thus, the proposed approach can be adopted for distinguishing glucose solution levels, and it is a potential candidate for early-stage detection of glucose levels in diabetes patients. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparison of spectroscopy technologies for improved monitoring of cell culture processes in miniature bioreactors

PubMed Central

van den Berg, Frans; Racher, Andrew J.; Martin, Elaine B.; Jaques, Colin

2017-01-01

Cell culture process development requires the screening of large numbers of cell lines and process conditions. The development of miniature bioreactor systems has increased the throughput of such studies; however, there are limitations with their use. One important constraint is the limited number of offline samples that can be taken compared to those taken for monitoring cultures in large‐scale bioreactors. The small volume of miniature bioreactor cultures (15 mL) is incompatible with the large sample volume (600 µL) required for bioanalysers routinely used. Spectroscopy technologies may be used to resolve this limitation. The purpose of this study was to compare the use of NIR, Raman, and 2D‐fluorescence to measure multiple analytes simultaneously in volumes suitable for daily monitoring of a miniature bioreactor system. A novel design‐of‐experiment approach is described that utilizes previously analyzed cell culture supernatant to assess metabolite concentrations under various conditions while providing optimal coverage of the desired design space. Multivariate data analysis techniques were used to develop predictive models. Model performance was compared to determine which technology is more suitable for this application. 2D‐fluorescence could more accurately measure ammonium concentration (RMSECV 0.031 g L−1) than Raman and NIR. Raman spectroscopy, however, was more robust at measuring lactate and glucose concentrations (RMSECV 1.11 and 0.92 g L−1, respectively) than the other two techniques. The findings suggest that Raman spectroscopy is more suited for this application than NIR and 2D‐fluorescence. The implementation of Raman spectroscopy increases at‐line measuring capabilities, enabling daily monitoring of key cell culture components within miniature bioreactor cultures. © 2017 American Institute of Chemical Engineers Biotechnol. Prog., 33:337–346, 2017 PMID:28271638

Ultra-trace levels analysis of microcystins and nodularin in surface water by on-line solid-phase extraction with high-performance liquid chromatography tandem mass spectrometry.

PubMed

Balest, Lydia; Murgolo, Sapia; Sciancalepore, Lucia; Montemurro, Patrizia; Abis, Pier Paolo; Pastore, Carlo; Mascolo, Giuseppe

2016-06-01

An on-line solid phase extraction coupled with high-performance liquid chromatography in tandem with mass spectrometry (on-line SPE/HPLC/MS-MS) method for the determination of five microcystins and nodularin in surface waters at submicrogram per liter concentrations has been optimized. Maximum recoveries were achieved by carefully optimizing the extraction sample volume, loading solvent, wash solvent, and pH of the sample. The developed method was also validated according to both UNI EN ISO IEC 17025 and UNICHIM guidelines. Specifically, ten analytical runs were performed at three different concentration levels using a reference mix solution containing the six analytes. The method was applied for monitoring the concentrations of microcystins and nodularin in real surface water during a sampling campaign of 9 months in which the ELISA method was used as standard official method. The results of the two methods were compared showing good agreement when the highest concentration values of MCs were found. Graphical abstract An on-line SPE/HPLC/MS-MS method for the determination of five microcystins and nodularin in surface waters at sub μg L(-1) was optimized and compared with ELISA assay method for real samples.

Measurement and estimated health risks of semivolatile organic compounds (PCBs, PAHs, pesticides, and phthalates) in ambient air at the Hanford Site

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patton, G.W.; Cooper, A.T.; Blanton, M.L.

1997-09-01

Air samples for polychlorinated biphenyls (PCBs), chlorinated pesticides, phthalate plasticizers, and polycyclic aromatic hydrocarbons (PAHs) were collected at three Hanford Site locations (300-Area South Gate, southeast of 200-East Area, and a background location near Rattlesnake Springs). Samples were collected using high-volume air samplers equipped with a glass fiber filter and polyurethane foam plug sampling train. Target compounds were extracted from the sampling trains and analyzed using capillary gas chromatography with either electron capture detection or mass selective detection. Twenty of the 28 PCB congeners analyzed were found above the detection limits, with 8 of the congeners accounting for over 80%more » of the average PCB concentrations. The average sum of all individual PCB congeners ranged from 500-740 pg/m{sup 3}, with little apparent difference between the sampling locations. Twenty of the 25 pesticides analyzed were found above the detection limits, with endosulfan I, endosulfan II, and methoxychlor having the highest average concentrations. With the exception of the endosulfans, all other average pesticide concentrations were below 100 pg/m{sup 3}. There was little apparent difference between the air concentrations of pesticides measured at each location. Sixteen of the 18 PAHs analyzed were found above the detection limit. Phenanthrene, fluoranthene, pyrene, fluorene, chrysene, benzo(b)fluoranthene, and naphthalene were the only PAHs with average concentrations above 100 pg/m{sup 3}. Overall, the 300 Area had higher average PAH concentrations compared to the 200-East Area and the background location at Rattlesnake Springs; however, the air concentrations at the 300-Area also are influenced by sources on the Hanford Site and from nearby communities.« less

Low concentrations of persistent organic pollutants (POPs) in air at Cape Verde.

PubMed

Nøst, Therese Haugdahl; Halse, Anne Karine; Schlabach, Martin; Bäcklund, Are; Eckhardt, Sabine; Breivik, Knut

2018-01-15

Ambient air is a core medium for monitoring of persistent organic pollutants (POPs) under the Stockholm Convention and is used in studies of global transports of POPs and their atmospheric sources and source regions. Still, data based on active air sampling remain scarce in many regions. The primary objectives of this study were to (i) monitor concentrations of selected POPs in air outside West Africa, and (ii) to evaluate potential atmospheric processes and source regions affecting measured concentrations. For this purpose, an active high-volume air sampler was installed on the Cape Verde Atmospheric Observatory at Cape Verde outside the coast of West Africa. Sampling commenced in May 2012 and 43 samples (24h sampling) were collected until June 2013. The samples were analyzed for selected polychlorinated biphenyls (PCBs), polybrominated diphenyl ethers (PBDEs), hexachlorobenzene (HCB) and chlordanes. The concentrations of these POPs at Cape Verde were generally low and comparable to remote sites in the Arctic for several compounds. Seasonal trends varied between compounds and concentrations exhibited strong temperature dependence for chlordanes. Our results indicate net volatilization from the Atlantic Ocean north of Cape Verde as sources of these POPs. Air mass back trajectories demonstrated that air masses measured at Cape Verde were generally transported from the Atlantic Ocean or the North African continent. Overall, the low concentrations in air at Cape Verde were likely explained by absence of major emissions in areas from which the air masses originated combined with depletion during long-range atmospheric transport due to enhanced degradation under tropical conditions (high temperatures and concentrations of hydroxyl radicals). Copyright © 2017 The Author(s). Published by Elsevier B.V. All rights reserved.

Field-based evaluation of semipermeable membrane devices (SPMDs) as passive air samplers of polyaromatic hydrocarbons (PAHs)

USGS Publications Warehouse

Bartkow, M.E.; Huckins, J.N.; Muller, J.F.

2004-01-01

Semipermeable membrane devices (SPMDs) have been used as passive air samplers of semivolatile organic compounds in a range of studies. However, due to a lack of calibration data for polyaromatic hydrocarbons (PAHs), SPMD data have not been used to estimate air concentrations of target PAHs. In this study, SPMDs were deployed for 32 days at two sites in a major metropolitan area in Australia. High-volume active sampling systems (HiVol) were co-deployed at both sites. Using the HiVol air concentration data from one site, SPMD sampling rates were measured for 12 US EPA Priority Pollutant PAHs and then these values were used to determine air concentrations at the second site from SPMD concentrations. Air concentrations were also measured at the second site with co-deployed HiVols to validate the SPMD results. PAHs mostly associated with the vapour phase (Fluorene to Pyrene) dominated both the HiVol and passive air samples. Reproducibility between replicate passive samplers was satisfactory (CV<20%) for the majority of compounds. Sampling rates ranged between 0.6 and 6.1 m3 d-1. SPMD-based air concentrations were calculated at the second site for each compound using these sampling rates and the differences between SPMD-derived air concentrations and those measured using a HiVol were, on average, within a factor of 1.5. The dominant processes for the uptake of PAHs by SPMDs were also assessed. Using the SPMD method described herein, estimates of particulate sorbed airborne PAHs with five rings or greater were within 1.8-fold of HiVol measured values. ?? 2004 Elsevier Ltd. All rights reserved.

Effect of different surgical procedures on the accuracy of prediction of the plasma concentration of fentanyl: comparison between mastectomy and laparoscopic prostatectomy.

PubMed

Fujita, Yoshihito; Yoshizawa, Saya; Hoshika, Maiko; Inoue, Koichi; Matsushita, Shoko; Oka, Hisao; Sobue, Kazuya

2017-01-01

The accuracy of simulation-predicted fentanyl concentration in different types of surgical procedure is not fully understood. We wished to estimate the effect of different types of surgical procedure on the accuracy of such simulations. Fifty patients who had undergone elective mastectomy or laparoscopic prostatectomy (American Society of Anesthesiologists physical status = I-II) were enrolled. Anesthesia was maintained throughout surgery with sevoflurane and a bolus infusion of fentanyl. A maintenance infusion was administered with 8 mL/kg/h Ringer's acetate solution from the start of anesthesia to completion of blood sampling. An infusion to compensate for blood loss was administered (one to two volumes of hydroxyethyl starch). A blood sample was drawn every 30 min during anesthesia.We measured the plasma concentration of fentanyl in 358 samples from 50 patients. The plasma concentration of fentanyl was correlated significantly with the simulated predicted fentanyl concentration ( r  = 0.734, P  < 0.01) but 36.0% of all samples had a difference greater than ±0.5 ng/mL. Approximately 0.3 ng/mL of a fixed bias was shown throughout mastectomy. During laparoscopic prostatectomy, the fixed bias gradually became negative from ≈0.3 to -0.3 ng/mL as the sampling stage proceeded. The predicted concentration of fentanyl was significantly correlated with the plasma concentration of fentanyl ( r  = 0.734). However, there were different patterns of a fixed bias between mastectomy and laparoscopic prostatectomy groups. We should pay attention to this tendency among different surgical procedures. UMIN000005110.

Estimating subsurface water volumes and transit times in Hokkaido river catchments, Japan, using high-accuracy tritium analysis

NASA Astrophysics Data System (ADS)

Gusyev, Maksym; Yamazaki, Yusuke; Morgenstern, Uwe; Stewart, Mike; Kashiwaya, Kazuhisa; Hirai, Yasuyuki; Kuribayashi, Daisuke; Sawano, Hisaya

2015-04-01

The goal of this study is to estimate subsurface water transit times and volumes in headwater catchments of Hokkaido, Japan, using the New Zealand high-accuracy tritium analysis technique. Transit time provides insights into the subsurface water storage and therefore provides a robust and quick approach to quantifying the subsurface groundwater volume. Our method is based on tritium measurements in river water. Tritium is a component of meteoric water, decays with a half-life of 12.32 years, and is inert in the subsurface after the water enters the groundwater system. Therefore, tritium is ideally suited for characterization of the catchment's responses and can provide information on mean water transit times up to 200 years. Only in recent years has it become possible to use tritium for dating of stream and river water, due to the fading impact of the bomb-tritium from thermo-nuclear weapons testing, and due to improved measurement accuracy for the extremely low natural tritium concentrations. Transit time of the water discharge is one of the most crucial parameters for understanding the response of catchments and estimating subsurface water volume. While many tritium transit time studies have been conducted in New Zealand, only a limited number of tritium studies have been conducted in Japan. In addition, the meteorological, orographic and geological conditions of Hokkaido Island are similar to those in parts of New Zealand, allowing for comparison between these regions. In 2014, three field trips were conducted in Hokkaido in June, July and October to sample river water at river gauging stations operated by the Ministry of Land, Infrastructure, Transport and Tourism (MLIT). These stations have altitudes between 36 m and 860 m MSL and drainage areas between 45 and 377 km2. Each sampled point is located upstream of MLIT dams, with hourly measurements of precipitation and river water levels enabling us to distinguish between the snow melt and baseflow contributions to the river discharge. For the June sampling, the tritium and stable isotope results indicate below normal river discharges with a strong contribution of snow melt at some sampling points, and relatively short groundwater transit times. The tritium concentration results are used to interpret mean transit times (MTTs) for each sampling point using a tritium input curve constructed from historical International Atomic Energy Agency and available Japanese data, and subsurface volumes are estimated from the MTTs and measured river discharges.