Hydrocarbon group type determination in jet fuels by high performance liquid chromatography

NASA Technical Reports Server (NTRS)

Antoine, A. C.

1977-01-01

Results are given for the analysis of some jet and diesel fuel samples which were prepared from oil shale and coal syncrudes. Thirty-two samples of varying chemical composition and physical properties were obtained. Hydrocarbon types in these samples were determined by fluorescent indicator adsorption (FIA) analysis, and the results from three laboratories are presented and compared. Recently, rapid high performance liquid chromatography (HPLC) methods have been proposed for hydrocarbon group type analysis, with some suggestion for their use as a replacement of the FIA technique. Two of these methods were used to analyze some of the samples, and these results are also presented and compared. Two samples of petroleum-based Jet A fuel are similarly analyzed.

First European interlaboratory comparison of tetracycline and age determination with red fox teeth following oral rabies vaccination programs.

PubMed

Robardet, Emmanuelle; Demerson, Jean-Michel; Andrieu, Sabrina; Cliquet, Florence

2012-10-01

The first European interlaboratory comparison of tetracycline and age determination with red fox (Vulpes vulpes) tooth samples was organized by the European Union Reference Laboratory for rabies. Performance and procedures implemented by member states were compared. These techniques are widely used to monitor bait uptake in European oral rabies vaccination campaigns. A panel of five red fox half-mandibles comprising one weak positive juvenile sample, two positive adult samples, one negative juvenile sample, and one negative adult sample were sent, along with a technical questionnaire, to 12 laboratories participating on a voluntary basis. The results of only three laboratories (25%) were 100% correct. False-negative results were more frequently seen in weak positive juvenile samples (58%) but were infrequent in positive adult samples (4%), probably due to differences in the ease of reading the two groups of teeth. Four laboratories (44%) had correct results for age determination on all samples. Ages were incorrectly identified in both adult and juvenile samples, with 11 and 17% of discordant results, respectively. Analysis of the technical questionnaires in parallel with test results suggested that all laboratories cutting mandible sections between the canine and first premolar obtained false results. All the laboratories using longitudinal rather than transverse sections and those not using a mounting medium also produced false results. Section thickness appeared to affect the results; no mistakes were found in laboratories using sections <150 μm thick. Factors having a potential impact on the success of laboratories were discussed, and recommendations proposed. Such interlaboratory trials underline the importance of using standardized procedures for biomarker detection in oral rabies vaccination campaigns. Several changes can be made to improve analysis quality and increase the comparability of bait uptake frequencies among member states.

Development of Nomarski microscopy for quantitative determination of surface topography

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

Hartman, J. S.; Gordon, R. L.; Lessor, D. L.

1979-01-01

The use of Nomarski differential interference contrast (DIC) microscopy has been extended to provide nondestructive, quantitative analysis of a sample's surface topography. Theoretical modeling has determined the dependence of the image intensity on the microscope's optical components, the sample's optical properties, and the sample's surface orientation relative to the microscope. Results include expressions to allow the inversion of image intensity data to determine sample surface slopes. A commercial Nomarski system has been modified and characterized to allow the evaluation of the optical model. Data have been recorded with smooth, planar samples that verify the theoretical predictions.

Selected problems with boron determination in water treatment processes. Part I: comparison of the reference methods for ICP-MS and ICP-OES determinations.

PubMed

Kmiecik, Ewa; Tomaszewska, Barbara; Wątor, Katarzyna; Bodzek, Michał

2016-06-01

The aim of the study was to compare the two reference methods for the determination of boron in water samples and further assess the impact of the method of preparation of samples for analysis on the results obtained. Samples were collected during different desalination processes, ultrafiltration and the double reverse osmosis system, connected in series. From each point, samples were prepared in four different ways: the first was filtered (through a membrane filter of 0.45 μm) and acidified (using 1 mL ultrapure nitric acid for each 100 mL of samples) (FA), the second was unfiltered and not acidified (UFNA), the third was filtered but not acidified (FNA), and finally, the fourth was unfiltered but acidified (UFA). All samples were analysed using two analytical methods: inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES). The results obtained were compared and correlated, and the differences between them were studied. The results show that there are statistically significant differences between the concentrations obtained using the ICP-MS and ICP-OES techniques regardless of the methods of sampling preparation (sample filtration and preservation). Finally, both the ICP-MS and ICP-OES methods can be used for determination of the boron concentration in water. The differences in the boron concentrations obtained using these two methods can be caused by several high-level concentrations in selected whole-water digestates and some matrix effects. Higher concentrations of iron (from 1 to 20 mg/L) than chromium (0.02-1 mg/L) in the samples analysed can influence boron determination. When iron concentrations are high, we can observe the emission spectrum as a double joined and overlapping peak.

The influence of freezer storage of urine samples on the BONN-Risk-Index for calcium oxalate crystallization.

PubMed

Laube, Norbert; Zimmermann, Diana J

2004-01-01

This study was performed to quantify the effect of a 1-week freezer storage of urine on its calcium oxalate crystallization risk. Calcium oxalate is the most common urinary stone material observed in urolithiasis patients in western and affluent countries. The BONN-Risk-Index of calcium oxalate crystallization risk in human urine is determined from a crystallization experiment performed on untreated native urine samples. We tested the influence of a 1-week freezing on the BONN-Risk-Index value as well as the effect of the sample freezing on the urinary osmolality. In vitro crystallization experiments in 49 native urine samples from stone-forming and non-stone forming individuals were performed in order to determine their calcium oxalate crystallization risk according to the BONN-Risk-Index approach. Comparison of the results derived from original sample investigations with those obtained from the thawed aliquots by statistical evaluation shows that i) no significant deviation from linearity between both results exists and ii) both results are identical by statistical means. This is valid for both, the BONN-Risk-Index and the osmolality data. The differences in the BONN-Risk-Index results of both procedures of BONN-Risk-Index determination, however, exceed the clinically acceptable difference. Thus, determination of the urinary calcium oxalate crystallization risk from thawed urine samples cannot be recommended.

Optimization of microwave digestion for mercury determination in marine biological samples by cold vapour atomic absorption spectrometry.

PubMed

Cardellicchio, Nicola; Di Leo, Antonella; Giandomenico, Santina; Santoro, Stefania

2006-01-01

Optimization of acid digestion method for mercury determination in marine biological samples (dolphin liver, fish and mussel tissues) using a closed vessel microwave sample preparation is presented. Five digestion procedures with different acid mixtures were investigated: the best results were obtained when the microwave-assisted digestion was based on sample dissolution with HNO3-H2SO4-K2Cr2O7 mixture. A comparison between microwave digestion and conventional reflux digestion shows there are considerable losses of mercury in the open digestion system. The microwave digestion method has been tested satisfactorily using two certified reference materials. Analytical results show a good agreement with certified values. The microwave digestion proved to be a reliable and rapid method for decomposition of biological samples in mercury determination.

The determination of the energy values and the composition analysis of M-16 rifle black powders

NASA Astrophysics Data System (ADS)

Satee, R.; Dararutana, P.; Phutdhawong, W.

2017-09-01

The determination of the energy values, specifically the heat of combustion of various M-16 black powders was the important part of the bullet efficiency investigations. The calorimetric bomb is commonly used for these determinations. Four M-16 black powders from the different sources were used as samples for this research. It was found that, after using calorimetric bomb technique, the gross heating value in Joules/g of sample S1-S4 were 10,647, 10,416, 5,281 and 3,878 respectively. The chemical compositions of carbon (C), hydrogen (H), nitrogen (N) and sulfer (S) have also been determined. The results indicated that carbon and nitrogen compositions of sample S1 shown the highest values and provided little differences with sample S2 while sample S3 and S4 shown the lowest carbon and nitrogen percentage composition. The hydrogen composition of all samples was equally valued, however, only sample 3 and 4 displayed sulfur values while no sulfur values were detected from sample 1 and 2. From these results, the heat values and chemical composition of M-16 black powders were characterized their sources and the energy values might be estimated from the amount of carbon and nitrogen in the black powders. Thus, it would be possible to use this determination analysis in the forensic investigation.

Quantitative Real-Time Legionella PCR for Environmental Water Samples: Data Interpretation

PubMed Central

Joly, Philippe; Falconnet, Pierre-Alain; André, Janine; Weill, Nicole; Reyrolle, Monique; Vandenesch, François; Maurin, Max; Etienne, Jerome; Jarraud, Sophie

2006-01-01

Quantitative Legionella PCRs targeting the 16S rRNA gene (specific for the genus Legionella) and the mip gene (specific for the species Legionella pneumophila) were applied to a total of 223 hot water system samples (131 in one laboratory and 92 in another laboratory) and 37 cooling tower samples (all in the same laboratory). The PCR results were compared with those of conventional culture. 16S rRNA gene PCR results were nonquantifiable for 2.8% of cooling tower samples and up to 39.1% of hot water system samples, and this was highly predictive of Legionella CFU counts below 250/liter. PCR cutoff values for identifying hot water system samples containing >103 CFU/liter legionellae were determined separately in each laboratory. The cutoffs differed widely between the laboratories and had sensitivities from 87.7 to 92.9% and specificities from 77.3 to 96.5%. The best specificity was obtained with mip PCR. PCR cutoffs could not be determined for cooling tower samples, as the results were highly variable and often high for culture-negative samples. Thus, quantitative Legionella PCR appears to be applicable to samples from hot water systems, but the positivity cutoff has to be determined in each laboratory. PMID:16597985

[Determination of ethylene glycol in biological fluids--propylene glycol interferences].

PubMed

Gomółka, Ewa; Cudzich-Czop, Sylwia; Sulka, Adrianna

2013-01-01

Many laboratories in Poland do not use gas chromatography (GC) method for determination of ethylene glycol (EG) and methanol in blood of poisoned patients, they use non specific spectrophotometry methods. One of the interfering substances is propylene glycol (PG)--compound present in many medical and cosmetic products: drops, air freshens, disinfectants, electronic cigarettes and others. In Laboratory of Analytical Toxicology and Drug Monitoring in Krakow determination of EG is made by GC method. The method enables to distinguish and make resolution of (EG) and (PG) in biological samples. In the years 2011-2012 in several serum samples from diagnosed patients PG was present in concentration from several to higher than 100 mg/dL. The aim of the study was to estimate PG interferences of serum EG determination by spectrophotometry method. Serum samples containing PG and EG were used in the study. The samples were analyzed by two methods: GC and spectrophotometry. Results of serum samples spiked with PG with no EG analysed by spectrophotometry method were improper ("false positive"). The results were correlated to PG concentration in samples. Calculated cross-reactivity of PG in the method was 42%. Positive results of EG measured by spectrophotometry method must be confirmed by reference GC method. Spectrophotometry method shouldn't be used for diagnostics and monitoring of patients poisoned by EG.

Evaluation of trace elements in lung samples from coal miners using neutron activation analysis.

PubMed

Saiki, M; Saldiva, P H; Alice, S H

1999-01-01

In this study, instrumental neutron activation analysis was applied to the determination of Sc, La, Ce, Nd, Sm, Eu, Tb, Yb, Lu, Hf, Th, and U in lung samples from miners working in coal mines located in the state of Santa Catarina, Brazil. These results were compared to those from a control group constituted of healthy individuals. The results showed that the elements determined exhibit considerable intersubject variability within a single group of individuals and the mean values of concentrations in miners' lungs were higher than those of normal individuals. Lung samples presented U concentrations varying from 11 to 890 micrograms/kg. Therefore, for some samples, the contribution of the uranium fission products in the analysis of La, Ce, Nd, and Sm was considered by determining the interference correction factors. The accuracy of the results was evaluated by analyzing certified reference materials.

External quality-assurance results for the National Atmospheric Deposition Program/National Trends Network during 1991

USGS Publications Warehouse

Nilles, M.A.; Gordon, J.D.; Schroder, L.J.; Paulin, C.E.

1995-01-01

The U.S. Geological Survey used four programs in 1991 to provide external quality assurance for the National Atmospheric Deposition Program/National Trends Network (NADP/NTN). An intersite-comparison program was used to evaluate onsite pH and specific-conductance determinations. The effects of routine sample handling, processing, and shipping of wet-deposition samples on analyte determinations and an estimated precision of analyte values and concentrations were evaluated in the blind-audit program. Differences between analytical results and an estimate of the analytical precision of four laboratories routinely measuring wet deposition were determined by an interlaboratory-comparison program. Overall precision estimates for the precipitation-monitoring system were determined for selected sites by a collocated-sampler program. Results of the intersite-comparison program indicated that 93 and 86 percent of the site operators met the NADP/NTN accuracy goal for pH determinations during the two intersite-comparison studies completed during 1991. The results also indicated that 96 and 97 percent of the site operators met the NADP/NTN accuracy goal for specific-conductance determinations during the two 1991 studies. The effects of routine sample handling, processing, and shipping, determined in the blind-audit program indicated significant positive bias (a=.O 1) for calcium, magnesium, sodium, potassium, chloride, nitrate, and sulfate. Significant negative bias (or=.01) was determined for hydrogen ion and specific conductance. Only ammonium determinations were not biased. A Kruskal-Wallis test indicated that there were no significant (*3t=.01) differences in analytical results from the four laboratories participating in the interlaboratory-comparison program. Results from the collocated-sampler program indicated the median relative error for cation concentration and deposition exceeded eight percent at most sites, whereas the median relative error for sample volume, sulfate, and nitrate concentration at all sites was less than four percent. The median relative error for hydrogen ion concentration and deposition ranged from 4.6 to 18.3 percent at the four sites and as indicated in previous years of the study, was inversely proportional to the acidity of the precipitation at a given site. Overall, collocated-sampling error typically was five times that of laboratory error estimates for most analytes.

Photoacoustic spectroscopy and thermal relaxation method to evaluate corn moisture content

NASA Astrophysics Data System (ADS)

Pedrochi, F.; Medina, A. N.; Bento, A. C.; Baesso, M. L.; Luz, M. L. S.; Dalpasquale, V. A.

2005-06-01

In this study, samples of popcorn with different degrees of moisture were analyzed. The optical absorption bands at the mid infrared were measured using photoacoustic spectroscopy and were correlated to the sample moisture. The results were in agreement with moisture data determined by the well known reference method, the Karl Fischer. In addition, the thermal relaxation method was used to determine the sample specific heat as a function of the moisture content. The results were also in agreement with the two mentioned methods.

Simultaneous determination of V, Ni and Fe in fuel fly ash using solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry.

PubMed

Cárdenas Valdivia, A; Vereda Alonso, E; López Guerrero, M M; Gonzalez-Rodriguez, J; Cano Pavón, J M; García de Torres, A

2018-03-01

A green and simple method has been proposed in this work for the simultaneous determination of V, Ni and Fe in fuel ash samples by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GFAAS). The application of fast programs in combination with direct solid sampling allows eliminating pretreatment steps, involving minimal manipulation of sample. Iridium treated platforms were applied throughout the present study, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9931. The concentrations found in the fuel ash samples analysed ranged from 0.66% to 4.2% for V, 0.23-0.7% for Ni and 0.10-0.60% for Fe. Precision (%RSD) were 5.2%, 10.0% and 9.8% for V, Ni and Fe, respectively, obtained as the average of the %RSD of six replicates of each fuel ash sample. The optimum conditions established were applied to the determination of the target analytes in fuel ash samples. In order to test the accuracy and applicability of the proposed method in the analysis of samples, five ash samples from the combustion of fuel in power stations, were analysed. The method accuracy was evaluated by comparing the results obtained using the proposed method with the results obtained by ICP OES previous acid digestion. The results showed good agreement between them. The goal of this work has been to develop a fast and simple methodology that permits the use of aqueous standards for straightforward calibration and the simultaneous determination of V, Ni and Fe in fuel ash samples by direct SS HR CS GFAAS. Copyright © 2017 Elsevier B.V. All rights reserved.

[Free crystalline silica: a comparison of methods for its determination in total dust].

PubMed

Maciejewska, Aleksandra; Szadkowska-Stańczyk, Irena; Kondratowicz, Grzegorz

2005-01-01

The major objective of the study was to compare and investigate the usefulness of quantitative analyses of free crystalline silica (FCS) in the assessment of dust exposure in samples of total dust of varied composition, using three methods: chemical method in common use in Poland; infrared spectrometry; and x-ray powder diffraction. Mineral composition and FCS contents were investigated in 9 laboratory samples of raw materials, materials, and industrial wastes, containing from about 2 to over 80% of crystalline silica and reduced to particles of size corresponding with that of total dust. Sample components were identified using XRD and FT-IR methods. Ten independent determinations of FCS with each of the three study methods were performed in dust samples. An analysis of linear correlation was applied to investigate interrelationship between mean FCS determinations. In analyzed dust samples, along with silica dust there were numerous minerals interfering with silica during the quantitative analysis. Comparison of mean results of FCS determinations showed that the results obtained using the FT-IR method were by 12-13% lower than those obtained with two other methods. However, the differences observed were within the limits of changeability of results associated with their precision and dependence on reference materials used. Assessment of occupational exposure to dusts containing crystalline silica can be performed on the basis of quantitative analysis of FCS in total dusts using each of the compared methods. The FT-IR method is most appropriate for the FCS determination in samples of small amount of silica or collected at low dust concentrations; the XRD method for the analysis of multicomponent samples; and the chemical method in the case of medium and high FCS contents in samples or high concentrations of dusts in the work environment.

[Standard sample preparation method for quick determination of trace elements in plastic].

PubMed

Yao, Wen-Qing; Zong, Rui-Long; Zhu, Yong-Fa

2011-08-01

Reference sample was prepared by masterbatch method, containing heavy metals with known concentration of electronic information products (plastic), the repeatability and precision were determined, and reference sample preparation procedures were established. X-Ray fluorescence spectroscopy (XRF) analysis method was used to determine the repeatability and uncertainty in the analysis of the sample of heavy metals and bromine element. The working curve and the metrical methods for the reference sample were carried out. The results showed that the use of the method in the 200-2000 mg x kg(-1) concentration range for Hg, Pb, Cr and Br elements, and in the 20-200 mg x kg(-1) range for Cd elements, exhibited a very good linear relationship, and the repeatability of analysis methods for six times is good. In testing the circuit board ICB288G and ICB288 from the Mitsubishi Heavy Industry Company, results agreed with the recommended values.

Correlation between viral loads of cytomegalovirus in blood and bronchoalveolar lavage specimens from lung transplant recipients determined by histology and immunohistochemistry.

PubMed

Chemaly, Roy F; Yen-Lieberman, Belinda; Castilla, Elias A; Reilly, Amy; Arrigain, Susana; Farver, Carol; Avery, Robin K; Gordon, Steven M; Procop, Gary W

2004-05-01

Cytomegalovirus (CMV) is an important pathogen in lung transplant recipients. Early detection of CMV end-organ disease should help with treatment management. We determined the CMV viral load by hybrid capture in bronchoalveolar lavage (BAL) fluid samples from patients who had undergone lung transplantation. For 39 of these samples (from 25 patients), corresponding transbronchial biopsy samples were available for CMV immunohistochemistry (IHC). The CMV IHC results were interpreted and categorized as positive or negative, and the positive results were subcategorized as typical if cells with both significant nuclear enlargement or Cowdry A-type inclusions and positive staining were present or as atypical if definitive nuclear staining was seen but significant nuclear enlargement was not. Diagnostic CMV viral inclusions were reported in the anatomic diagnosis, based on hematoxylin-eosin staining alone, for three (8%) of the biopsy samples. CMV was detected by IHC in 13 (33%) samples (5 typical, 8 atypical). The median CMV viral load in BAL samples was 0 copies/ml for BAL samples from patients with IHC-negative biopsy samples; 47,678 copies/ml for BAL samples from patients with biopsy samples with positive, atypical staining; and 1,548,827 copies/ml for BAL samples from patients with biopsy samples with positive, typical staining (P < 0.001). Compared to routine pathology of biopsy samples, the use of IHC increased the diagnostic yield of CMV. Also, the CMV viral load in BAL fluid samples increased along with immunoreactivity from negative to positive, atypical staining to positive, typical staining. The CMV viral load determined with the end-organ sample, the BAL fluid sample, was higher than the corresponding viral load determined with blood. Both IHC and determination of the CMV viral load in BAL samples may be useful for the detection of individuals at risk for the development of fulminant invasive CMV disease.

Age determination of bottled Chinese rice wine by VIS-NIR spectroscopy

NASA Astrophysics Data System (ADS)

Yu, Haiyan; Lin, Tao; Ying, Yibin; Pan, Xingxiang

2006-10-01

The feasibility of non-invasive visible and near infrared (VIS-NIR) spectroscopy for determining wine age (1, 2, 3, 4, and 5 years) of Chinese rice wine was investigated. Samples of Chinese rice wine were analyzed in 600 mL square brown glass bottles with side length of approximately 64 mm at room temperature. VIS-NIR spectra of 100 bottled Chinese rice wine samples were collected in transmission mode in the wavelength range of 350-1200 nm by a fiber spectrometer system. Discriminant models were developed based on discriminant analysis (DA) together with raw, first and second derivative spectra. The concentration of alcoholic degree, total acid, and °Brix was determined to validate the NIR results. The calibration result for raw spectra was better than that for first and second derivative spectra. The percentage of samples correctly classified for raw spectra was 98%. For 1-, 2-, and 3-year-old sample groups, the sample were all correctly classified, and for 4- and 5-year-old sample groups, the percentage of samples correctly classified was 92.9%, respectively. In validation analysis, the percentage of samples correctly classified was 100%. The results demonstrated that VIS-NIR spectroscopic technique could be used as a non-invasive, rapid and reliable method for predicting wine age of bottled Chinese rice wine.

Detection of Cytomegalovirus (CMV) DNA in EDTA Whole-Blood Samples: Evaluation of the Quantitative artus CMV LightCycler PCR Kit in Conjunction with Automated Sample Preparation▿

PubMed Central

Michelin, Birgit D. A.; Hadžisejdić, Ita; Bozic, Michael; Grahovac, Maja; Hess, Markus; Grahovac, Blaženka; Marth, Egon; Kessler, Harald H.

2008-01-01

Whole blood has been found to be a reliable matrix for the detection and quantitation of cytomegalovirus (CMV) DNA. In this study, the performance of the artus CMV LightCycler (LC) PCR kit in conjunction with automated sample preparation on a BioRobot EZ1 workstation was evaluated. The accuracy, linearity, analytical sensitivity, and inter- and intra-assay variations were determined. A total of 102 clinical EDTA whole-blood samples were investigated, and results were compared with those obtained with the in vitro diagnostics (IVD)/Conformité Européene (CE)-labeled CMV HHV6,7,8 R-gene quantification kit. When the accuracy of the new kit was tested, seven of eight results were found to be within ±0.5 log10 unit of the expected panel results. Determination of linearity resulted in a quasilinear curve over more than 5 log units. The lower limit of detection of the assay was determined to be 139 copies/ml in EDTA whole blood. The interassay variation ranged from 15 to 58%, and the intra-assay variation ranged from 7 to 35%. When clinical samples were tested and the results were compared with those of the routinely used IVD/CE-labeled assay, 53 samples tested positive and 13 samples tested negative by both of the assays. One sample was found to be positive with the artus CMV LC PCR kit only, and 35 samples tested positive with the routinely used assay only. The majority of discrepant results were found with low-titer samples. In conclusion, use of the artus CMV LC PCR kit in conjunction with automated sample preparation on the BioRobot EZ1 workstation may be suitable for the detection and quantitation of CMV DNA in EDTA whole blood in the routine low-throughput laboratory; however, low-positive results may be missed by this assay. PMID:18272703

Detection of cytomegalovirus (CMV) DNA in EDTA whole-blood samples: evaluation of the quantitative artus CMV LightCycler PCR kit in conjunction with automated sample preparation.

PubMed

Michelin, Birgit D A; Hadzisejdic, Ita; Bozic, Michael; Grahovac, Maja; Hess, Markus; Grahovac, Blazenka; Marth, Egon; Kessler, Harald H

2008-04-01

Whole blood has been found to be a reliable matrix for the detection and quantitation of cytomegalovirus (CMV) DNA. In this study, the performance of the artus CMV LightCycler (LC) PCR kit in conjunction with automated sample preparation on a BioRobot EZ1 workstation was evaluated. The accuracy, linearity, analytical sensitivity, and inter- and intra-assay variations were determined. A total of 102 clinical EDTA whole-blood samples were investigated, and results were compared with those obtained with the in vitro diagnostics (IVD)/Conformité Européene (CE)-labeled CMV HHV6,7,8 R-gene quantification kit. When the accuracy of the new kit was tested, seven of eight results were found to be within +/-0.5 log(10) unit of the expected panel results. Determination of linearity resulted in a quasilinear curve over more than 5 log units. The lower limit of detection of the assay was determined to be 139 copies/ml in EDTA whole blood. The interassay variation ranged from 15 to 58%, and the intra-assay variation ranged from 7 to 35%. When clinical samples were tested and the results were compared with those of the routinely used IVD/CE-labeled assay, 53 samples tested positive and 13 samples tested negative by both of the assays. One sample was found to be positive with the artus CMV LC PCR kit only, and 35 samples tested positive with the routinely used assay only. The majority of discrepant results were found with low-titer samples. In conclusion, use of the artus CMV LC PCR kit in conjunction with automated sample preparation on the BioRobot EZ1 workstation may be suitable for the detection and quantitation of CMV DNA in EDTA whole blood in the routine low-throughput laboratory; however, low-positive results may be missed by this assay.

Use of slurry sampling for the direct determination of zinc in yogurt by high resolution-continuum source flame atomic absorption spectrometry.

PubMed

Brandao, Geovani C; de Jesus, Raildo M; da Silva, Erik G P; Ferreira, Sergio L C

2010-06-15

This paper presents an analytical procedure for the direct determination of zinc in yogurt employing sampling slurry and high resolution-continuum source flame atomic absorption spectrometry (HR-CS FAAS). The step optimization established the experimental conditions of: 2.0molL(-1) hydrochloric acid, a sonication time of 20min and a sample mass of 1.0g for a slurry volume of 25mL. This method allows the determination of zinc with a limit of quantification of 0.32microgg(-1). The precision expressed as relative standard deviation (RSD) were 0.82 and 2.08% for yogurt samples containing zinc concentrations of 4.85 and 2.49microgg(-1), respectively. The accuracy was confirmed by the analysis of a certified reference material of non-fat milk powder furnished by the National Institute of Standard and Technology. The proposed method was applied for the determination of zinc in seven yogurt samples. The zinc content was varied from 2.19 to 4.85microgg(-1). These results agreed with those reported in the literature. The samples were also analyzed after acid digestion and zinc determination by FAAS. No statistical difference was observed between the results obtained by both of the procedures performed.

Evaluation of nutrient quality-assurance data for Alexanders and Mount Rock Spring basins, Cumberland County, Pennsylvania

USGS Publications Warehouse

Witt, E. C.; Hippe, D.J.; Giovannitti, R.M.

1992-01-01

A total of 304 nutrient samples were collected from May 1990 through September 1991 to determine concentrations and loads of nutrients in water discharged from two spring basins in Cumberland County, Pa. Fifty-four percent of these nutrient samples were for the evaluation of (1) laboratory consistency, (2) container and preservative cleanliness, (3) maintenance of analyte representativeness as affected by three different preservation methods, and (4) comparison of analyte results with the "Most Probable Value" for Standard Reference Water Samples. Results of 37 duplicate analyses indicate that the Pennsylvania Department of Environmental Resources, Bureau of Laboratories (principal laboratory) remained within its ±10 percent goal for all but one analyte. Results of the blank analysis show that the sampling containers did not compromise the water quality. However, mercuric-chloride-preservation blanks apparently contained measurable ammonium in four of five samples and ammonium plus organic nitrogen in two of five samples. Interlaboratory results indicate substantial differences in the determination of nitrate and ammonium plus organic nitrogen between the principal laboratory and the U.S. Geological Survey National Water-Quality Laboratory. In comparison with the U.S. Environmental Protection Agency Quality-Control Samples, the principal laboratory was sufficiently accurate in its determination of nutrient anafytes. Analysis of replicate samples indicated that sulfuric-acid preservative best maintained the representativeness of the anafytes nitrate and ammonium plus organic nitrogen, whereas, mercuric chloride best maintained the representativeness of orthophosphate. Comparison of nutrient analyte determinations with the Most Probable Value for each preservation method shows that two of five analytes with no chemical preservative compare well, three of five with mercuric-chloride preservative compare well, and three of five with sulfuricacid preservative compare well.

Methods for determining soluble and insoluble Cr III and Cr VI compounds in welding fumes.

PubMed

Matczak, W; Chmielnicka, J

1989-01-01

An analytical procedure for simultaneous determination of soluble and insoluble Cr III and Cr VI compounds in welding fumes has been proposed. In the welding fume samples collected on a membrane filter, total chromium was determined with atomic absorption spectrophotometry (AAS). Glass filters with collected samples were divided into two parts. In one part of the sample, soluble and insoluble chromium was determined by means of AAS. The separation of soluble chromium III and VI was carried out on diphenylcarbazide resin. In the second part of the sample total chromium VI was determined by means of the colorimetric method with s-diphenylcarbazide. The difference in the results of these determinations allowed the calculation of the content of total Cr III, Cr III insolub. and Cr VI insolub. The results of determining chromium compounds in welding fumes samples collected in the welder's breathing zone and in experimental chambers are also presented in this paper. The content of total chromium in the fumes determined by AAS (from a membrane filtr) and that calculated from the sum of soluble and insoluble chromium (from a glass filter) were concordant and within the limits of the admissible error for the method. Total chromium content in welding fume samples collected individually was found to range from 2.4-4.2%. The percentage of particular chromium compounds as compared to total chromium (100%) amounted: total Cr III--34%, total Cr VI--66%, soluble chromium--66% and in this Cr III--20% and Cr VI--43%, insoluble chromium--34% and in this: Cr III--14% and Cr VI--20%.

Detection and quantification system for monitoring instruments

DOEpatents

Dzenitis, John M [Danville, CA; Hertzog, Claudia K [Houston, TX; Makarewicz, Anthony J [Livermore, CA; Henderer, Bruce D [Livermore, CA; Riot, Vincent J [Oakland, CA

2008-08-12

A method of detecting real events by obtaining a set of recent signal results, calculating measures of the noise or variation based on the set of recent signal results, calculating an expected baseline value based on the set of recent signal results, determining sample deviation, calculating an allowable deviation by multiplying the sample deviation by a threshold factor, setting an alarm threshold from the baseline value plus or minus the allowable deviation, and determining whether the signal results exceed the alarm threshold.

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

Adams, Wade C.

Oak Ridge Institute for Science and Education (ORISE) personnel visited the United Nuclear Corporation (UNC) Naval Products site on three separate occasions during the months of October and November 2011. The purpose of these visits was to conduct confirmatory surveys of soils associated with the Argyle Street sewer line that was being removed. Soil samples were collected from six different, judgmentally determined locations in the Argyle Street sewer trench. In addition to the six soil samples collected by ORISE, four replicate soil samples were collected by Cabrera Services, Inc. (CSI) for analysis by the ORISE laboratory. Replicate samples S0010 andmore » S0011 were final status survey (FSS) bias samples; S0012 was an FSS systematic sample; and S0015 was a waste characterization sample. Six soil samples were also collected for background determination. Uranium-235 and uranium-238 concentrations were determined via gamma spectroscopy; the spectra were also reviewed for other identifiable photopeaks. Radionuclide concentrations for these soil samples are provided. In addition to the replicate samples and the samples collected by ORISE, CSI submitted three soil samples for inter-laboratory comparison analyses. One sample was from the background reference area, one was from waste characterization efforts (material inside the sewer line), and one was a FSS sample. The inter-laboratory comparison analyses results between ORISE and CSI were in agreement, except for one sample collected in the reference area. Smear results For Argyle Street sewer pipes are tabulated.« less

Rapid determination of 237Np in soil samples by multi-collector inductively-coupled plasma mass spectrometry and gamma spectrometry.

PubMed

Yi, Xiaowei; Shi, Yanmei; Xu, Jiang; He, Xiaobing; Zhang, Haitao; Lin, Jianfeng

A radiochemical procedure is developed for the determination of 237 Np in soil with multi-collector inductively-coupled plasma mass spectrometry (MC-ICP-MS) and gamma-spectrometry. 239 Np (milked from 243 Am) was used as an isotopic tracer for chemical yield determination. The neptunium in the soil is separated by thenoyl-trifluoracetone extraction from 1 M HNO 3 solution after reducing Np to Np(IV) with ferrous sulfamate, and then purified with Dowex 1 × 2 anion exchange resin. 239 Np in the resulting solution is measured with gamma-spectrometry for chemical yield determination while the 237 Np is measured with MC-ICP-MS. Measurement results for soil samples are presented together with those for two reference samples. By comparing the determined value with the reference value of the 237 Np activity concentration, the feasibility of the procedure was validated.

Determination of Minimum Training Sample Size for Microarray-Based Cancer Outcome Prediction–An Empirical Assessment

PubMed Central

Cheng, Ningtao; Wu, Leihong; Cheng, Yiyu

2013-01-01

The promise of microarray technology in providing prediction classifiers for cancer outcome estimation has been confirmed by a number of demonstrable successes. However, the reliability of prediction results relies heavily on the accuracy of statistical parameters involved in classifiers. It cannot be reliably estimated with only a small number of training samples. Therefore, it is of vital importance to determine the minimum number of training samples and to ensure the clinical value of microarrays in cancer outcome prediction. We evaluated the impact of training sample size on model performance extensively based on 3 large-scale cancer microarray datasets provided by the second phase of MicroArray Quality Control project (MAQC-II). An SSNR-based (scale of signal-to-noise ratio) protocol was proposed in this study for minimum training sample size determination. External validation results based on another 3 cancer datasets confirmed that the SSNR-based approach could not only determine the minimum number of training samples efficiently, but also provide a valuable strategy for estimating the underlying performance of classifiers in advance. Once translated into clinical routine applications, the SSNR-based protocol would provide great convenience in microarray-based cancer outcome prediction in improving classifier reliability. PMID:23861920

Recommendations for representative ballast water sampling

NASA Astrophysics Data System (ADS)

Gollasch, Stephan; David, Matej

2017-05-01

Until now, the purpose of ballast water sampling studies was predominantly limited to general scientific interest to determine the variety of species arriving in ballast water in a recipient port. Knowing the variety of species arriving in ballast water also contributes to the assessment of relative species introduction vector importance. Further, some sampling campaigns addressed awareness raising or the determination of organism numbers per water volume to evaluate the species introduction risk by analysing the propagule pressure of species. A new aspect of ballast water sampling, which this contribution addresses, is compliance monitoring and enforcement of ballast water management standards as set by, e.g., the IMO Ballast Water Management Convention. To achieve this, sampling methods which result in representative ballast water samples are essential. We recommend such methods based on practical tests conducted on two commercial vessels also considering results from our previous studies. The results show that different sampling approaches influence the results regarding viable organism concentrations in ballast water samples. It was observed that the sampling duration (i.e., length of the sampling process), timing (i.e., in which point in time of the discharge the sample is taken), the number of samples and the sampled water quantity are the main factors influencing the concentrations of viable organisms in a ballast water sample. Based on our findings we provide recommendations for representative ballast water sampling.

Evaluation of the COBAS Hepatitis C Virus (HCV) TaqMan analyte-specific reagent assay and comparison to the COBAS Amplicor HCV Monitor V2.0 and Versant HCV bDNA 3.0 assays.

PubMed

Konnick, Eric Q; Williams, Sheri M; Ashwood, Edward R; Hillyard, David R

2005-05-01

Performance characteristics of the COBAS hepatitis C virus (HCV) TaqMan analyte-specific reagent (TM-ASR) assay using the QIAGEN BioRobot 9604 for RNA extraction were evaluated and compared to the COBAS Amplicor HCV Monitor V2.0 (Amplicor) and Versant HCV bDNA 3.0 (Versant) assays using clinical samples. Calibration of TM-ASR using Armored RNA allowed determination of the distribution of HCV RNA in clinical samples, using 22,399 clinical samples. Limit of detection, linearity, and inter- and intraassay assay precision were determined for the TM-ASR assay using multiple clinical specimen panels across multiple determinations. Genotype specificity for the TM-ASR assay was determined using samples with different HCV RNA genotypes evaluated and compared against predetermined results. Contamination control of the TM-ASR assay was evaluated using pools of HCV RNA-positive and -negative samples tested in a checkerboard pattern over 12 runs of 96 samples. Correlation of the TM-ASR, Amplicor, and Versant assays was determined using 100 paired clinical samples and Deming regression analysis. The TM-ASR performed well with respect to linearity, precision, and contamination control. The correlation between TM-ASR and the Amplicor and Versant assays was poor, with large differences between assay results for individual samples. Calibration of the TM-ASR assay with Armored RNA allowed for a wide dynamic range and description of the distribution of HCV RNA in clinical samples.

Evaluation of the COBAS Hepatitis C Virus (HCV) TaqMan Analyte-Specific Reagent Assay and Comparison to the COBAS Amplicor HCV Monitor V2.0 and Versant HCV bDNA 3.0 Assays

PubMed Central

Konnick, Eric Q.; Williams, Sheri M.; Ashwood, Edward R.; Hillyard, David R.

2005-01-01

Performance characteristics of the COBAS hepatitis C virus (HCV) TaqMan analyte-specific reagent (TM-ASR) assay using the QIAGEN BioRobot 9604 for RNA extraction were evaluated and compared to the COBAS Amplicor HCV Monitor V2.0 (Amplicor) and Versant HCV bDNA 3.0 (Versant) assays using clinical samples. Calibration of TM-ASR using Armored RNA allowed determination of the distribution of HCV RNA in clinical samples, using 22,399 clinical samples. Limit of detection, linearity, and inter- and intraassay assay precision were determined for the TM-ASR assay using multiple clinical specimen panels across multiple determinations. Genotype specificity for the TM-ASR assay was determined using samples with different HCV RNA genotypes evaluated and compared against predetermined results. Contamination control of the TM-ASR assay was evaluated using pools of HCV RNA-positive and -negative samples tested in a checkerboard pattern over 12 runs of 96 samples. Correlation of the TM-ASR, Amplicor, and Versant assays was determined using 100 paired clinical samples and Deming regression analysis. The TM-ASR performed well with respect to linearity, precision, and contamination control. The correlation between TM-ASR and the Amplicor and Versant assays was poor, with large differences between assay results for individual samples. Calibration of the TM-ASR assay with Armored RNA allowed for a wide dynamic range and description of the distribution of HCV RNA in clinical samples. PMID:15872232

Milestone Report - M3FT-15OR03120215 - Recommend HIP Conditions for AgZ

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

Bruffey, Stephanie H.; Jubin, Robert Thomas

2015-09-18

The purpose of this study was to continue research to determine if HIPing could directly convert I-Ag 0Z into a suitable waste form. Fiscal year (FY) 2015 work completed studies of Phase IIA, IIB, and IIC samples. Product consistency testing (PCT) of Phase IIA samples resulted in iodine release below detection limit for six of twelve samples. This is promising and indicates that a durable waste form may be produced through HIPing even if transformation of the zeolite to a distinct mineral phase does not occur. From PCT results of Phase IIA samples, it was determined that future pressing shouldmore » be conducted at a temperature of 900°C. Phase IIC testing continued production of samples to examine the effects of multiple source materials, compositional variations, and an expanded temperature range. The density of each sample was determined and x-ray diffraction (XRD) patterns were obtained. In all cases, there was nothing in the XRD analyses to indicate the creation of any AgI-containing silicon phase; the samples were found to be largely amorphous.« less

Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of Cr, Fe, Cu, Zn and Se in cereals

NASA Astrophysics Data System (ADS)

Huang, Shih-Yi; Jiang, Shiuh-Jen; Sahayam, A. C.

2014-11-01

Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry (USS-ETV-ICP-MS) has been applied to determine Cr, Fe, Cu, Zn and Se in several cereal samples. Thioacetamide was used as the modifier to enhance the ion signals. The background ions at the masses of interest were reduced in intensity significantly by using 1.0 mL min- 1 methane (CH4) as reaction cell gas in the dynamic reaction cell (DRC). Since the sensitivities of Cr, Fe, Cu, Zn and Se in different matrices were quite different, standard addition and isotope dilution methods were used for the determination of Cr, Fe, Cu, Zn and Se in these cereal samples. The method detection limits estimated from standard addition curves were about 1, 10, 4, 12 and 2 ng g- 1 for Cr, Fe, Cu, Zn and Se, respectively, in original cereal samples. This procedure has been applied to the determination of Cr, Fe, Cu, Zn and Se whose concentrations are in μg g- 1 (except Cr and Se) in standard reference materials (SRM) of National institute of standards and technology (NIST), NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour and two cereal samples purchased from a local market. The analysis results of reference materials agreed with certified values at 95% confidence level according to Student's T-test. The results for the real world cereal samples were also found to be in good agreement with the pneumatic nebulization DRC ICP-MS results of the sample solutions.

Off-Site Radiation Exposure Review Project: Phase 2 soils program

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

McArthur, R.D.; Miller, F.L. Jr.

1989-12-01

To help estimate population doses of radiation from fallout originating at the Nevada Test Site, soil samples were collected throughout the western United States. Each sample was prepared by drying and ball-milling, then analyzed by gamma-spectrometry to determine the amount of {sup 137}Cs it contained. Most samples were also analyzed by chemical separation and alpha-spectrometry to determine {sup 239 + 240}Pu and by isotope mass spectroscopy to determine the ratios of {sup 240}Pu to {sup 239}Pu and {sup 241}Pu to {sup 239}Pu. The total inventories of cesium and plutonium at 171 sites were computed from the results. This report describesmore » the sample collection, processing, and analysis, presents the analytical results, and assesses the quality of the data. 10 refs., 9 figs., 12 tabs.« less

In-situ pre-concentration through repeated sampling and pyrolysis for ultrasensitive determination of thallium in drinking water by electrothermal atomic absorption spectrometry.

PubMed

Liu, Liwei; Zheng, Huaili; Xu, Bincheng; Xiao, Lang; Chigan, Yong; Zhangluo, Yilan

2018-03-01

In this paper, a procedure for in-situ pre-concentration in graphite furnace by repeated sampling and pyrolysis is proposed for the determination of ultra-trace thallium in drinking water by graphite furnace atomic absorption spectrometry (GF-AAS). Without any other laborious enrichment processes that routinely result in analyte loss and contamination, thallium was directly concentrated in the graphite furnace automatically and subsequently subject to analysis. The effects of several key factors, such as the temperature for pyrolysis and atomization, the chemical modifier, and the repeated sampling times were investigated. Under the optimized conditions, a limit of detection of 0.01µgL -1 was obtained, which fulfilled thallium determination in drinking water by GB 5749-2006 regulated by China. Successful analysis of thallium in certified water samples and drinking water samples was demonstrated, with analytical results in good agreement with the certified values and those by inductively coupled plasma mass spectrometry (ICP-MS), respectively. Routine spike-recovery tests with randomly selected drinking water samples showed satisfactory results of 80-96%. The proposed method is simple and sensitive for screening of ultra-trace thallium in drinking water samples. Copyright © 2017. Published by Elsevier B.V.

Simultaneous determination of specific alpha and beta emitters by LSC-PLS in water samples.

PubMed

Fons-Castells, J; Tent-Petrus, J; Llauradó, M

2017-01-01

Liquid scintillation counting (LSC) is a commonly used technique for the determination of alpha and beta emitters. However, LSC has poor resolution and the continuous spectra for beta emitters hinder the simultaneous determination of several alpha and beta emitters from the same spectrum. In this paper, the feasibility of multivariate calibration by partial least squares (PLS) models for the determination of several alpha ( nat U, 241 Am and 226 Ra) and beta emitters ( 40 K, 60 Co, 90 Sr/ 90 Y, 134 Cs and 137 Cs) in water samples is reported. A set of alpha and beta spectra from radionuclide calibration standards were used to construct three PLS models. Experimentally mixed radionuclides and intercomparision materials were used to validate the models. The results had a maximum relative bias of 25% when all the radionuclides in the sample were included in the calibration set; otherwise the relative bias was over 100% for some radionuclides. The results obtained show that LSC-PLS is a useful approach for the simultaneous determination of alpha and beta emitters in multi-radionuclide samples. However, to obtain useful results, it is important to include all the radionuclides expected in the studied scenario in the calibration set. Copyright © 2016 Elsevier Ltd. All rights reserved.

TU-FG-BRB-02: The Impact of Using Dual-Energy CT for Determining Proton Stopping Powers: Comparison Between Theory and Experiments

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

Baer, E; Jee, K; Zhang, R

Purpose: To evaluate the clinical performance of dual-energy CT (DECT) in determining proton stopping power ratios (SPR) and demonstrate advantages over conventional single-energy CT (SECT). Methods: SECT and DECT scans of tissue-equivalent plastics as well as animal meat samples are performed with a Siemens SOMATOM Definition Flash. The methods of Schneider et al. (1996) and Bourque et al. (2014) are used to determine proton SPR on SECT and DECT images, respectively. Waterequivalent path length (WEPL) measurements of plastics and tissue samples are performed with a 195 MeV proton beam. WEPL values are determined experimentally using the depth-dose shift and dosemore » extinction methods. Results: Comparison between CT-based and experimental WEPL is performed for 12 tissue-equivalent plastic as well as 6 meat boxes containing animal liver, kidney, heart, stomach, muscle and bones. For plastic materials, results show a systematic improvement in determining SPR with DECT, with a mean absolute error of 0.4% compared to 1.7% for SECT. For the meat samples, preliminary results show the ability for DECT to determine WEPL with a mean absolute value of 1.1% over all meat boxes. Conclusion: This work demonstrates the potential in using DECT for determining proton SPR with plastic materials in a clinical context. Further work is required to show the benefits of DECT for tissue samples. While experimental uncertainties could be a limiting factor to show the benefits of DECT over SECT for the meat samples, further work is required to adapt the DECT formalism in the context of clinical use, where noise and artifacts play an important role.« less

Comparison of analytical methods for the determination of histamine in reference canned fish samples

NASA Astrophysics Data System (ADS)

Jakšić, S.; Baloš, M. Ž.; Mihaljev, Ž.; Prodanov Radulović, J.; Nešić, K.

2017-09-01

Two screening methods for histamine in canned fish, an enzymatic test and a competitive direct enzyme-linked immunosorbent assay (CD-ELISA), were compared with the reversed-phase liquid chromatography (RP-HPLC) standard method. For enzymatic and CD-ELISA methods, determination was conducted according to producers’ manuals. For RP-HPLC, histamine was derivatized with dansyl-chloride, followed by RP-HPLC and diode array detection. Results of analysis of canned fish, supplied as reference samples for proficiency testing, showed good agreement when histamine was present at higher concentrations (above 100 mg kg-1). At a lower level (16.95 mg kg-1), the enzymatic test produced some higher results. Generally, analysis of four reference samples according to CD-ELISA and RP-HPLC showed good agreement for histamine determination (r=0.977 in concentration range 16.95-216 mg kg-1) The results show that the applied enzymatic test and CD-ELISA appeared to be suitable screening methods for the determination of histamine in canned fish.

Salting-out assisted liquid-liquid extraction combined with gas chromatography-mass spectrometry for the determination of pyrethroid insecticides in high salinity and biological samples.

PubMed

Niu, Zongliang; Yu, Chunwei; He, Xiaowen; Zhang, Jun; Wen, Yingying

2017-09-05

A salting-out assisted liquid-liquid extraction (SALLE) combined with gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of four pyrethroid insecticides (PYRs) in high salinity and biological samples. Several parameters including sample pH, salting-out solution volume and salting-out solution pH influencing the extraction efficiency were systematically investigated with the aid of orthogonal design. The optimal extraction conditions of SALLE were: 4mL of salting-out solution with pH=4 and the sample pH=3. Under the optimum extraction and determination conditions, good responses for four PYRs were obtained in a range of 5-5000ng/mL, with linear coefficients greater than 0.998. The recoveries of the four PYRs ranged from 74% to 110%, with standard deviations ranging from 1.8% to 9.8%. The limits of detection based on a signal-to-noise ratio of 3 were between 1.5-60.6ng/mL. The method was applied to the determination of PYRs in urine, seawater and wastewater samples with a satisfactory result. The results demonstrated that this SALLE-GC-MS method was successfully applied to determine PYRs in high salinity and biological samples. SALLE avoided the need for the elimination of salinity and protein in the sample matrix, as well as clean-up of the extractant. Most of all, no centrifugation or any special apparatus are required, make this a promising method for rapid sample preparation procedure. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of trace metals in drinking water in Irbid City-Northern Jordan.

PubMed

Alomary, Ahmed

2013-02-01

Drinking water samples from Irbid, the second populated city in Jordan were analyzed for trace metals (As, Ba, Cd, Pb, Cr, Cu, Fe, Zn, Mn, Ni, and Se) content. The study was undertaken to determine if the metal concentrations were within the national and international guidelines. A total of 90 drinking water samples were collected from Al-Yarmouk University area. The samples were collected from three different water types: tap water (TW), home-purified water (HPW), and plant-purified water (PPW). All the samples were analyzed for trace metals using an inductively coupled plasma-optical emission spectrometry. All the samples analyzed were within the United States Environmental Protection Agency admissible pH limit (6.5-8.5). The results showed that concentrations of the trace metals vary significantly between the three drinking water types. The results showed that HPW samples have the lowest level of trace metals and the concentrations of some essential trace metals in these samples are less than the recommended amounts. Slight differences in the metal contents were found between HPW samples, little differences between PPW samples; however, significant differences were found between TW samples. Although some TW samples showed high levels of trace metals, however, the mean level of most elements determined in the samples were well within the Jordanian standards as well as the World Health Organization standards for drinking water.

Methods for Determining Particle Size Distributions from Nuclear Detonations.

DTIC Science & Technology

1987-03-01

Debris . . . 30 IV. Summary of Sample Preparation Method . . . . 35 V. Set Parameters for PCS ... ........... 39 VI. Analysis by Vendors...54 XV. Results From Brookhaven Analysis Using The Method of Cumulants ... ........... . 54 XVI. Results From Brookhaven Analysis of Sample...R-3 Using Histogram Method ......... .55 XVII. Results From Brookhaven Analysis of Sample R-8 Using Histogram Method ........... 56 XVIII.TEM Particle

Determinants of Weight Gain in Women with Early-Stage Breast Cancer

DTIC Science & Technology

2009-04-01

determination of HbA1C results. Serum and plasma are being stored to allow for future determination of sex hormone and cortisol levels...fresh whole blood is sent to Labcorp for determination of HbA1C results. Originally we had planned to begin shipping serum samples periodically to

Effects of L-ascorbic acid on physicochemical characteristics of wheat starch.

PubMed

Majzoobi, Mahsa; Radi, Mohsen; Farahnaky, Asgar; Tongdang, Tawee

2012-03-01

The main objective of this study was to determine the effects of l-ascorbic acid, as a permitted additive in bakery products, on characteristics of wheat starch. Suspensions of wheat starch (30%, w/w) in water containing 140 mg/kg ascorbic acid before and after gelatinization were prepared and studied using different techniques. The results of scanning electron microscopy showed that some spots appeared on the surface of the starch granules as a result of the addition of ascorbic acid. However, no changes in the starch crystalline pattern and its degree of crystallinity were observed by X-ray diffraction technique. For ungelatinized samples, no difference in the pasting properties of the samples was determined by the rapid visco analyzer, whereas for the gelatinized samples, peak and final viscosities decreased for the samples contained ascorbic acid. Determination of the intrinsic viscosities of the samples showed that addition of ascorbic acid to the gelatinized samples reduced the intrinsic viscosity. In general, it was found that ascorbic acid had some degradation effects on wheat starch molecules particularly after gelatinization. © 2012 Institute of Food Technologists®

Determination of germanium by AAS in chloride-containing matrices.

PubMed

Anwari, M A; Abbasi, H U; Volkan, M; Ataman, O Y

1996-06-01

Interference effects of NaCl on the ET-AAS determination of Ge have been studied. The use of several matrix modifiers to alleviate this problem such as Ni and Zn perchlorates and nitrates, nitric acid, ammonium nitrate are reported. The stabilizing effect of Zn and Ni perchlorates allows the use of high pretreatment temperatures. NaCl is thus thermally volatilized from the atomizer by employing pretreatment temperatures higher than 1500 degrees C resulting in an improved sensitivity. Germanium levels in zinc plant slag samples, have been determined and compared to those obtained for the same samples spiked with NaCl with platform and wall atomization using nickel perchlorate as a matrix modifier. The results were compared with those from a hydride generation system equipped with a liquid nitrogen trap. The recoveries for germanium have been almost complete and amount to 99% for the original slag samples and 80% for 15% (w/w) NaCl containing spiked samples.

Radiological results for samples collected on paired glass- and cellulose-fiber filters at the Sandia complex, Tonopah Test Range, Nevada

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

Mizell, Steve A.; Shadel, Craig A.

Airborne particulates are collected at U.S. Department of Energy sites that exhibit radiological contamination on the soil surface to help assess the potential for wind to transport radionuclides from the contamination sites. Collecting these samples was originally accomplished by drawing air through a cellulose-fiber filter. These filters were replaced with glass-fiber filters in March 2011. Airborne particulates were collected side by side on the two filter materials between May 2013 and May 2014. Comparisons of the sample mass and the radioactivity determinations for the side-by-side samples were undertaken to determine if the change in the filter medium produced significant results.more » The differences in the results obtained using the two filter types were assessed visually by evaluating the time series and correlation plots and statistically by conducting a nonparametric matched-pair sign test. Generally, the glass-fiber filters collect larger samples of particulates and produce higher radioactivity values for the gross alpha, gross beta, and gamma spectroscopy analyses. However, the correlation between the radioanalytical results for the glass-fiber filters and the cellulose-fiber filters was not strong enough to generate a linear regression function to estimate the glass-fiber filter sample results from the cellulose-fiber filter sample results.« less

[Sampling, storage and transport of biological materials collected from living and deceased subjects for determination of concentration levels of ethyl alcohol and similarly acting substances. A proposal of updating the blood and urine sampling protocol].

PubMed

Wiergowski, Marek; Reguła, Krystyna; Pieśniak, Dorota; Galer-Tatarowicz, Katarzyna; Szpiech, Beata; Jankowski, Zbigniew

2007-01-01

The present paper emphasizes the most common mistakes committed at the beginning of an analytical procedure. To shorten the time and decrease the cost of determinations of substances with similar to alcohol activity, it is postulated to introduce mass-scale screening analysis of saliva collected from a living subject at the site of the event, with all positive results confirmed in blood or urine samples. If no saliva sample is collected for toxicology, a urine sample, allowing for a stat fast screening analysis, and a blood sample, to confirm the result, should be ensured. Inappropriate storage of a blood sample in the tube without a preservative can cause sample spilling and its irretrievable loss. The authors propose updating the "Blood/urine sampling protocol", with the updated version to be introduced into practice following consultations and revisions.

Heavy metal concentrations and the variations of foraminifers in the Silivri-Kumbagi area (NW Marmara Sea, Turkey)

NASA Astrophysics Data System (ADS)

Ünal Yümün, Zeki; Murat Kılıç, Ali; Önce, Melike

2016-04-01

In the area between Silivri (İstanbul) and Kumbagi (Tekirdag), NW of Marmara Sea, there is a considerable extent in marine pollution from industrial and settlements wastes, sea transports, and agricultural activities. The most important one of these pollutions is the spread of heavy metals. Our research investigated sediments in order to determine whether heavy minerals affected biota such as recent foraminifers, or not. Our investigation area starts from Marmara Ereglisi, in the east, continues to Tekirdag and Kumbagi, in the west. 10 sea-water samples, 10 sediment-core samples and one 10 m core-drilling sample, taken 250 m off-shore from coast line. As a result of this sampling geochemical analysis of the bottom-mud and water samples were done and the ratio of heavy metals and other contaminants determined. For heavy metal analyses, concentration analysis of 12 heavy metals (Cd, Fe, Cu, Pb, Zn, Al, Co, Cr, Mn, Ni, As, and Hg) has been conducted, as ppm, in sediment samples taken from the levels in which foraminifers are collected. Perpendicular (spatial) heavy metal concentration changes have been determined with off-shore drilling samples and horizontal changes (geochronological) have been determined with the help of core samples. Especially, it has been understood that heavy metal concentrations in recent sediments are higher compared to the past. In this research the samples have been taken from each 10 cm. of core and drilling samples to collect the benthic foraminifers. In this context, 15 grams of dry sediment sample taken from each level, have been washed in 125 μm sieves in order to determine its benthic foraminifer content. Benthic foraminifera from these samples have been identified taxonomically and their morphological differentiation has been determined after taking SEM photos. As a result of this study, the foraminifera types of "Adelosinacliarensis, Adelosinamediteranensis, Adelosinapulchella, Ammonia compacta, Ammonia parkinsonia, Ammonia tepida, Cribroelphidiumpoeyonum, Cycloforinacontorta, Elphidiumaculeatum, Elphidiumcomplanatum, Elphidiumcrispum, Elphidiumgalvestonense, Lobatulalobatula, Massilinasecans, Miliolinellasubrotunda, Pseudotriloculinaoblanga, Quinqueloculina seminula, Quinqueloculina polygona, Spiroloculinaangulosa, Spiroloculinaexcavata, Triloculina marioni" have been determined. Especially in the Elphidiumcrispumand Ammonia compacta, collected from the core samples taken from Marmara Ereglisi (Tekirdag) and Silivri (Istanbul) offshore, some morphological variations, colour changes, abnormality and multiple-individuals, were observed. Increasing of the heavy metal concentration in the levels of these morphological variations is noticeable.

Application of an ETV-ICP system for the determination of elements in human hair*1

NASA Astrophysics Data System (ADS)

Plantikow-Voβgätter, F.; Denkhaus, E.

1996-01-01

When determining element contents in hair samples without sample digestion it is necessary to analyze large sample volumes in order to minimize problems of inhomogeneity of biological sample materials. Therefore an electrothermal vaporization system (ETV) is used for solid sample introduction into an inductively coupled plasma (ICP) for the determination of matrix and trace elements in hair. This paper concentrates on the instrumental aspects without time consuming sample preparation. The results obtained for optimization tests, ETV operating parameters and ICP operating parameters, are shown and discussed. Standard additions are used for calibration for the determination of Zn, Mg, and Mn in human hair. Studies including reproducibility and detection limits for chosen elements have been carried out on certified reference materials (CRMs). The determination of reproducibility (relative standard deviation (RSD) of n = 10) and detection limits (DLs) of Zn (RSD < 8.5%, DL < 0.8 μ g -1), Mn (RSD < 14.1%, DL < 0.3 μ g -1), and Mg (RSD < 7.4%, DL < 6.6 μ g -1) are satisfactory. The concentration values found show good agreement with the corresponding certified values. Further sample preparation steps, including hair sampling, washing procedure and homogenization for hair, relating to measurements of real hair samples are described.

Measurement of rivaroxaban and apixaban in serum samples of patients

PubMed Central

Harenberg, Job; Krämer, Sandra; Du, Shanshan; Zolfaghari, Shabnam; Schulze, Astrid; Krämer, Roland; Weiss, Christel; Wehling, Martin; Lip, Gregory Y H

2014-01-01

Background The determination of rivaroxaban and apixaban from serum samples of patients may be beneficial in specific clinical situations when additional blood sampling for plasma and thus the determination of factor Xa activity is not feasible or results are not plausible. Materials and methods The primary aim of this study was to compare the concentrations of rivaroxaban and apixaban in serum with those measured in plasma. Secondary aims were the performance of three different chromogenic methods and concentrations in patients on treatment with rivaroxaban 10 mg od (n = 124) or 20 mg od (n = 94) or apixaban 5 mg bid (n = 52) measured at different time. Results Concentrations of rivaroxaban and apixaban in serum were about 20–25% higher compared with plasma samples with a high correlation (r = 0·79775–0·94662) using all assays (all P < 0·0001). The intraclass correlation coefficients were about 0·90 for rivaroxaban and 0·55 for apixaban. Mean rivaroxaban concentrations were higher at 2 and 3 h compared with 1 and 12 h after administration measured from plasma and serum samples (all P-values < 0·05) and were not different between 1 vs. 12 h (plasma and serum). Conclusions The results indicate that rivaroxaban and apixaban concentrations can be determined specifically from serum samples. PMID:24931429

Monitoring of platinum surface contamination in seven Dutch hospital pharmacies using inductively coupled plasma mass spectrometry

PubMed Central

Huitema, A. D. R.; Bakker, E. N.; Douma, J. W.; Schimmel, K. J. M.; van Weringh, G.; de Wolf, P. J.; Schellens, J. H. M.; Beijnen, J. H.

2007-01-01

Objective: To develop, validate, and apply a method for the determination of platinum contamination, originating from cisplatinum, oxaliplatinum, and carboplatinum. Methods: Inductively coupled plasma mass spectrometry (ICP-MS) was used to determine platinum in wipe samples. The sampling procedure and the analytical conditions were optimised and the assay was validated. The method was applied to measure surface contamination in seven Dutch hospital pharmacies. Results: The developed method allowed reproducible quantification of 0.50 ng l−1 platinum (5 pg/wipe sample). Recoveries for stainless steel and linoleum surfaces ranged between 50.4 and 81.4% for the different platinum compounds tested. Platinum contamination was reported in 88% of the wipe samples. Although a substantial variation in surface contamination of the pharmacies was noticed, in most pharmacies, the laminar-airflow (LAF) hoods, the floor in front of the LAF hoods, door handles, and handles of service hatches showed positive results. This demonstrates that contamination is spread throughout the preparation rooms. Conclusion: We developed and validated an ultra sensitive and reliable ICP-MS method for the determination of platinum in surface samples. Surface contamination with platinum was observed in all hospital pharmacies sampled. The interpretation of these results is, however, complicated. PMID:17377802

Thermogravimetric analysis for the determination of water release rate from microcrystalline cellulose dry powder and wet bead systems.

PubMed

Mayville, Francis C; Wigent, Rodney J; Schwartz, Joseph B

2006-01-01

The purpose of this work was to determine the total amount of water contained in dry powder and wet bead samples of microcrystalline cellulose, MCC, (Avicel PH-101), taken from various stages of the extrusion/marumerization process used to make beads and to determine the kinetic rates of water release from each sample. These samples were allowed to equilibrate in controlled humidity chambers at 25 degrees C. The total amount of water in each sample, after equilibration, was determined by thermogravimetric analysis (TGA) as a function of temperature. The rates of water release from these samples were determined by using isothermal gravimetric analysis (ITGA) as a function of time. Analysis of the results for these studies suggest that water was released from these systems by several different kinetic mechanisms. The water release mechanisms for these systems include: zero order, second order, and diffusion controlled kinetics. It is believed that all three kinetic mechanisms will occur at the same time, however; only one mechanism will be prominent. The prominent mechanism was based on the amount of water present in the sample.

Porous calcium polyphosphate bone substitutes: additive manufacturing versus conventional gravity sinter processing-effect on structure and mechanical properties.

PubMed

Hu, Youxin; Shanjani, Yaser; Toyserkani, Ehsan; Grynpas, Marc; Wang, Rizhi; Pilliar, Robert

2014-02-01

Porous calcium polyphosphate (CPP) structures proposed as bone-substitute implants and made by sintering CPP powders to form bending test samples of approximately 35 vol % porosity were machined from preformed blocks made either by additive manufacturing (AM) or conventional gravity sintering (CS) methods and the structure and mechanical characteristics of samples so made were compared. AM-made samples displayed higher bending strengths (≈1.2-1.4 times greater than CS-made samples), whereas elastic constant (i.e., effective elastic modulus of the porous structures) that is determined by material elastic modulus and structural geometry of the samples was ≈1.9-2.3 times greater for AM-made samples. X-ray diffraction analysis showed that samples made by either method displayed the same crystal structure forming β-CPP after sinter annealing. The material elastic modulus, E, determined using nanoindentation tests also showed the same value for both sample types (i.e., E ≈ 64 GPa). Examination of the porous structures indicated that significantly larger sinter necks resulted in the AM-made samples which presumably resulted in the higher mechanical properties. The development of mechanical properties was attributed to the different sinter anneal procedures required to make 35 vol % porous samples by the two methods. A primary objective of the present study, in addition to reporting on bending strength and sample stiffness (elastic constant) characteristics, was to determine why the two processes resulted in the observed mechanical property differences for samples of equivalent volume percentage of porosity. An understanding of the fundamental reason(s) for the observed effect is considered important for developing improved processes for preparation of porous CPP implants as bone substitutes for use in high load-bearing skeletal sites. Copyright © 2013 Wiley Periodicals, Inc.

Determination of ammonium in river water and sewage samples by capillary zone electrophoresis with direct UV detection.

PubMed

Fukushi, Keiichi; Ito, Hideyuki; Kimura, Kenichi; Yokota, Kuriko; Saito, Keiitsu; Chayama, Kenji; Takeda, Sahori; Wakida, Shin-ichi

2006-02-17

We developed capillary zone electrophoresis (CZE) with direct UV detection for determination of ammonium in environmental water samples. Ammonium in the samples was partly converted into ammonia in the alkaline background electrolyte (BGE) during migration and was detected by molecular absorption of ammonia at 190 nm in approximately 7 min. The limit of detection (LOD) for ammonium was 0.24 mg/l (as nitrogen) at a signal-to-noise ratio of three. The respective values of the relative standard deviation (RSD) of peak area, peak height, and migration time for ammonium were 2.1, 1.8, and 0.46%. Major alkali and alkaline earth metal ions coexisting in the samples did not interfere with ammonium determination by the proposed method. The proposed method determined ammonium in surface water and sewage samples. The results were compared to those obtained using ion chromatography (IC).

Tank Vapor Characterization Project: Tank 241-S-102 fourth temporal study: Headspace gas and vapor characterization results from samples collected on December 19, 1996

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

Pool, K.H.; Evans, J.C.; Olsen, K.B.

1997-08-01

This report presents the results from analyses of samples taken from the headspace of waste storage tank 241-S-102 (Tank S-102) at the Hanford Site in Washington State. Tank headspace samples collected by SGN Eurisys Service Corporation (SESC) were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by SESC. Ammonia was determined to be above the immediate notification limit of 150 ppm as specified by the sampling and analysis planmore » (SAP). Hydrogen was the principal flammable constituent of the Tank S-102 headspace, determined to be present at approximately 2.410% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <2.973% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <2.973% of the LFL. Average measured concentrations of targeted gases, inorganic vapors, and selected organic vapors are provided in Table S.1. A summary of experimental methods, including sampling methodology, analytical procedures, and quality assurance and control methods are presented in Section 2.0. Detailed descriptions of the analytical results are provided in Section 3.0.« less

Geostatistics and the representative elementary volume of gamma ray tomography attenuation in rocks cores

USGS Publications Warehouse

Vogel, J.R.; Brown, G.O.

2003-01-01

Semivariograms of samples of Culebra Dolomite have been determined at two different resolutions for gamma ray computed tomography images. By fitting models to semivariograms, small-scale and large-scale correlation lengths are determined for four samples. Different semivariogram parameters were found for adjacent cores at both resolutions. Relative elementary volume (REV) concepts are related to the stationarity of the sample. A scale disparity factor is defined and is used to determine sample size required for ergodic stationarity with a specified correlation length. This allows for comparison of geostatistical measures and representative elementary volumes. The modifiable areal unit problem is also addressed and used to determine resolution effects on correlation lengths. By changing resolution, a range of correlation lengths can be determined for the same sample. Comparison of voxel volume to the best-fit model correlation length of a single sample at different resolutions reveals a linear scaling effect. Using this relationship, the range of the point value semivariogram is determined. This is the range approached as the voxel size goes to zero. Finally, these results are compared to the regularization theory of point variables for borehole cores and are found to be a better fit for predicting the volume-averaged range.

Determination of arsenic and cadmium in crude oil by direct sampling graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

de Jesus, Alexandre; Zmozinski, Ariane Vanessa; Damin, Isabel Cristina Ferreira; Silva, Márcia Messias; Vale, Maria Goreti Rodrigues

2012-05-01

In this work, a direct sampling graphite furnace atomic absorption spectrometry method has been developed for the determination of arsenic and cadmium in crude oil samples. The samples were weighed directly on the solid sampling platforms and introduced into the graphite tube for analysis. The chemical modifier used for both analytes was a mixture of 0.1% Pd + 0.06% Mg + 0.06% Triton X-100. Pyrolysis and atomization curves were obtained for both analytes using standards and samples. Calibration curves with aqueous standards could be used for both analytes. The limits of detection obtained were 5.1 μg kg- 1 for arsenic and 0.2 μg kg- 1 for cadmium, calculated for the maximum amount of sample that can be analyzed (8 mg and 10 mg) for arsenic and cadmium, respectively. Relative standard deviations lower than 20% were obtained. For validation purposes, a calibration curve was constructed with the SRM 1634c and aqueous standards for arsenic and the results obtained for several crude oil samples were in agreement according to paired t-test. The result obtained for the determination of arsenic in the SRM against aqueous standards was also in agreement with the certificate value. As there is no crude oil or similar reference material available with a certified value for cadmium, a digestion in an open vessel under reflux using a "cold finger" was adopted for validation purposes. The use of paired t-test showed that the results obtained by direct sampling and digestion were in agreement at a 95% confidence level. Recovery tests were carried out with inorganic and organic standards and the results were between 88% and 109%. The proposed method is simple, fast and reliable, being appropriated for routine analysis.

Effect of paratuberculosis on culling, milk production, and milk quality in dairy herds.

PubMed

Hendrick, Steven H; Kelton, David F; Leslie, Ken E; Lissemore, Kerry D; Archambault, Marie; Duffield, Todd F

2005-10-15

To determine the effect of paratuberculosis on culling, milk production, and milk quality in infected dairy herds. Cross-sectional study. 689 lactating dairy cows in 9 herds. Milk, blood, and fecal samples were obtained from all cows. Fecal samples were evaluated via mycobacterial culture. Serum samples were tested with a commercially available ELISA for antibodies against Mycobacterium avium subsp paratuberculosis, and preserved milk samples were tested with an ELISA for antibodies against M paratuberculosis. Mixed effect and proportional hazards models were used to determine the effect of paratuberculosis on 305-day milk, fat, and protein production; somatic cell count linear score; and the risk of culling. Cows with positive results of bacteriologic culture of feces and milk ELISA produced less milk, fat, and protein, compared with herdmates with negative results. No difference in 305-day milk or fat production was detected in cows with positive results of serum ELISA, compared with seronegative cows. The 3 survival analyses revealed that cows with positive results of each test were at higher risk of being culled than cows with negative results. Paratuberculosis status, as determined by use of all 3 diagnostic tests, was not associated with milk somatic cell count linear score. Results suggest that for the 9 herds in this study, paratuberculosis significantly decreased milk production and cow longevity.

Chemical analyses of hot springs, pools, geysers, and surface waters from Yellowstone National Park, Wyoming, and vicinity, 1974-1975

USGS Publications Warehouse

Ball, James W.; Nordstrom, D. Kirk; Jenne, Everett A.; Vivit, Davison V.

1998-01-01

This report presents all analytical determinations for samples collected from Yellowstone National Park and vicinity during 1974 and 1975. Water temperature, pH, Eh, and dissolved O2 were determined on-site. Total alkalinity and F were determined on the day of sample collection. Flame atomic-absorption spectrometry was used to determine concentrations of Li, Na, K, Ca, and Mg. Ultraviolet/visible spectrophotometry was used to determine concentrations of Fe(II), Fe(III), As(III), and As(V). Direct-current plasma-optical-emission spectrometry was used to determine the concentrations of B, Ba, Cd, Cs, Cu, Mn, Ni, Pb, Rb, Sr, and Zn. Two samples collected from Yellowstone Park in June 1974 were used as reference samples for testing the plasma analytical method. Results of these tests demonstrate acceptable precision for all detectable elements. Charge imbalance calculations revealed a small number of samples that may have been subject to measurement errors in pH or alkalinity. These data represent some of the most complete analyses of Yellowstone waters available.

Determination of sulphur in various vegetables by solid sampling high-resolution electrothermal molecular absorption spectrometry.

PubMed

Gunduz, Sema; Akman, Suleyman

2015-04-01

Sulphur was determined in various vegetables via molecular absorption of carbon monosulphide (CS) at 258.056 nm using a solid sampling high resolution continuum source electrothermal atomic absorption spectrometer (SS HR-CS ETAAS). Samples were dried, ground and directly introduced into the ruthenium coated graphite furnace as 0.05 to 0.50mg. All determinations were performed using palladium+citric acid modifier and applying a pyrolysis temperature of 1000 °C and a volatilisation temperature of 2400 °C. The results were in good agreement with certified sulphur concentrations of various vegetal CRM samples applying linear calibration technique prepared from thioacetamide. The limit of detection and characteristic mass of the method were 7.5 and 8.7 ng of S, respectively. The concentrations of S in various spinach, leek, lettuce, radish, Brussels sprouts, zucchini and chard samples were determined. It was showed that distribution of sulphur in CRM and grinded food samples were homogeneous even in micro-scale. Copyright © 2014 Elsevier Ltd. All rights reserved.

Usage of DNA Fingerprinting Technology for Quality Control in Molecular Lab Bench Work.

PubMed

McIntosh, Linda Y; Lal, Janella E; Qin, Dahui

2018-01-01

One of the major quality assurance (QA) goals in many molecular laboratories is to avoid sample pipetting errors on the lab bench; especially when pipetting into multiwell plates. A pipetting error can cause a switch in patient samples, which can lead to recording the wrong results for the patient samples involved. Such pipetting errors are difficult to identify when it happens in lab bench work. DNA fingerprinting is a powerful tool in determining sample identities. Our laboratory has explored the usage of this technology in our QA process and successfully established that DNA fingerprinting can be used to monitor possible sample switch in gene rearrangement lab bench work. We use florescent light to quench the florescence in the gene rearrangement polymerase chain reaction products. After that, DNA fingerprinting technology is used to identify the sample DNA in the gene rearrangement polymerase chain reaction plate. The result is compared with the corresponding patient's blood sample DNA to determine whether there is a sample switch during the lab bench work.

Assessment of airborne heavy metal pollution in soil and lichen in the Meric-Ergene Basin, Turkey.

PubMed

Hanedar, Asude

2015-01-01

In the present study, accumulations of airborne heavy metals in lichen and soil samples were determined on the basis of pollutant source groups by conducting Zinc (Zn), Lead (Pb), Iron (Fe), Copper (Cu), Chromium (Cr), Cadmium (Cd), Arsenic (As), Cobalt (Co) and Manganese (Mn) analyses on a total of 48 samples collected in the periods of May 2014 and August 2014 from 12 sampling points in a heavily industrialized area, a mixed industrial and residential area, an agricultural area and a background area in the Meric-Ergene Basin, and pH and total organic carbon determination was carried out on soil samples. With the obtained data, heavy metal levels were statistically assessed in detail by being associated with each other and with their probable sources; the accumulations found in soil and lichen samples were compared and spatial variances were set forth. Based on the results, it was observed that heavy metal pollution is at high levels particularly in industrialized areas, and that the differences between the cleanest and most polluted levels determined from soil samples for As, Cr, Cd and Pb reach 10 folds. The highest levels of all heavy metals were determined in both the soil and lichen samples collected from the areas in the south-east part of the region, where industrial activities and particularly leather and chemical industries are concentrated. With the comparison of the indication properties of soil and lichen, it was determined that significant and comparable results can be observed in both matrices.

[The design and application of domestic mid-IR fiber optics].

PubMed

Weng, Shi-fu; Gao, Jian-ping; Xu, Yi-zhuang; Yang, Li-min; Bian, Bei-ya; Xiang, Hai-bo; Wu, Jin-guang

2004-05-01

The combination of mid-IR fiber optics and FTIR has made the non-invasive determination of samples in situ, with long distances, and in vivo possible. In this paper domestic mid-IR fiber optics was improved to investigate the transmission ability of fiber optics and its application to the sample determination. New design was applied to obtaining one bare fiber optics, which has a minor energy loss and higher signal-to-noise ratio. The spectra of H2O/EtOH and tissue samples were measured using the new designed fiber optics and the results show that home-made mid-IR fiber optics can be applied to the field of determination of general and biological samples.

Investigations related to evaluation of ultramicrofluorometer

NASA Technical Reports Server (NTRS)

Whitcomb, B.

1981-01-01

High resolution emission and excitation fluorescent spectra were obtained for several samples in an effort to determine the optimum operational design for the instrument. The instrument was used to determine the required nature of a sample which could be detected, and in so doing, several different sample preparation techniques were considered. Numerous experiments were performed to determine the capabilities of the instrument with regard to the detection of suitably prepared virus specimens. Significant results were obtained in several areas. The fluorescent spectra indicated that substantial changes in the laser might be used advantageously to greatly improve the performance of the instrument. In the existing configuration, the instrument was shown to be capable of detecting the presence of suitably prepared virus samples.

Neuromuscular dose-response studies: determining sample size.

PubMed

Kopman, A F; Lien, C A; Naguib, M

2011-02-01

Investigators planning dose-response studies of neuromuscular blockers have rarely used a priori power analysis to determine the minimal sample size their protocols require. Institutional Review Boards and peer-reviewed journals now generally ask for this information. This study outlines a proposed method for meeting these requirements. The slopes of the dose-response relationships of eight neuromuscular blocking agents were determined using regression analysis. These values were substituted for γ in the Hill equation. When this is done, the coefficient of variation (COV) around the mean value of the ED₅₀ for each drug is easily calculated. Using these values, we performed an a priori one-sample two-tailed t-test of the means to determine the required sample size when the allowable error in the ED₅₀ was varied from ±10-20%. The COV averaged 22% (range 15-27%). We used a COV value of 25% in determining the sample size. If the allowable error in finding the mean ED₅₀ is ±15%, a sample size of 24 is needed to achieve a power of 80%. Increasing 'accuracy' beyond this point requires increasing greater sample sizes (e.g. an 'n' of 37 for a ±12% error). On the basis of the results of this retrospective analysis, a total sample size of not less than 24 subjects should be adequate for determining a neuromuscular blocking drug's clinical potency with a reasonable degree of assurance.

Comparison of sampling and test methods for determining asphalt content and moisture correction in asphalt concrete mixtures.

DOT National Transportation Integrated Search

1985-03-01

The purpose of this report is to identify the difference, if any, in AASHTO and OSHD test procedures and results. This report addresses the effect of the size of samples taken in the field and evaluates the methods of determining the moisture content...

The microwave induced plasma with optical emission spectrometry (MIP-OES) in 23 elements determination in geological samples.

PubMed

Niedzielski, P; Kozak, L; Wachelka, M; Jakubowski, K; Wybieralska, J

2015-01-01

The article presents the optimisation, validation and application of the microwave induced plasma optical emission spectrometry (MIP-OES) dedicated for a routine determination of Ag, Al, B, Ba, Bi, Ca, Cd, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Mo, Na, Ni, Pb, Sr, Tl, Zn, in the geological samples. The three procedures of sample preparation has been proposed: sample digestion with the use of hydrofluoric acid for determination of total concentration of elements, extraction by aqua regia for determination of the quasi-total element concentration and extraction by hydrochloric acid solution to determine contents of the elements in acid leachable fraction. The detection limits were on the level 0.001-0.121 mg L(-1) (from 0.010-0.10 to 1.2-12 mg kg(-1) depend on the samples preparation procedure); the precision: 0.20-1.37%; accuracy 85-115% (for recovery for certified standards materials analysis and parallel analysis by independent analytical techniques: X-ray fluorescence (XRF) and flame absorption spectrometry (FAAS)). The conformity of the results obtained by MIP-OES analytical procedures with the results obtained by XRF and FAAS analysis allows to propose the procedures for studies of elemental composition of the fraction of the geological samples. Additionally, the MIP-OES technique is much less expensive than ICP techniques and much less time-consuming than AAS techniques. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of arsenic in geological materials by electrothermal atomic-absorption spectrometry after hydride generation

USGS Publications Warehouse

Sanzolone, R.F.; Chao, T.T.; Welsch, E.P.

1979-01-01

Rock and soil samples are decomposed with HClO4-HNO3; after further treatment, arsine is generated and absorbed in a dilute silver nitrate solution. Aliquots of this solution are injected into a carbon rod atomizer. Down to 1 ppm As in samples can be determined and there are no significant interferences, even from chromium in soils. Good results were obtained for geochemical reference samples. ?? 1979.

Unified Model for the Overall Efficiency of Inlets Sampling from Horizontal Aerosol Flows

NASA Astrophysics Data System (ADS)

Hangal, Sunil Pralhad

When sampling aerosols from ambient or industrial air environments, the sampled aerosol must be representative of the aerosol in the free stream. The changes that occur during sampling must be assessed quantitatively so that sampling errors can be compensated for. In this study, unified models have been developed for the overall efficiency of tubular sharp-edged inlets sampling from horizontal aerosol flows oriented at 0 to 90^circ relative to the wind direction in the vertical (pitch) and horizontal plane(yaw). In the unified model, based on experimental data, the aspiration efficiency is represented by a single equation with different inertial parameters at 0 to 60^ circ and 45 to 90^circ . Tnt transmission efficiency is separated into two components: one due to gravitational settling in the boundary layer and the other due to impaction. The gravitational settling component is determined by extending a previously developed isoaxial sampling model to nonisoaxial sampling. The impaction component is determined by a new model that quantifies the particle losses caused by wall impaction. The model also quantifies the additional particle losses resulting from turbulent motion in the vena contracta which is formed in the inlet when the inlet velocity is higher than the wind velocity. When sampling aerosols in ambient or industrial environments with an inlet, small changes in wind direction or physical constraints in positioning the inlet in the system necessitates the assessment of sampling efficiency in both the vertical and horizontal plane. The overall sampling efficiency of tubular inlets has been experimentally investigated in yaw and pitch orientations at 0 to 20 ^circ from horizontal aerosol flows using a wind tunnel facility. The model for overall sampling efficiency has been extended to include both yaw and pitch sampling based on the new data. In this model, the difference between yaw and pitch is expressed by the effect of gravity on the impaction process inside the inlet described by a newly developed gravity effect angle. At yaw, the gravity effect angle on the wall impaction process does not change with sampling angle. At pitch, the gravity effect on the impaction process results in particle loss increase for upward and decrease for downward sampling. Using the unified model, graphical representations have been developed for sampling at small angles. These can be used in the field to determine the overall sampling efficiency of inlets at several operating conditions and the operating conditions that result in an acceptable sampling error. Pitch and diameter factors have been introduced for relating the efficiency values over a wide range of conditions to those of a reference condition. The pitch factor determines the overall sampling efficiency at pitch from yaw values, and the diameter factor determines the overall sampling efficiency at different inlet diameters.

RECOMMENDATIONS FOR SAMPLING OF TANK 18 IN F TANK FARM

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

Shine, G.

2009-12-14

Representative sampling is required for characterization of the residual floor material in Tank 18 prior to operational closure. Tank 18 is an 85-foot diameter, 34-foot high carbon steel tank with nominal operating volume of 1,300,000 gallons. It is a Type IV tank, and has been in service storing radioactive materials since 1959. Recent mechanical cleaning of the tank removed all mounds of material. Anticipating a low level of solids in the residual material, Huff and Thaxton [2009] developed a plan to sample the material during the final clean-up process while it would still be resident in sufficient quantities to supportmore » analytical determinations in four quadrants of the tank. Execution of the plan produced fewer solids than expected to support analytical determinations in all four quadrants. Huff and Thaxton [2009] then restructured the plan to characterize the residual floor material separately in the North and the South regions: two 'hemispheres.' This document provides sampling recommendations to complete the characterization of the residual material on the tank bottom following the guidance in Huff and Thaxton [2009] to split the tank floor into a North and a South hemisphere. The number of samples is determined from a modification of the formula previously published in Edwards [2001] and the sample characterization data for previous sampling of Tank 18 described by Oji [2009]. The uncertainty is quantified by an upper 95% confidence limit (UCL95%) on each analyte's mean concentration in Tank 18. The procedure computes the uncertainty in analyte concentration as a function of the number of samples, and the final number of samples is determined when the reduction in the uncertainty from an additional sample no longer has a practical impact on results. The characterization of the full suite of analytes in the North hemisphere is currently supported by a single Mantis rover sample obtained from a compact region near the center riser. A floor scrape sample was obtained from a compact region near the northeast riser and has been analyzed for a shortened list of key analytes. Since the unused portion of the floor scrape sample material is archived and available in sufficient quantity, additional analyses need to be performed to complete results for the full suite of constituents. The characterization of the full suite of analytes in the South hemisphere is currently supported by a single Mantis rover sample; there have been no floor scrape samples previously taken from the South hemisphere. The criterion to determine the number of additional samples was based on the practical reduction in the uncertainty when a new sample is added. This was achieved when five additional samples are obtained. In addition, two archived samples will be used if a contingency such as failing to demonstrate the comparability of the Mantis samples to the floor scrape samples occurs. To complete sampling of the Tank 18 residual floor material, three additional samples should be taken from the North hemisphere and four additional samples should be taken from the South hemisphere. One of the samples from each hemisphere will be archived in case of need. Two of the three additional samples from the North hemisphere and three of the four additional samples from the South hemisphere will be analyzed. Once the results are available, differences between the Mantis and three floor scrape samples (the sample previously obtained near NE riser plus the two additional samples that will be analyzed) results will be evaluated. If there are no statistically significant analyte concentration differences between the Mantis and floor scrape samples, those results will be combined and then UCL95%s will be calculated. If the analyte concentration differences between the Mantis and floor scrape samples are statistically significant, the UCL95%s will be calculated without the Mantis sample results. If further reduction in the upper confidence limits is needed and can be achieved by the addition of the archived samples, they will be analyzed and included in the statistical computations. Initially, the analyte concentrations in the residual material on the floor of Tank 18 will be determined separately in the North and the South hemispheres. However, if final sampling results show that differences between the North and South samples are consistent within sampling variation, then the final computations can be based on consolidating all sample results from the tank floor. Recommended locations may be subject to physical tank access and sampling constraints for the additional samples. The recommendations have been discussed in Section 4 and are based on partitioning the Tank 18 floor into an inner and an outer ring and six 60{sup o} sectors depicted in Figure 1. The location of the border between the inner and outer rings is based on dividing the residual material into two approximately equal volumes.« less

U.S. Geological Survey nutrient preservation experiment; nutrient concentration data for surface-, ground-, and municipal-supply water samples and quality-assurance samples

USGS Publications Warehouse

Patton, Charles J.; Truitt, Earl P.

1995-01-01

This report is a compilation of analytical results from a study conducted at the U.S. Geological Survey, National Water Quality Laboratory (NWQL) in 1992 to assess the effectiveness of three field treatment protocols to stabilize nutrient concentra- tions in water samples stored for about 1 month at 4C. Field treatments tested were chilling, adjusting sample pH to less than 2 with sulfuric acid and chilling, and adding 52 milligrams of mercury (II) chloride per liter of sample and chilling. Field treatments of samples collected for determination of ammonium, nitrate plus nitrite, nitrite, dissolved Kjeldahl nitrogen, orthophosphate, and dissolved phosphorus included 0.45-micrometer membrane filtration. Only total Kjeldahl nitrogen and total phosphorus were determined in unfiltered samples. Data reported here pertain to water samples collected in April and May 1992 from 15 sites within the continental United States. Also included in this report are analytical results for nutrient concentrations in synthetic reference samples that were analyzed concurrently with real samples.

THE DETERMINATION OF TRACES OF IRON IN SAMPLES OF PLATINUM BY NE TRON- ACTIVATION ANALYSIS

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

Morris, D.F.C.; Killick, R.A.

1963-11-01

A neutron-activation analysis method for the determination of traces of iron in samples of purified platinum is described. The nuclear reactor BEPO at Harwell was used as the neutron source. A rapid radiochemical separation procedure using carriers was employed to decontaminate the iron activity from most other induced activities. The analysis is completed by discriminated gamma scintillation counting. Results of analyses of seven samples of platinum are quoted. The method of analysis has the advantage that it obviates difficulties caused by reagent blanks or by contamination from traces of inactive iron after irradiation. Interference resulting from nuclear reactions of elementsmore » other than iron in the samples appears to be of no consequence. (auth)« less

The effect of as long-term Mars simulation on a microbial permafrost soil community and macromolecules such as DNA, polypeptides and cell wall components.

NASA Astrophysics Data System (ADS)

Finster, K.; Hansen, A.; Liengaard, L.; Kristoffersen, T.; Mikkelsen, K.; Merrison, J.; Lomstein, B.

Ten freeze-dried and homogenized samples of a 2300 years old Spitsbergen permafrost soil containing a complex microbial community were aseptically transferred to inert glass tubes and subjected to a 30 days Martian simulation experiment. During this period the samples received an UV dose equivalent to 80 Martian Sol. Data loggers in 4 out the ten samples monitored the temperature 0-2 mm below the surface of the sample. After removal from the simulation chamber, the samples were sliced in 1.5 to 6 mm thick horizons (H1, 0-1.5 mm; H2, 1.5-3 mm; H3, 3-6 mm; H4, 6-9 mm; H5, 9-15 mm; H6, 15-21 mm; H7, 21-27 mm and H8, 27-33 mm), resulting in 10 subsamples from each soil horizon. The subsamples from each horizon were pooled and used for the following investigations: 1. Determination of the bacterial number after staining with SYBR-gold, 2. Determination of the number of dead and living bacteria using the BacLight kit, 3. Determination of the total amount of extractable DNA, 4. Determination of the number of culturable aerobic and anaerobic bacteria, 5. Determination of the concentration of the total hydrolysable amino acids and D and L enantiomers, 6. Determination of the muramic acid contentration. The results of the experiments will be presented and discussed in our communication

Chemical Characterization of an Envelope A Sample from Hanford Tank 241-AN-103

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

Hay, M.S.

2000-08-23

A whole tank composite sample from Hanford waste tank 241-AN-103 was received at the Savannah River Technology Center (SRTC) and chemically characterized. Prior to characterization the sample was diluted to {approximately}5 M sodium concentration. The filtered supernatant liquid, the total dried solids of the diluted sample, and the washed insoluble solids obtained from filtration of the diluted sample were analyzed. A mass balance calculation of the three fractions of the sample analyzed indicate the analytical results appear relatively self-consistent for major components of the sample. However, some inconsistency was observed between results where more than one method of determination wasmore » employed and for species present in low concentrations. A direct comparison to previous analyses of material from tank 241-AN-103 was not possible due to unavailability of data for diluted samples of tank 241-AN-103 whole tank composites. However, the analytical data for other types of samples from 241-AN-103 we re mathematically diluted and compare reasonably with the current results. Although the segments of the core samples used to prepare the sample received at SRTC were combined in an attempt to produce a whole tank composite, determination of how well the results of the current analysis represent the actual composition of the Hanford waste tank 241-AN-103 remains problematic due to the small sample size and the large size of the non-homogenized waste tank.« less

Comparison of a specific HPLC determination of toxic aconite alkaloids in processed Radix aconiti with a titration method of total alkaloids.

PubMed

Csupor, Dezso; Borcsa, Botond; Heydel, Barbara; Hohmann, Judit; Zupkó, István; Ma, Yan; Widowitz, Ute; Bauer, Rudolf

2011-10-01

In traditional Chinese medicine, Aconitum (Ranunculaceae) roots are only applied after processing. Nevertheless, several cases of poisoning by improperly processed aconite roots have been reported. The aim of this study was to develop a reliable analytical method to assess the amount of toxic aconite alkaloids in commercial aconite roots, and to compare this method with the commonly used total alkaloid content determination by titration. The content of mesaconitine, aconitine, and hypaconitine in 16 commercial samples of processed aconite roots was determined by an HPLC method and the total alkaloid content by indirect titration. Five samples were selected for in vivo toxicological investigation. In most of the commercial samples, toxic alkaloids were not detectable, or only traces were found. In four samples, we could detect >0.04% toxic aconite alkaloids, the highest with a content of 0.16%. The results of HPLC analysis were compared with the results obtained by titration, and no correlation was found between the two methods. The in vivo results reassured the validity of the HPLC determination. Samples with mesaconitine, aconitine, and hypaconitine content below the HPLC detection limit still contained up to 0.2% alkaloids determined by titration. Since titration of alkaloids gives no information selectively on the aconitine-type alkaloid content and toxicity of aconite roots this method is not appropriate for safety assessment. The HPLC method developed by us provides a quick and reliable assessment of toxicity and should be considered as a purity test in pharmacopoeia monographs.

Quality Control for Ambient Sampling of PCDD/PCDF from Open Combustion Sources

EPA Science Inventory

Both long duration (> 6 h) and high temperature (up to 139o C) sampling efforts were conducted using ambient air sampling methods to determine if either high volume throughput or higher than ambient sampling temperatures resulted in loss of target polychlorinated dibenzodioxins/d...

Biostatistics Series Module 5: Determining Sample Size

PubMed Central

Hazra, Avijit; Gogtay, Nithya

2016-01-01

Determining the appropriate sample size for a study, whatever be its type, is a fundamental aspect of biomedical research. An adequate sample ensures that the study will yield reliable information, regardless of whether the data ultimately suggests a clinically important difference between the interventions or elements being studied. The probability of Type 1 and Type 2 errors, the expected variance in the sample and the effect size are the essential determinants of sample size in interventional studies. Any method for deriving a conclusion from experimental data carries with it some risk of drawing a false conclusion. Two types of false conclusion may occur, called Type 1 and Type 2 errors, whose probabilities are denoted by the symbols σ and β. A Type 1 error occurs when one concludes that a difference exists between the groups being compared when, in reality, it does not. This is akin to a false positive result. A Type 2 error occurs when one concludes that difference does not exist when, in reality, a difference does exist, and it is equal to or larger than the effect size defined by the alternative to the null hypothesis. This may be viewed as a false negative result. When considering the risk of Type 2 error, it is more intuitive to think in terms of power of the study or (1 − β). Power denotes the probability of detecting a difference when a difference does exist between the groups being compared. Smaller α or larger power will increase sample size. Conventional acceptable values for power and α are 80% or above and 5% or below, respectively, when calculating sample size. Increasing variance in the sample tends to increase the sample size required to achieve a given power level. The effect size is the smallest clinically important difference that is sought to be detected and, rather than statistical convention, is a matter of past experience and clinical judgment. Larger samples are required if smaller differences are to be detected. Although the principles are long known, historically, sample size determination has been difficult, because of relatively complex mathematical considerations and numerous different formulas. However, of late, there has been remarkable improvement in the availability, capability, and user-friendliness of power and sample size determination software. Many can execute routines for determination of sample size and power for a wide variety of research designs and statistical tests. With the drudgery of mathematical calculation gone, researchers must now concentrate on determining appropriate sample size and achieving these targets, so that study conclusions can be accepted as meaningful. PMID:27688437

Studies with sample conductivity, insertion rates, and particle deflection in a continuous flow electrophoresis system

NASA Technical Reports Server (NTRS)

Williams, G., Jr.

1982-01-01

The continuous flow electrophoresis system makes electrophoresis possible in a free-flowing film of aqueous electrolyte medium. The sample continuously enters the electrolyte at the top of the chamber and is subjected to the action of a lateral dc field. This divides the sample into fractions since each component has a distinctive electrophoretic mobility. Tests were made using monodisperse polystyrene latex microspheres to determine optimum sample conductivity, insertion rates and optimum electric field applications as baseline data for future STS flight experiments. Optimum sample flow rates for the selected samples were determined to be approximately 26 micro-liters/min. Experiments with samples in deionized water yielded best results and voltages in the 20 V/cm to 30 V/cm range were optimum. Deflections of formaldehyde fixed turkey and bovine erythrocytes were determined using the continuous flow electrophoresis system. The effects of particle interactions on sample resolution and migration in the chamber was also evaluated.

INAA Application for Trace Element Determination in Biological Reference Material

NASA Astrophysics Data System (ADS)

Atmodjo, D. P. D.; Kurniawati, S.; Lestiani, D. D.; Adventini, N.

2017-06-01

Trace element determination in biological samples is often used in the study of health and toxicology. Determination change to its essentiality and toxicity of trace element require an accurate determination method, which implies that a good Quality Control (QC) procedure should be performed. In this study, QC for trace element determination in biological samples was applied by analyzing the Standard Reference Material (SRM) Bovine muscle 8414 NIST using Instrumental Neutron Activation Analysis (INAA). Three selected trace element such as Fe, Zn, and Se were determined. Accuracy of the elements showed as %recovery and precision as %coefficient of variance (%CV). The result showed that %recovery of Fe, Zn, and Se were in the range between 99.4-107%, 92.7-103%, and 91.9-112%, respectively, whereas %CV were 2.92, 3.70, and 5.37%, respectively. These results showed that INAA method is precise and accurate for trace element determination in biological matrices.

Determination of inorganic elements in poppy straw by scanning electron microscopy with energy dispersive spectrometry as a means of ascertaining origin.

PubMed

Copur, E; Göger, N G; Orbey, T; Sener, B

2005-01-01

Cultivation of poppy as a source of opium alkaloids for legitimate medical purposes has a long tradition in Turkey. The main products are poppy straw and concentrate of poppy straw, obtained from dried poppy capsules. The aims of the study reported in the present article were to establish inorganic element profiles for the poppy-growing provinces of Turkey by means of x-ray analysis by scanning electron microscopy with energy dispersive spectrometry (SEM/EDS) and to explore the potential of the technique for determination of origin. Ten elements (sodium, magnesium, silicon, phosphorus, sulphur, chlorine, potassium, calcium, copper and zinc) were analysed in poppy straw samples from 67 towns in nine provinces. As regards the determination of origin, the most significant finding was the presence of copper and zinc in the poppy straw samples from 8 of the 15 towns in Afyon Province. Since those elements are not normally found in soil, it is assumed that their presence is the result of environmental (industrial) contamination. Differences in the samples from the other eight provinces were less significant, possibly a result of their geographical proximity. Nevertheless, differences in the samples were apparent. Because the findings are relative rather than absolute in terms of presence or absence of individual inorganic elements, further research is required to convert them into operationally usable results. The inorganic element profiles generated in the study have been used to form the basis for the development of a comprehensive database on poppy straw samples, which may be used in comparing samples and determining their origin.

Biomass Determination Using Wood Specific Gravity from Increment Cores

Treesearch

Michael C. Wiemann; G. Bruce Williamson

2013-01-01

Wood specific gravity (SG) is one of the most important variables used to determine biomass. Measurement of SG is problematic because it requires tedious, and often difficult, sampling of wood from standing trees. Sampling is complicated because the SG usually varies nonrandomly within trees, resulting in systematic errors. Off-center pith and hollow or decayed stems...

A new method for evaluating radon and thoron alpha-activities per unit volume inside and outside various natural material samples by calculating SSNTD detection efficiencies for the emitted alpha-particles and measuring the resulting track densities.

PubMed

Misdaq, M A; Aitnouh, F; Khajmi, H; Ezzahery, H; Berrazzouk, S

2001-08-01

A Monte Carlo computer code for determining detection efficiencies of the CR-39 and LR-115 II solid-state nuclear track detectors (SSNTD) for alpha-particles emitted by the uranium and thorium series inside different natural material samples was developed. The influence of the alpha-particle initial energy on the SSNTD detection efficiencies was investigated. Radon (222Rn) and thoron (220Rn) alpha-activities per unit volume were evaluated inside and outside the natural material samples by exploiting data obtained for the detection efficiencies of the SSNTD utilized for the emitted alpha-particles, and measuring the resulting track densities. Results obtained were compared to those obtained by other methods. Radon emanation coefficients have been determined for some of the considered material samples.

Determination of Multiple Near-Surface Residual Stress Components in Laser Peened Aluminum Alloy via the Contour Method

NASA Astrophysics Data System (ADS)

Toparli, M. Burak; Fitzpatrick, Michael E.; Gungor, Salih

2015-09-01

In this study, residual stress fields, including the near-surface residual stresses, were determined for an Al7050-T7451 sample after laser peening. The contour method was applied to measure one component of the residual stress, and the relaxed stresses on the cut surfaces were then measured by X-ray diffraction. This allowed calculation of the three orthogonal stress components using the superposition principle. The near-surface results were validated with results from incremental hole drilling and conventional X-ray diffraction. The results demonstrate that multiple residual stress components can be determined using a combination of the contour method and another technique. If the measured stress components are congruent with the principal stress axes in the sample, then this allows for determination of the complete stress tensor.

Measuring solids concentration in stormwater runoff: comparison of analytical methods.

PubMed

Clark, Shirley E; Siu, Christina Y S

2008-01-15

Stormwater suspended solids typically are quantified using one of two methods: aliquot/subsample analysis (total suspended solids [TSS]) or whole-sample analysis (suspended solids concentration [SSC]). Interproject comparisons are difficult because of inconsistencies in the methods and in their application. To address this concern, the suspended solids content has been measured using both methodologies in many current projects, but the question remains about how to compare these values with historical water-quality data where the analytical methodology is unknown. This research was undertaken to determine the effect of analytical methodology on the relationship between these two methods of determination of the suspended solids concentration, including the effect of aliquot selection/collection method and of particle size distribution (PSD). The results showed that SSC was best able to represent the known sample concentration and that the results were independent of the sample's PSD. Correlations between the results and the known sample concentration could be established for TSS samples, but they were highly dependent on the sample's PSD and on the aliquot collection technique. These results emphasize the need to report not only the analytical method but also the particle size information on the solids in stormwater runoff.

Visual accumulation tube for size analysis of sands

USGS Publications Warehouse

Colby, B.C.; Christensen, R.P.

1956-01-01

The visual-accumulation-tube method was developed primarily for making size analyses of the sand fractions of suspended-sediment and bed-material samples. Because the fundamental property governing the motion of a sediment particle in a fluid is believed to be its fall velocity. the analysis is designed to determine the fall-velocity-frequency distribution of the individual particles of the sample. The analysis is based on a stratified sedimentation system in which the sample is introduced at the top of a transparent settling tube containing distilled water. The procedure involves the direct visual tracing of the height of sediment accumulation in a contracted section at the bottom of the tube. A pen records the height on a moving chart. The method is simple and fast, provides a continuous and permanent record, gives highly reproducible results, and accurately determines the fall-velocity characteristics of the sample. The apparatus, procedure, results, and accuracy of the visual-accumulation-tube method for determining the sedimentation-size distribution of sands are presented in this paper.

Evaluation of a gas chromatography method for azelaic acid determination in selected biological samples

PubMed Central

Garelnabi, Mahdi; Litvinov, Dmitry; Parthasarathy, Sampath

2010-01-01

Background: Azelaic acid (AzA) is the best known dicarboxilic acid to have pharmaceutical benefits and clinical applications and also to be associated with some diseases pathophysiology. Materials and Methods: We extracted and methylesterified AzA and determined its concentration in human plasma obtained from healthy individuals and also in mice fed AzA containing diet for three months. Results: AzA was detected in Gas Chromatography (GC) and confirmed by Liquid chromatography mass spectrometry (LCMS), and gas chromatography mass spectrometry (GCMC). Our results have shown that AzA can be determined efficiently in selected biological samples by GC method with 1nM limit of detection (LoD) and the limit of quantification (LoQ); was established at 50nM. Analytical Sensitivity as assayed by hexane demonstrated an analytical sensitivity at 0.050nM. The method has demonstrated 8-10% CV batch repeatability across the sample types and 13-18.9% CV for the Within-Lab Precision analysis. The method has shown that AzA can efficiently be recovered from various sample preparation including liver tissue homogenate (95%) and human plasma (97%). Conclusions: Because of its simplicity and lower limit of quantification, the present method provides a useful tool for determining AzA in various biological sample preparations. PMID:22558586

Determination of total tin in geological materials by electrothermal atomic-absorption spectrophotometry using a tungsten-impregnated graphite furnace

USGS Publications Warehouse

Zhou, L.; Chao, T.T.; Meier, A.L.

1984-01-01

An electrothermal atomic-absorption spectrophotometric method is described for the determination of total tin in geological materials, with use of a tungsten-impregnated graphite furnace. The sample is decomposed by fusion with lithium metaborate and the melt is dissolved in 10% hydrochloric acid. Tin is then extracted into trioctylphosphine oxide-methyl isobutyl ketone prior to atomization. Impregnation of the furnace with a sodium tungstate solution increases the sensitivity of the determination and improves the precision of the results. The limits of determination are 0.5-20 ppm of tin in the sample. Higher tin values can be determined by dilution of the extract. Replicate analyses of eighteen geological reference samples with diverse matrices gave relative standard deviations ranging from 2.0 to 10.8% with an average of 4.6%. Average tin values for reference samples were in general agreement with, but more precise than, those reported by others. Apparent recoveries of tin added to various samples ranged from 95 to 111% with an average of 102%. ?? 1984.

Energy dispersive X-ray fluorescence spectrometry for the direct multi-element analysis of dried blood spots

NASA Astrophysics Data System (ADS)

Marguí, E.; Queralt, I.; García-Ruiz, E.; García-González, E.; Rello, L.; Resano, M.

2018-01-01

Home-based collection protocols for clinical specimens are actively pursued as a means of improving life quality of patients. In this sense, dried blood spots (DBS) are proposed as a non-invasive and even self-administered alternative to sampling whole venous blood. This contribution explores the potential of energy dispersive X-ray fluorescence spectrometry for the simultaneous and direct determination of some major (S, Cl, K, Na), minor (P, Fe) and trace (Ca, Cu, Zn) elements in blood, after its deposition onto clinical filter papers, thus giving rise to DBS. For quantification purposes the best strategy was to use matrix-matched blood samples of known analyte concentrations. The accuracy and precision of the method were evaluated by analysis of a blood reference material (Seronorm™ trace elements whole blood L3). Quantitative results were obtained for the determination of P, S, Cl, K and Fe, and limits of detection for these elements were adequate, taking into account their typical concentrations in real blood samples. Determination of Na, Ca, Cu and Zn was hampered by the occurrence of high sample support (Na, Ca) and instrumental blanks (Cu, Zn). Therefore, the quantitative determination of these elements at the levels expected in blood samples was not feasible. The methodology developed was applied to the analysis of several blood samples and the results obtained were compared with those reported by standard techniques. Overall, the performance of the method developed is promising and it could be used to determine the aforementioned elements in blood samples in a simple, fast and economic way. Furthermore, its non-destructive nature enables further analyses by means of complementary techniques to be carried out.

Determination of HIV Status in African Adults With Discordant HIV Rapid Tests.

PubMed

Fogel, Jessica M; Piwowar-Manning, Estelle; Donohue, Kelsey; Cummings, Vanessa; Marzinke, Mark A; Clarke, William; Breaud, Autumn; Fiamma, Agnès; Donnell, Deborah; Kulich, Michal; Mbwambo, Jessie K K; Richter, Linda; Gray, Glenda; Sweat, Michael; Coates, Thomas J; Eshleman, Susan H

2015-08-01

In resource-limited settings, HIV infection is often diagnosed using 2 rapid tests. If the results are discordant, a third tie-breaker test is often used to determine HIV status. This study characterized samples with discordant rapid tests and compared different testing strategies for determining HIV status in these cases. Samples were previously collected from 173 African adults in a population-based survey who had discordant rapid test results. Samples were classified as HIV positive or HIV negative using a rigorous testing algorithm that included two fourth-generation tests, a discriminatory test, and 2 HIV RNA tests. Tie-breaker tests were evaluated, including rapid tests (1 performed in-country), a third-generation enzyme immunoassay, and two fourth-generation tests. Selected samples were further characterized using additional assays. Twenty-nine samples (16.8%) were classified as HIV positive and 24 of those samples (82.8%) had undetectable HIV RNA. Antiretroviral drugs were detected in 1 sample. Sensitivity was 8.3%-43% for the rapid tests; 24.1% for the third-generation enzyme immunoassay; 95.8% and 96.6% for the fourth-generation tests. Specificity was lower for the fourth-generation tests than the other tests. Accuracy ranged from 79.5% to 91.3%. In this population-based survey, most HIV-infected adults with discordant rapid tests were virally suppressed without antiretroviral drugs. Use of individual assays as tie-breaker tests was not a reliable method for determining HIV status in these individuals. More extensive testing algorithms that use a fourth-generation screening test with a discriminatory test and HIV RNA test are preferable for determining HIV status in these cases.

Using soil test results to determine fertilizer applications

Treesearch

C. B. Davey

2002-01-01

Using soil test results is a very useful practice IF the sample(s) of soil are good representations of the nursery soil. The lab results can be no more accurate than the samples submitted, and IF you know the texture of the nursery soil, and IF you know which soil extractant was used by the lab, and IF you know what crop is to be grown, and IF, for trees, which species...

Determination of geostatistically representative sampling locations in Porsuk Dam Reservoir (Turkey)

NASA Astrophysics Data System (ADS)

Aksoy, A.; Yenilmez, F.; Duzgun, S.

2013-12-01

Several factors such as wind action, bathymetry and shape of a lake/reservoir, inflows, outflows, point and diffuse pollution sources result in spatial and temporal variations in water quality of lakes and reservoirs. The guides by the United Nations Environment Programme and the World Health Organization to design and implement water quality monitoring programs suggest that even a single monitoring station near the center or at the deepest part of a lake will be sufficient to observe long-term trends if there is good horizontal mixing. In stratified water bodies, several samples can be required. According to the guide of sampling and analysis under the Turkish Water Pollution Control Regulation, a minimum of five sampling locations should be employed to characterize the water quality in a reservoir or a lake. The European Union Water Framework Directive (2000/60/EC) states to select a sufficient number of monitoring sites to assess the magnitude and impact of point and diffuse sources and hydromorphological pressures in designing a monitoring program. Although existing regulations and guidelines include frameworks for the determination of sampling locations in surface waters, most of them do not specify a procedure in establishment of monitoring aims with representative sampling locations in lakes and reservoirs. In this study, geostatistical tools are used to determine the representative sampling locations in the Porsuk Dam Reservoir (PDR). Kernel density estimation and kriging were used in combination to select the representative sampling locations. Dissolved oxygen and specific conductivity were measured at 81 points. Sixteen of them were used for validation. In selection of the representative sampling locations, care was given to keep similar spatial structure in distributions of measured parameters. A procedure was proposed for that purpose. Results indicated that spatial structure was lost under 30 sampling points. This was as a result of varying water quality in the reservoir due to inflows, point and diffuse inputs, and reservoir hydromorphology. Moreover, hot spots were determined based on kriging and standard error maps. Locations of minimum number of sampling points that represent the actual spatial structure of DO distribution in the Porsuk Dam Reservoir

Mass load estimation errors utilizing grab sampling strategies in a karst watershed

USGS Publications Warehouse

Fogle, A.W.; Taraba, J.L.; Dinger, J.S.

2003-01-01

Developing a mass load estimation method appropriate for a given stream and constituent is difficult due to inconsistencies in hydrologic and constituent characteristics. The difficulty may be increased in flashy flow conditions such as karst. Many projects undertaken are constrained by budget and manpower and do not have the luxury of sophisticated sampling strategies. The objectives of this study were to: (1) examine two grab sampling strategies with varying sampling intervals and determine the error in mass load estimates, and (2) determine the error that can be expected when a grab sample is collected at a time of day when the diurnal variation is most divergent from the daily mean. Results show grab sampling with continuous flow to be a viable data collection method for estimating mass load in the study watershed. Comparing weekly, biweekly, and monthly grab sampling, monthly sampling produces the best results with this method. However, the time of day the sample is collected is important. Failure to account for diurnal variability when collecting a grab sample may produce unacceptable error in mass load estimates. The best time to collect a sample is when the diurnal cycle is nearest the daily mean.

Quantitative surface topography determination by Nomarski reflection microscopy. 2: Microscope modification, calibration, and planar sample experiments

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

Hartman, J.S.; Gordon, R.L.; Lessor, D.L.

1980-09-01

The application of reflective Nomarski differential interference contrast microscopy for the determination of quantitative sample topography data is presented. The discussion includes a review of key theoretical results presented previously plus the experimental implementation of the concepts using a commercial Momarski microscope. The experimental work included the modification and characterization of a commercial microscope to allow its use for obtaining quantitative sample topography data. System usage for the measurement of slopes on flat planar samples is also discussed. The discussion has been designed to provide the theoretical basis, a physical insight, and a cookbook procedure for implementation to allow thesemore » results to be of value to both those interested in the microscope theory and its practical usage in the metallography laboratory.« less

Identification of offal adulteration in beef by laser induced breakdown spectroscopy (LIBS).

PubMed

Velioglu, Hasan Murat; Sezer, Banu; Bilge, Gonca; Baytur, Süleyman Efe; Boyaci, Ismail Hakki

2018-04-01

Minced meat is the major ingredient in sausages, beef burgers, and similar products; and thus it is the main product subjected to adulteration with meat offal. Determination of this kind of meat adulteration is crucial due to religious, economic and ethical concerns. The aim of the present study is to discriminate the beef meat and offal samples by using laser induced breakdown spectroscopy (LIBS). To this end, LIBS and multivariate data analysis were used to discriminate pure beef and offal samples qualitatively and to determine the offal mixture adulteration quantitatively. In this analysis, meat samples were frozen and LIBS analysis were performed. The results indicate that by using principal component analysis (PCA), discrimination of pure offal and offal mixture adulterated beef samples can be achieved successfully. Besides, adulteration ratio can be determined using partial least square analysis method (PLS) with 0.947 coefficient of determination (R 2 ) and 3.8% of limit of detection (LOD) values for offal mixture adulterated beef samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

Determination of the Landau Lifshitz damping parameter of composite magnetic fluids

NASA Astrophysics Data System (ADS)

Fannin, P. C.; Malaescu, I.; Marin, C. N.

2007-01-01

Measurements of the frequency dependent, complex magnetic susceptibility, χ(ω)= χ‧( ω)- iχ″( ω), in the GHz range, are used to investigate the effect which the mixing of two different magnetic fluids has on the value of the damping parameter, α, of the Landau-Lifshitz equation. The magnetic fluid samples investigated in this study were three kerosene-based magnetic fluids, stabilised with oleic acid, denoted as MF1, MF2 and MF3. Sample MF1 was a magnetic fluid with Mn 0.6Fe 0.4Fe 2O 4 particles, sample MF2 was a magnetic fluid with Ni 0.4Zn 0.6Fe 2O 4 particles and sample MF3 was a composite magnetic fluid obtained by mixing a part of sample MF1 with a part of sample MF2, in proportion of 1:1. The experimental results revealed that the value of the damping parameter of the composite sample (sample MF3) is between the α values obtained for its constituents (samples MF1 and MF2). Based on the superposition principle, which states that the susceptibility of a magnetic fluid sample is a superposition of individual contributions of the magnetic particles, a theoretical model is proposed. The experimental results are shown to be in close agreement with the theoretical results. This result is potentially useful in the design of microwave-operating materials, in that it enables one to determine a particular value of damping parameter.

Cadmium, lead, tin, total mercury, and methylmercury in canned tuna commercialised in São Paulo, Brazil.

PubMed

de Paiva, Esther Lima; Morgano, Marcelo Antonio; Milani, Raquel Fernanda

2017-09-01

The objective of this work was to determine levels of inorganic contaminants in 30 samples of five commercial brands of canned tuna, acquired on the local market in Campinas, São Paulo, Brazil, in the year of 2015. Total mercury and methylmercury (MeHg+) were determined by atomic absorption with thermal decomposition and amalgamation; and cadmium, lead, and tin were determined by inductively coupled plasma optical emission spectrometry. Results indicated that 20% of the tuna samples surpassed limits determined by the Brazilian and European Commission legislation for cadmium; for lead, the maximum value found was 59 µg kg -1 and tin was not detected in any samples. The maximum values found for total Hg and MeHg+ were 261 and 258 µg kg -1 , respectively. As from the results obtained, it was estimated that the consumption of four cans per week (540 g) of tuna canned in water could surpass the provisional tolerable monthly intake for MeHg + by 100%.

Usage of CT data in biomechanical research

NASA Astrophysics Data System (ADS)

Safonov, Roman A.; Golyadkina, Anastasiya A.; Kirillova, Irina V.; Kossovich, Leonid Y.

2017-02-01

Object of study: The investigation is focused on development of personalized medicine. The determination of mechanical properties of bone tissues based on in vivo data was considered. Methods: CT, MRI, natural experiments on versatile test machine Instron 5944, numerical experiments using Python programs. Results: The medical diagnostics methods, which allows determination of mechanical properties of bone tissues based on in vivo data. The series of experiments to define the values of mechanical parameters of bone tissues. For one and the same sample, computed tomography (CT), magnetic resonance imaging (MRI), ultrasonic investigations and mechanical experiments on single-column test machine Instron 5944 were carried out. The computer program for comparison of CT and MRI images was created. The grayscale values in the same points of the samples were determined on both CT and MRI images. The Haunsfield grayscale values were used to determine rigidity (Young module) and tensile strength of the samples. The obtained data was compared to natural experiments results for verification.

Probability of detecting nematode infestations for quarantine sampling with imperfect extraction efficacy

PubMed Central

Chen, Peichen; Liu, Shih-Chia; Liu, Hung-I; Chen, Tse-Wei

2011-01-01

For quarantine sampling, it is of fundamental importance to determine the probability of finding an infestation when a specified number of units are inspected. In general, current sampling procedures assume 100% probability (perfect) of detecting a pest if it is present within a unit. Ideally, a nematode extraction method should remove all stages of all species with 100% efficiency regardless of season, temperature, or other environmental conditions; in practice however, no method approaches these criteria. In this study we determined the probability of detecting nematode infestations for quarantine sampling with imperfect extraction efficacy. Also, the required sample and the risk involved in detecting nematode infestations with imperfect extraction efficacy are presented. Moreover, we developed a computer program to calculate confidence levels for different scenarios with varying proportions of infestation and efficacy of detection. In addition, a case study, presenting the extraction efficacy of the modified Baermann's Funnel method on Aphelenchoides besseyi, is used to exemplify the use of our program to calculate the probability of detecting nematode infestations in quarantine sampling with imperfect extraction efficacy. The result has important implications for quarantine programs and highlights the need for a very large number of samples if perfect extraction efficacy is not achieved in such programs. We believe that the results of the study will be useful for the determination of realistic goals in the implementation of quarantine sampling. PMID:22791911

Determining the 40K radioactivity in rocks using x-ray spectrometry

NASA Astrophysics Data System (ADS)

Pilakouta, M.; Kallithrakas-Kontos, N.; Nikolaou, G.

2017-09-01

In this paper we propose an experimental method for the determination of potassium-40 (40K) radioactivity in commercial granite samples using x-ray fluorescence (XRF). The method correlates the total potassium concentration (yield) in samples deduced by XRF analysis with the radioactivity of the sample due to the 40K radionuclide. This method can be used in an undergraduate student laboratory. A brief theoretical background and description of the method, as well as some results and their interpretation, are presented.

Aerial Sampling of Emissions from Biomass Pile Burns in ...

EPA Pesticide Factsheets

Abstract (already cleared). Emissions from burning piles of post-harvest timber slash in Grande Ronde, Oregon were sampled using an instrument platform lofted into the plume using a tether-controlled aerostat or balloon. Emissions of carbon monoxide, carbon dioxide, methane, particulate matter (PM2.5 µm), black carbon, ultraviolet absorbing PM, elemental/organic carbon, semi-volatile organics (polycyclic aromatic hydrocarbons and polychlorinated dibenzodioxins/dibenzofurans), filter-based metals, and volatile organics were sampled for determination of emission factors. The effect on emissions from covering or not covering piles with polyethylene sheets to prevent fuel wetting was determined. Results showed that the uncovered (“wet”) piles burned with lower combustion efficiency and higher emissions of volatile organic compounds. Results for other pollutants will also be discussed. This work determines the first known in-field emission factors for burning of timber slash piles. The results also document the effect on emissions of covering the piles with polyethylene covers to reduce the moisture content of the biomass.

High purity polyimide analysis by solid sampling graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Santos, Rafael F.; Carvalho, Gabriel S.; Duarte, Fabio A.; Bolzan, Rodrigo C.; Flores, Erico M. M.

2017-03-01

In this work, Cr, Cu, Mn, Na and Ni were determined in high purity polyimides (99.5%) by solid sampling graphite furnace atomic absorption spectrometry (SS-GFAAS) using Zeeman effect background correction system with variable magnetic field, making possible the simultaneous measurement at high or low sensitivity. The following analytical parameters were evaluated: pyrolysis and atomization temperatures, feasibility of calibration with aqueous solution, linear calibration range, sample mass range and the use of chemical modifier. Calibration with aqueous standard solutions was feasible for all analytes. No under or overestimated results were observed and up to 10 mg sample could be introduced on the platform for the determination of Cr, Cu, Mn, Na and Ni. The relative standard deviation ranged from 3 to 20%. The limits of detection (LODs) achieved using the high sensitivity mode were as low as 7.0, 2.5, 1.7, 17 and 0.12 ng g- 1 for Cr, Cu, Mn, Na and Ni, respectively. No addition of chemical modifier was necessary, except for Mn determination where Pd was required. The accuracy was evaluated by analyte spike and by comparison of the results with those obtained by inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry after microwave-assisted digestion in a single reaction chamber system and also by neutron activation analysis. No difference among the results obtained by SS-GFAAS and those obtained by alternative analytical methods using independent techniques. SS-GFAAS method showed some advantages, such as the determination of metallic contaminants in high purity polyimides with practically no sample preparation, very low LODs, calibration with aqueous standards and determination in a wide range of concentration.

Innovative application of the moisture analyzer for determination of dry mass content of processed cheese

NASA Astrophysics Data System (ADS)

Kowalska, Małgorzata; Janas, Sławomir; Woźniak, Magdalena

2018-04-01

The aim of this work was the presentation of an alternative method of determination of the total dry mass content in processed cheese. The authors claim that the presented method can be used in industry's quality control laboratories for routine testing and for quick in-process control. For the test purposes both reference method of determination of dry mass in processed cheese and moisture analyzer method were used. The tests were carried out for three different kinds of processed cheese. In accordance with the reference method, the sample was placed on a layer of silica sand and dried at the temperature of 102 °C for about 4 h. The moisture analyzer test required method validation, with regard to drying temperature range and mass of the analyzed sample. Optimum drying temperature of 110 °C was determined experimentally. For Hochland cream processed cheese sample, the total dry mass content, obtained using the reference method, was 38.92%, whereas using the moisture analyzer method, it was 38.74%. An average analysis time in case of the moisture analyzer method was 9 min. For the sample of processed cheese with tomatoes, the reference method result was 40.37%, and the alternative method result was 40.67%. For the sample of cream processed cheese with garlic the reference method gave value of 36.88%, and the alternative method, of 37.02%. An average time of those determinations was 16 min. Obtained results confirmed that use of moisture analyzer is effective. Compliant values of dry mass content were obtained for both of the used methods. According to the authors, the fact that the measurement took incomparably less time for moisture analyzer method, is a key criterion of in-process control and final quality control method selection.

Estimation of reference intervals from small samples: an example using canine plasma creatinine.

PubMed

Geffré, A; Braun, J P; Trumel, C; Concordet, D

2009-12-01

According to international recommendations, reference intervals should be determined from at least 120 reference individuals, which often are impossible to achieve in veterinary clinical pathology, especially for wild animals. When only a small number of reference subjects is available, the possible bias cannot be known and the normality of the distribution cannot be evaluated. A comparison of reference intervals estimated by different methods could be helpful. The purpose of this study was to compare reference limits determined from a large set of canine plasma creatinine reference values, and large subsets of this data, with estimates obtained from small samples selected randomly. Twenty sets each of 120 and 27 samples were randomly selected from a set of 1439 plasma creatinine results obtained from healthy dogs in another study. Reference intervals for the whole sample and for the large samples were determined by a nonparametric method. The estimated reference limits for the small samples were minimum and maximum, mean +/- 2 SD of native and Box-Cox-transformed values, 2.5th and 97.5th percentiles by a robust method on native and Box-Cox-transformed values, and estimates from diagrams of cumulative distribution functions. The whole sample had a heavily skewed distribution, which approached Gaussian after Box-Cox transformation. The reference limits estimated from small samples were highly variable. The closest estimates to the 1439-result reference interval for 27-result subsamples were obtained by both parametric and robust methods after Box-Cox transformation but were grossly erroneous in some cases. For small samples, it is recommended that all values be reported graphically in a dot plot or histogram and that estimates of the reference limits be compared using different methods.

Evaluation of direct saponification method for determination of cholesterol in meats.

PubMed

Adams, M L; Sullivan, D M; Smith, R L; Richter, E F

1986-01-01

A gas chromatographic (GC) method has been developed for determination of cholesterol in meats. The method involves ethanolic KOH saponification of the sample material, homogeneous-phase toluene extraction of the unsaponifiables, derivatization of cholesterol to its trimethylsilylether, and quantitation by GC-flame ionization detection using 5-alpha-cholestane as internal standard. This direct saponification method is compared with the current AOAC official method for determination of cholesterol in 20 different meat products. The direct saponification method eliminates the need for initial lipid extraction, thus offering a 30% savings in labor, and requires fewer solvents than the AOAC method. It produced comparable or slightly higher cholesterol results than the AOAC method in all meat samples examined. Precision, determined by assaying a turkey meat sample 16 times over 4 days, was excellent (CV = 1.74%). Average recovery of cholesterol added to meat samples was 99.8%.

Determination of the molar mass of argon from high-precision acoustic comparisons.

PubMed

Feng, X J; Zhang, J T; Moldover, M R; Yang, I; Plimmer, M D; Lin, H

2017-06-01

This article describes the accurate determination of the molar mass M of a sample of argon gas used for the determination of the Boltzmann constant. The method of one of the authors (Moldover et al 1988 J. Res. Natl. Bur. Stand. 93 85-144) uses the ratio of the square speed of sound in the gas under analysis and in a reference sample of known molar mass. A sample of argon that was isotopically-enriched in 40 Ar was used as the reference, whose unreactive impurities had been independently measured. The results for three gas samples are in good agreement with determinations by gravimetric mass spectrometry; (〈 M acoustic / M mass-spec 〉 - 1) = (-0.31 ± 0.69) × 10 -6 , where the indicated uncertainty is one standard deviation that does not account for the uncertainties from the acoustic and mass-spectroscopy references.

Determination of the molar mass of argon from high-precision acoustic comparisons

PubMed Central

Feng, X J; Zhang, J T; Moldover, M R; Yang, I; Plimmer, M D; Lin, H

2017-01-01

This article describes the accurate determination of the molar mass M of a sample of argon gas used for the determination of the Boltzmann constant. The method of one of the authors (Moldover et al 1988 J. Res. Natl. Bur. Stand. 93 85–144) uses the ratio of the square speed of sound in the gas under analysis and in a reference sample of known molar mass. A sample of argon that was isotopically-enriched in 40Ar was used as the reference, whose unreactive impurities had been independently measured. The results for three gas samples are in good agreement with determinations by gravimetric mass spectrometry; (〈Macoustic/Mmass-spec〉 − 1) = (−0.31 ± 0.69) × 10−6, where the indicated uncertainty is one standard deviation that does not account for the uncertainties from the acoustic and mass-spectroscopy references. PMID:29332953

RECOMMENDATIONS FOR SAMPLING OF TANK 19 IN F TANK FARM

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

Harris, S.; Shine, G.

2009-12-14

Representative sampling is required for characterization of the residual material in Tank 19 prior to operational closure. Tank 19 is a Type IV underground waste storage tank located in the F-Tank Farm. It is a cylindrical-shaped, carbon steel tank with a diameter of 85 feet, a height of 34.25 feet, and a working capacity of 1.3 million gallons. Tank 19 was placed in service in 1961 and initially received a small amount of low heat waste from Tank 17. It then served as an evaporator concentrate (saltcake) receiver from February 1962 to September 1976. Tank 19 also received the spentmore » zeolite ion exchange media from a cesium removal column that once operated in the Northeast riser of the tank to remove cesium from the evaporator overheads. Recent mechanical cleaning of the tank removed all mounds of material. Anticipating a low level of solids in the residual waste, Huff and Thaxton [2009] developed a plan to sample the waste during the final clean-up process while it would still be resident in sufficient quantities to support analytical determinations in four quadrants of the tank. Execution of the plan produced fewer solids than expected to support analytical determinations in all four quadrants. Huff and Thaxton [2009] then restructured the plan to characterize the residual separately in the North and the South regions: two 'hemispheres.' This document provides sampling recommendations to complete the characterization of the residual material on the tank bottom following the guidance in Huff and Thaxton [2009] to split the tank floor into a North and a South hemisphere. The number of samples is determined from a modification of the formula previously published in Edwards [2001] and the sample characterization data for previous sampling of Tank 19 described by Oji [2009]. The uncertainty is quantified by an upper 95% confidence limit (UCL95%) on each analyte's mean concentration in Tank 19. The procedure computes the uncertainty in analyte concentration as a function of the number of samples, and the final number of samples is determined when the reduction in the uncertainty from an additional sample no longer has a practical impact on results. The characterization of the full suite of analytes in the North and South hemispheres is currently supported by a single Mantis rover sample in each hemisphere. A floor scrape sample was obtained from a compact region near the center riser slightly in the South hemisphere and has been analyzed for a shortened list of key analytes. There is not enough additional material from the floor scrape sample material for completing the full suite of constituents. No floor scrape samples have been previously taken from the North hemisphere. The criterion to determine the number of additional samples was based on the practical reduction in the uncertainty when a new sample is added. This was achieved when five additional samples are obtained. In addition, two archived samples will be used if a contingency such as failing to demonstrate the comparability of the Mantis samples to the floor scrape samples occurs. To complete sampling of the Tank 19 residual floor material, four additional samples should be taken from the North hemisphere and four additional samples should be taken from the South hemisphere. One of the samples from each hemisphere will be archived in case of need. Three of the four additional samples from each hemisphere will be analyzed. Once the results are available, differences between the Mantis and three floor scrape sample results will be evaluated. If there are no statistically significant analyte concentration differences between the Mantis and floor scrape samples, those results will be combined and then UCL95%s will be calculated. If the analyte concentration differences between the Mantis and floor scrape samples are statistically significant, the UCL95%s will be calculated without the Mantis sample results. If further reduction in the upper confidence limits is needed and can be achieved by the addition of the archived samples, they will be analyzed and included in the statistical computations. Initially the analyte concentrations in the residual material on the floor of Tank 19 will be determined separately in the North and the South hemispheres. However, if final sampling results show that differences between the North and South samples are consistent within sampling variation, then the final computations can be based on consolidating all sample results from the tank floor. Recommended locations may be subject to physical tank access and sampling constraints for the additional samples. The recommendations have been discussed in Section 4 and are based on partitioning the Tank 19 floor into an inner and an outer ring and six 60{sup o} sectors depicted in Figure 1. The location of the border between the inner and outer rings is based on dividing the residual material into two approximately equal volumes.« less

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

E.N. Stepanov; I.I. Mel'nikov; V.P. Gridasov

In active production at OAO Magnitogorskii Metallurgicheskii Kombinat (MMK), samples of melt materials were taken during shutdown and during planned repairs at furnaces 1 and 8. In particular, coke was taken from the tuyere zone at different distances from the tuyere tip. The mass of the point samples was 2-15 kg, depending on the sampling zone. The material extracted from each zone underwent magnetic separation and screening by size class. The resulting coke sample was averaged out and divided into parts: one for determining the granulometric composition and mechanical strength; and the other for technical analysis and determination of themore » physicochemical properties of the coke.« less

A "three-in-one" sample preparation method for simultaneous determination of B-group water-soluble vitamins in infant formula using VitaFast(®) kits.

PubMed

Zhang, Heng; Lan, Fang; Shi, Yupeng; Wan, Zhi-Gang; Yue, Zhen-Feng; Fan, Fang; Lin, Yan-Kui; Tang, Mu-Jin; Lv, Jing-Zhang; Xiao, Tan; Yi, Changqing

2014-06-15

VitaFast(®) test kits designed for the microbiological assay in microtiter plate format can be applied to quantitative determination of B-group water-soluble vitamins such as vitamin B12, folic acid and biotin, et al. Compared to traditional microbiological methods, VitaFast(®) kits significantly reduce sample processing time and provide greater reliability, higher productivity and better accuracy. Recently, simultaneous determination of vitamin B12, folic acid and biotin in one sample is urgently required when evaluating the quality of infant formulae in our practical work. However, the present sample preparation protocols which are developed for individual test systems, are incompatible with simultaneous determination of several analytes. To solve this problem, a novel "three-in-one" sample preparation method is herein developed for simultaneous determination of B-group water-soluble vitamins using VitaFast(®) kits. The performance of this novel "three-in-one" sample preparation method was systematically evaluated through comparing with individual sample preparation protocols. The experimental results of the assays which employed "three-in-one" sample preparation method were in good agreement with those obtained from conventional VitaFast(®) extraction methods, indicating that the proposed "three-in-one" sample preparation method is applicable to the present three VitaFast(®) vitamin test systems, thus offering a promising alternative for the three independent sample preparation methods. The proposed new sample preparation method will significantly improve the efficiency of infant formulae inspection. Copyright © 2013 Elsevier Ltd. All rights reserved.

Rare earths and other trace elements in Luna 16 soil.

NASA Technical Reports Server (NTRS)

Helmke, P. A.; Haskin, L. A.

1972-01-01

An analysis has been made of four small samples of material brought to earth by the Luna 16 mission, with the aim to determine rare earths and other trace elements in these samples. The analytical results are tabulated, and the rare earth abundances are compared with the average for chondrites. A comparison is also made with the results of similar analyses of Apollo samples.

Laboratory simulation of the effects of overburden stress on the specific storage of shallow artesian aquifers

USGS Publications Warehouse

Sepúlveda, Nicasio; Zack, A.L.; Krishna, J.H.; Quinones-Aponte, Vicente; Gomez-Gomez, Fernando; Morris, G.L.

1990-01-01

A laboratory experiment to measure the specific storage of an aquifer material was conducted. A known dead load, simulating an overburden load, was applied to a sample of completely saturated aquifer material contained inside a cylinder. After the dead load was applied, water was withdrawn from the sample, causing the hydrostatic pressure to decrease and the effective stress to increase. The resulting compression of the sample and the amount of water withdrawn were measured after equilibrium was reached. The procedure was repeated by increasing the dead load and the hydrostatic pressure followed by withdrawing water to determine new values of effective stress and compaction. The simulated dead loads are typical of those experienced by shallow artesian aquifers. The void ratio and the effective stress of the aquifer sample, as simulated by different dead loads, determine the pore volume compressibility which, in turn, determines the values of specific storage. An analytical algorithm was used to independently determine the stress dependent profile of specific storage. These values are found to be in close agreement with laboratory results. Implications for shallow artesian aquifers, with relatively small overburden stress, are also addressed.

Spectrophotometric methods for the determination of urea in real samples using silver nanoparticles by standard addition and 2nd order derivative methods

NASA Astrophysics Data System (ADS)

Ali, Nauman; Ismail, Muhammad; Khan, Adnan; Khan, Hamayun; Haider, Sajjad; Kamal, Tahseen

2018-01-01

In this work, we have developed simple, sensitive and inexpensive methods for the spectrophotometric determination of urea in urine samples using silver nanoparticles (AgNPs). The standard addition and 2nd order derivative methods were adopted for this purpose. AgNPs were prepared by chemical reduction of AgNO3 with hydrazine using 1,3-di-(1H-imidazol-1-yl)-2-propanol (DIPO) as a stabilizing agent in aqueous medium. The proposed methods were based on the complexation of AgNPs with urea. Using this concept, urea in the urine samples was successfully determined spectrophotometric methods. The results showed high percent recovery with ± RSD. The recoveries of urea in the three urine samples by spectrophotometric standard addition were 99.2% ± 5.37, 96.3% ± 4.49, 104.88% ± 4.99 and that of spectrophotometric 2nd order derivative method were 115.3% ± 5.2, 103.4% ± 2.6, 105.93% ± 0.76. The results show that these methods can open doors for a potential role of AgNPs in the clinical determination of urea in urine, blood, biological, non-biological fluids.

Application of EMA-qPCR as a complementary tool for the detection and monitoring of Legionella in different water systems.

PubMed

Qin, Tian; Tian, Zhengan; Ren, Hongyu; Hu, Guangchun; Zhou, Haijian; Lu, Jinxing; Luo, Chengwang; Liu, Zunyu; Shao, Zhujun

2012-05-01

Legionella are prevalent in human-made water systems and cause legionellosis in humans. Conventional culturing and polymerase chain reaction (PCR) techniques are not sufficiently accurate for the quantitative analysis of live Legionella bacteria in water samples because of the presence of viable but nonculturable cells and dead cells. Here, we report a rapid detection method for viable Legionella that combines ethidium monoazide (EMA) with quantitative real-time PCR (qPCR) and apply this method to detect Legionella in a large number of water samples from different sources. Results yielded that samples treated with 5 μg/ml EMA for 10 min and subsequently exposed to light irradiation for 5 min were optimal for detecting Legionella. EMA treatment before qPCR could block the signal from approximately 4 log(10) of dead cells. When investigating environmental water samples, the percent-positive rate obtained by EMA-qPCR was significantly higher than conventional PCR and culture methods, and slightly lower than qPCR. The bacterial count of Legionella determined by EMA-qPCR were mostly greater than those determined by culture assays and lower than those determined by qPCR. Acceptable correlations were found between the EMA-qPCR and qPCR results for cooling towers, piped water and hot spring water samples (r = 0.849, P < 0.001) and also found between the EMA-qPCR and culture results for hot spring water samples (r = 0.698, P < 0.001). The results indicate that EMA-qPCR could be used as a complementary tool for the detection and monitoring of Legionella in water systems, especially in hot spring water samples.

Amino Acid profile as a feasible tool for determination of the authenticity of fruit juices.

PubMed

Asadpoor, Mostafa; Ansarin, Masoud; Nemati, Mahboob

2014-12-01

Fruit juice is a nutrient rich food product with a direct connection to public health. The purpose of this research was to determine the amino acid profile of juices and provide a quick and accurate indicator for determining their authenticity. The method of analysis was HPLC with fluorescence detector and pre-column derivatization by orthophtaldialdehyde (OPA). Sixty-six samples of fruit juices were analyzed, and fourteen amino acids were identified and determined in the sampled fruit juices. The fruit samples used for this analysis were apples, oranges, cherry, pineapple, mango, apricot, pomegranate, peach and grapes. The results showed that 32% of samples tested in this study had a lower concentrate percentage as compared to that of their labels and/or other possible authenticity problems in the manufacturing process. The following samples showed probable adulteration: four cherry juice samples, two pomegranate juice samples, one mango, three grape, four peach, seven orange, two apple and one apricot juice samples. In general, determining the amount of amino acids and comparing sample amino acids profiles with the standard values seems to be an indicator for quality control. This method can provide the regulatory agencies with a tool, to help produce a healthier juice. The aim of this study is the analytical control of the fruit juice composition is becoming an important issue, and HPLC can provide an important and essential tool for more accurate research as well as for routine analysis.

New directional results and determination of absolute archaeointensity using both the classical Thellier and the multi-specimen procedures for two kilns excavated at Osterietta, Italy

NASA Astrophysics Data System (ADS)

Tema, Evdokia; Camps, Pierre; Ferrara, Enzo

2014-05-01

A detailed rock-magnetic and archaeomagnetic study has been carried out on two rescue excavation kilns discovered during the works to expand a highway at the location of Osterietta, in Northen Italy. Systematic archaeomagnetic sampling was carried out collecting 15 samples from the first kiln (OSA) and 8 samples from the second kiln (OSB), all of them oriented in situ with a magnetic compass and an inclinometer. Magnetic mineralogy measurements have been carried out in order to determine the main magnetic carrier of the samples and to check their thermal stability. Standard thermal demagnetization procedures have been used to determine the archaeomagnetic direction registered by the bricks during their last firing. Demagnetization results show a very stable characteristic remanent magnetization (ChRM). We averaged the directions for each kiln separately and calculated the statistical parameters assuming a Fisherian distribution. The archaeointensity of both kilns has also been recovered with both the classical Thellier-Thellier method and the multi-specimen procedure (MSP-DSC). During the Thellier experiments, regular partial thermoremanent magnetization checks have been performed and the effect of the anisotropy of the thermoremanent magnetization (TRM) and cooling rate upon TRM intensity acquisition have been investigated in all samples. The multi-specimen procedure was performed with a very fast-heating oven developed at Montpellier (France). The intensity results obtained from both methods have been compared and the full geomagnetic field vector determined for each kiln has been used for archaeomagnetic dating. The obtained results show that the kilns were almost contemporaneous and their last use occurred in the 1750-1850 AD time interval.

Reexamining Sample Size Requirements for Multivariate, Abundance-Based Community Research: When Resources are Limited, the Research Does Not Have to Be.

PubMed

Forcino, Frank L; Leighton, Lindsey R; Twerdy, Pamela; Cahill, James F

2015-01-01

Community ecologists commonly perform multivariate techniques (e.g., ordination, cluster analysis) to assess patterns and gradients of taxonomic variation. A critical requirement for a meaningful statistical analysis is accurate information on the taxa found within an ecological sample. However, oversampling (too many individuals counted per sample) also comes at a cost, particularly for ecological systems in which identification and quantification is substantially more resource consuming than the field expedition itself. In such systems, an increasingly larger sample size will eventually result in diminishing returns in improving any pattern or gradient revealed by the data, but will also lead to continually increasing costs. Here, we examine 396 datasets: 44 previously published and 352 created datasets. Using meta-analytic and simulation-based approaches, the research within the present paper seeks (1) to determine minimal sample sizes required to produce robust multivariate statistical results when conducting abundance-based, community ecology research. Furthermore, we seek (2) to determine the dataset parameters (i.e., evenness, number of taxa, number of samples) that require larger sample sizes, regardless of resource availability. We found that in the 44 previously published and the 220 created datasets with randomly chosen abundances, a conservative estimate of a sample size of 58 produced the same multivariate results as all larger sample sizes. However, this minimal number varies as a function of evenness, where increased evenness resulted in increased minimal sample sizes. Sample sizes as small as 58 individuals are sufficient for a broad range of multivariate abundance-based research. In cases when resource availability is the limiting factor for conducting a project (e.g., small university, time to conduct the research project), statistically viable results can still be obtained with less of an investment.

Efficiently estimating salmon escapement uncertainty using systematically sampled data

USGS Publications Warehouse

Reynolds, Joel H.; Woody, Carol Ann; Gove, Nancy E.; Fair, Lowell F.

2007-01-01

Fish escapement is generally monitored using nonreplicated systematic sampling designs (e.g., via visual counts from towers or hydroacoustic counts). These sampling designs support a variety of methods for estimating the variance of the total escapement. Unfortunately, all the methods give biased results, with the magnitude of the bias being determined by the underlying process patterns. Fish escapement commonly exhibits positive autocorrelation and nonlinear patterns, such as diurnal and seasonal patterns. For these patterns, poor choice of variance estimator can needlessly increase the uncertainty managers have to deal with in sustaining fish populations. We illustrate the effect of sampling design and variance estimator choice on variance estimates of total escapement for anadromous salmonids from systematic samples of fish passage. Using simulated tower counts of sockeye salmon Oncorhynchus nerka escapement on the Kvichak River, Alaska, five variance estimators for nonreplicated systematic samples were compared to determine the least biased. Using the least biased variance estimator, four confidence interval estimators were compared for expected coverage and mean interval width. Finally, five systematic sampling designs were compared to determine the design giving the smallest average variance estimate for total annual escapement. For nonreplicated systematic samples of fish escapement, all variance estimators were positively biased. Compared to the other estimators, the least biased estimator reduced bias by, on average, from 12% to 98%. All confidence intervals gave effectively identical results. Replicated systematic sampling designs consistently provided the smallest average estimated variance among those compared.

Determination of rare-earth elements in Luna 16 regolith sample by chemical spectral method

NASA Technical Reports Server (NTRS)

Stroganova, N. S.; Ryabukhin, V. A.; Laktinova, N. V.; Ageyeva, L. V.; Galkina, I. P.; Gatinskaya, N. G.; Yermakov, A. N.; Karyakin, A. V.

1974-01-01

An analysis was made of regolith from layer A of the Luna 16 sample for rare earth elements, by a chemical spectral method. Chemical and ion exchange concentrations were used to determine the content of 12 elements and Y at the level 0.001 to 0.0001 percent with 10 to 15 percent reproducibility of the emission determination. Results within the limits of reproducibility agree with data obtained by mass spectra, activation, and X-ray fluorescent methods.

Plagioclase mineralogy of olivine alkaline basalt

NASA Technical Reports Server (NTRS)

Hoffer, J. M.

1973-01-01

A geological and mineralogical study of the Potrillo volcanics is reported. The investigation consisted first of field mapping to establish and identify the different rock types and volcanic features in order to determine the geological history. Next, samples were collected and analyzed petrographically to determine suitable rocks from the various stratigraphic units for study of plagioclase. Samples selected for further study were crushed and the plagioclase extracted for the determination of composition and structural state. These results were then related to the petrology and crystallization of the basalt.

Interlaboratory comparison for the determination of the soluble fraction of metals in welding fume samples.

PubMed

Berlinger, Balazs; Harper, Martin

2018-02-01

There is interest in the bioaccessible metal components of aerosols, but this has been minimally studied because standardized sampling and analytical methods have not yet been developed. An interlaboratory study (ILS) has been carried out to evaluate a method for determining the water-soluble component of realistic welding fume (WF) air samples. Replicate samples were generated in the laboratory and distributed to participating laboratories to be analyzed according to a standardized procedure. Within-laboratory precision of replicate sample analysis (repeatability) was very good. Reproducibility between laboratories was not as good, but within limits of acceptability for the analysis of typical aerosol samples. These results can be used to support the development of a standardized test method.

Determination of oestrous cycle of the rats by direct examination: how reliable?

PubMed

Yener, T; Turkkani Tunc, A; Aslan, H; Aytan, H; Cantug Caliskan, A

2007-02-01

For determination of the oestrous cycle in rats classical Papanicolaou technique has long been used successfully. Instead of using many stains in Papanicolaou, staining the vaginal secretions with only methylene blue has also been defined. Recently a new technique in which vaginal samples are directly examined under light microscope has been introduced. The aim of this study was to assess the reliability of this new technique by comparing it with the classical staining techniques. From 20 Wistar rats 60 vaginal samples were collected with a micropipette, three from each. Briefly, the vagina was flushed two to three times then the fluid was placed onto a glass slide. The fluid was equally distributed onto three glass slides. The glass slides were coded. Two samples were stained with Papanicolaou and methylene blue while the other one was examined directly. Determination of the phases of the oestrous cycle was made by the same histologist who was blinded to the groups and coding system. After determination of the oestrous phase in all samples, the results were compared and it was found that the results were matching. In conclusion, the same results can be obtained with the direct examination technique and this technique is reliable, so there is no need to use relatively time-consuming, less practical and more expensive techniques such as Papanicolaou or methylene blue.

Comparison study of two procedures for the determination of emamectin benzoate in medicated fish feed.

PubMed

Farer, Leslie J; Hayes, John M

2005-01-01

A new method has been developed for the determination of emamectin benzoate in fish feed. The method uses a wet extraction, cleanup by solid-phase extraction, and quantitation and separation by liquid chromatography (LC). In this paper, we compare the performance of this method with that of a previously reported LC assay for the determination of emamectin benzoate in fish feed. Although similar to the previous method, the new procedure uses a different sample pretreatment, wet extraction, and quantitation method. The performance of the new method was compared with that of the previously reported method by analyses of 22 medicated feed samples from various commercial sources. A comparison of the results presented here reveals slightly lower assay values obtained with the new method. Although a paired sample t-test indicates the difference in results is significant, this difference is within the method precision of either procedure.

Determination of the MRI contrast agent Gd-DTPA by SEC-ICP-MS.

PubMed

Loreti, Valeria; Bettmer, Jörg

2004-08-01

The simultaneous determination of Gd(3+) and Gd-DTPA (DTPA: diethylenetriamino-pentaacetic acid), often used as contrast agent, is described. The proposed approach combines size-exclusion chromatography (SEC) and inductively coupled plasma-mass spectrometry (ICP-MS) for element-selective detection in order to determine also high-molecular Gd-complexes if present. This method was applied to the analysis of urine samples of a patient to whom Gd-DTPA was intravenously administered. The results showed that no conversion or adsorption of Gd-DTPA could be observed in any sample, even free Gd(3+) could not be detected. Urine excretion behaviour was monitored and it was proved that Gd-DTPA was almost completely (>99%) excreted by urination within one day. Traces of Gd-DTPA could be measured in hair samples, but extraction with tetramethylammonium hydroxide (TMAH) resulted in degradation of Gd-DTPA.

An investigation on mechanical properties of steel fibre reinforced for underwater welded joint

NASA Astrophysics Data System (ADS)

Navin, K.; Zakaria, M. S.; Zairi, S.

2017-09-01

Underwater pipelines are always exposed to water and have a high tendency to have corrosion especially on the welded joint. This research is about using fiber glass as steel fiber to coat the welded joint to determine the effectiveness in corrosion prevention of the welded joint. Number of coating is varied to determine the better number coating to coat the pipeline. Few samples were left without immersion in salt water and few samples are immersed into salt water with same salinity as sea water. The material sample is prepared in dog bone shape to enable to be used in Universal Tensile Machine (UTM). The material prepared is left immersed for recommended time and tested in Universal Tensile Machine. Upon analyzing the result, the result is used to determine the breakage point whether broken on the welded joint or different place and also the suitable number of coating to be used.

Exploring the Utilization of Low-Pressure, Piston-Cylinder Experiments to Determine the Bulk Compositions of Finite, Precious Materials

NASA Technical Reports Server (NTRS)

Vander Kaaden, K. E.; McCubbin, F. M.; Harrington, A. D.

2017-01-01

Determining the bulk composition of precious materials with a finite mass (e.g., meteorite samples) is extremely important in the fields of Earth and Planetary Science. From meteorite studies we are able to place constraints on large scale planetary processes like global differentiation and subsequent volcanism, as well as smaller scale processes like crystallization in a magma chamber or sedimentary compaction at the surface. However, with meteorite samples in particular, far too often we are limited by how precious the sample is as well as its limited mass. In this study, we have utilized aliquots of samples previously studied for toxicological hazards, including both the fresh samples (lunar mare basalt NWA 4734, lunar regolith breccia NWA 7611, martian basalt Tissint, martian regolith breccia NWA 7034, a vestian basalt Berthoud, a vestian regolith breccia NWA 2060, and a terrestrial mid-ocean ridge basalt (MORB)), and those that underwent iron leaching (Tissint, NWA 7034, NWA 4734, MORB). With these small masses of material, we performed low pressure (approx. 0.75 GPa), high temperature (greater than 1600 degrees Celsius) melting experiments. Each sample was analyzed using a JEOL 8530F electron microprobe to determine the bulk composition of the materials that were previously examined. When available, the results of our microprobe data were compared with bulk rock compositions in the literature. The results of this study show that with this technique, only approx. 50 mg of sample is required to accurately determine the bulk composition of the materials of interest.

Solid-state characterization and impurities determination of fluconazol generic products marketed in Morocco

PubMed Central

Bourichi, Houda; Brik, Youness; Hubert, Philipe; Cherrah, Yahia; Bouklouze, Abdelaziz

2012-01-01

In this paper, we report the results of quality control based in physicochemical characterization and impurities determination of three samples of fluconazole drug substances marketed in Morocco. These samples were supplied by different pharmaceuticals companies. The sample A, as the discovered product, was supplied by Pfizer, while samples B and C (generics), were manufactured by two different Indian industries. Solid-state characterization of the three samples was realized with different physicochemical methods as: X-ray powder diffraction, Fourier-transformation infrared spectroscopy, differential scanning calorimetry. High performance liquid chromatography was used to quantify the impurities in the different samples. The results from the physicochemical methods cited above, showed difference in polymorph structure of the three drug substances. Sample A consisted in pure polymorph III, sample B consisted in pure polymorph II, sample C consisted in a mixture of fluconazole Form III, form II and the monohydrate. This result was confirmed by differential scanning calorimetry. Also it was demonstrated that solvents used during the re-crystallization step were among the origins of these differences in the structure form. On the other hand, the result of the stability study under humidity and temperature showed that fluconazole polymorphic transformation could be owed to the no compliance with the conditions of storage. The HPLC analysis of these compounds showed the presence of specific impurities for each polymorphic form, and a possible relationship could be exist between impurities and crystalline form of fluconazole. PMID:29403776

Extractive procedure for uranium determination in water samples by liquid scintillation counting.

PubMed

Gomez Escobar, V; Vera Tomé, F; Lozano, J C; Martín Sánchez, A

1998-07-01

An extractive procedure for uranium determination using liquid scintillation counting with the URAEX cocktail is described. Interference from radon and a strong influence of nitrate ion were detected in this procedure. Interference from radium, thorium and polonium emissions were very low when optimal operating conditions were reached. Quenching effects were considered and the minimum detectable activity was evaluated for different sample volumes. Isotopic analysis of samples can be performed using the proposed method. Comparisons with the results obtained with the general procedure used in alpha spectrometry with passivated implanted planar silicon detectors showed good agreement. The proposed procedure is thus suitable for uranium determination in water samples and can be considered as an alternative to the laborious conventional chemical preparations needed for alpha spectrometry methods using semiconductor detectors.

Heterogenic Solid Biofuel Sampling Methodology and Uncertainty Associated with Prompt Analysis

PubMed Central

Pazó, Jose A.; Granada, Enrique; Saavedra, Ángeles; Patiño, David; Collazo, Joaquín

2010-01-01

Accurate determination of the properties of biomass is of particular interest in studies on biomass combustion or cofiring. The aim of this paper is to develop a methodology for prompt analysis of heterogeneous solid fuels with an acceptable degree of accuracy. Special care must be taken with the sampling procedure to achieve an acceptable degree of error and low statistical uncertainty. A sampling and error determination methodology for prompt analysis is presented and validated. Two approaches for the propagation of errors are also given and some comparisons are made in order to determine which may be better in this context. Results show in general low, acceptable levels of uncertainty, demonstrating that the samples obtained in the process are representative of the overall fuel composition. PMID:20559506

Prediction of Asbestos Exposure Resulting From Asbestos Aerosolization Determined Using the Releasable Asbestos Field Sampler (RAFS)

EPA Science Inventory

Activity-based sampling (ABS) used to evaluate breathing zone exposure to a contaminant present in soil resulting from various activities, involves breathing zone sampling for contaminants while that activity is performed. A probabilistic model based upon aerosol physics and flui...

Determination of fossil carbon content in Swedish waste fuel by four different methods.

PubMed

Jones, Frida C; Blomqvist, Evalena W; Bisaillon, Mattias; Lindberg, Daniel K; Hupa, Mikko

2013-10-01

This study aimed to determine the content of fossil carbon in waste combusted in Sweden by using four different methods at seven geographically spread combustion plants. In total, the measurement campaign included 42 solid samples, 21 flue gas samples, 3 sorting analyses and 2 investigations using the balance method. The fossil carbon content in the solid samples and in the flue gas samples was determined using (14)C-analysis. From the analyses it was concluded that about a third of the carbon in mixed Swedish waste (municipal solid waste and industrial waste collected at Swedish industry sites) is fossil. The two other methods (the balance method and calculations from sorting analyses), based on assumptions and calculations, gave similar results in the plants in which they were used. Furthermore, the results indicate that the difference between samples containing as much as 80% industrial waste and samples consisting of solely municipal solid waste was not as large as expected. Besides investigating the fossil content of the waste, the project was also established to investigate the usability of various methods. However, it is difficult to directly compare the different methods used in this project because besides the estimation of emitted fossil carbon the methods provide other information, which is valuable to the plant owner. Therefore, the choice of method can also be controlled by factors other than direct determination of the fossil fuel emissions when considering implementation in the combustion plants.

Four reference soil and rock samples for measuring element availability in the Western Energy Regions

USGS Publications Warehouse

Crock, J.G.; Severson, R.C.

1980-01-01

Attaining acceptable precision in extractable element determinations is more difficult than in total element determinations. In total element determinations, dissolution of the sample is qualitatively checked by the clarity of the solution and the absence of residues. These criteria cannot be used for extracts. Possibilities for error are introduced in virtually every step in soil extractions. Therefore, the use of reference materials whose homogeneity and element content are reasonably well known is essential for determination of extractable elements. In this report, estimates of homogeneity and element content are presented for four reference samples. Bulk samples of about 100 kilograms of each sample were ground to pass an 80-mesh sieve. The samples were homogenized and split using a Jones-type splitter. Fourteen splits of each reference sample were analyzed for total content of Ca, Co, Cu, Fe, K, Mg, Mn, Na, and Zn; DTPA-extractable Cd, Co, Cu, Fe, Mn, Ni, Pb, and Zn; exchangeable Ca, Mg, K, and Na; cation exchange capacity water-saturation-extractable Ca, Mg, K, Na, C1, and SO4; soil pH; and hot-water-extractable boron. Error measured between splits was small, indicating that the samples were homogenized adequately and that the laboratory procedure provided reproducible results.

Spectrophotometric determination of gold(III) in forensic and pharmaceutical samples and results complemented with ICP AES and EDXRF analysis

NASA Astrophysics Data System (ADS)

Nagaraja, Vani; Kumar, M. Kiran; Giddappa, Nagendrappa

2017-02-01

Spectrophotometric method with three systems were developed here for the determination of gold(III) using o-dianisidine, aniline sulphate and catechol. Gold(III),in the system 1 it oxidizes o-dianisidine, in the system 2 it oxidizes catechol followed by its coupling with o-dianisidine, in the system 3 it oxidizes catechol followed by its coupling with aniline sulphate forming dye products with respective λmax 446 nm, 540 nm, and 505 nm. All the three systems were optimized and analytical parameters were calculated. The molar absorptivity values were 9.27 × 104, 1.97 × 104 and 1.62 × 104 respectively for the systems 1, 2 and 3 with the corresponding Sandell sensitivity values (μg cm- 2), 0.0021, 0.0096 and 0.011. The optimized systems were used for the determination of gold present in some forensic jewellery and pharmaceutical samples and the results obtained were compared with the results of all samples determined by Inductively Coupled Plasma - Atomic Emission Spectrometric method and a few of them were also complemented by Energy Dispersive X-Ray Fluorescent spectral analysis.

Spectrophotometric determination of gold(III) in forensic and pharmaceutical samples and results complemented with ICP AES and EDXRF analysis.

PubMed

Nagaraja, Vani; Kumar, M Kiran; Giddappa, Nagendrappa

2017-02-15

Spectrophotometric method with three systems were developed here for the determination of gold(III) using o-dianisidine, aniline sulphate and catechol. Gold(III),in the system 1 it oxidizes o-dianisidine, in the system 2 it oxidizes catechol followed by its coupling with o-dianisidine, in the system 3 it oxidizes catechol followed by its coupling with aniline sulphate forming dye products with respective λ max 446nm, 540nm, and 505nm. All the three systems were optimized and analytical parameters were calculated. The molar absorptivity values were 9.27×10 4 , 1.97×10 4 and 1.62×10 4 respectively for the systems 1, 2 and 3 with the corresponding Sandell sensitivity values (μgcm -2 ), 0.0021, 0.0096 and 0.011. The optimized systems were used for the determination of gold present in some forensic jewellery and pharmaceutical samples and the results obtained were compared with the results of all samples determined by Inductively Coupled Plasma - Atomic Emission Spectrometric method and a few of them were also complemented by Energy Dispersive X-Ray Fluorescent spectral analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

Results of interlaboratory comparison of fission-track age standards: Fission-track workshop-1984

USGS Publications Warehouse

Miller, D.S.; Duddy, I.R.; Green, P.F.; Hurford, A.J.; Naeser, C.W.

1985-01-01

Five samples were made available as standards for the 1984 Fission Track Workshop held in the summer of 1984 (Rensselaer Polytechnic Institute, Troy, New York). Two zircons, two apatites and a sphene were distributed prior to the meeting to 40 different laboratories. To date, 24 different analysts have reported results. The isotopic ages of the standards ranged from 16.8 to 98.7 Myr. Only the statement that the age of each sample was less than 200 Myr was provided with the set of standards distributed. Consequently, each laboratory was required to use their laboratory's accepted treatment (irradiation level, etching conditions, counting conditions, etc.) for these samples. The results show that some workers have serious problems in achieving accurate age determinations. This emphasizes the need to calibrate experimental techniques and counting procedures against age standards before unknown ages are determined. Any fission-track age determination published or submitted for publication can only be considered reliable if it is supported by evidence of consistent determinations on age standards. Only this can provide the scientific community with the background to build up confidence concerning the validity of the fission-track method. ?? 1985.

Investigation of chemical modifiers for the direct determination of arsenic in fish oil using high-resolution continuum source graphite furnace atomic absorption spectrometry.

PubMed

Pereira, Éderson R; de Almeida, Tarcísio S; Borges, Daniel L G; Carasek, Eduardo; Welz, Bernhard; Feldmann, Jörg; Campo Menoyo, Javier Del

2016-04-01

High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) has been applied for the development of a method for the determination of total As in fish oil samples using direct analysis. The method does not use any sample pretreatment, besides dilution with 1-propanole, in order to decrease the oil viscosity. The stability and sensitivity of As were evaluated using ruthenium and iridium as permanent chemical modifiers and palladium added in solution over the sample. The best results were obtained with ruthenium as the permanent modifier and palladium in solution added to samples and standard solutions. Under these conditions, aqueous standard solutions could be used for calibration for the fish oil samples diluted with 1-propanole. The pyrolysis and atomization temperatures were 1400 °C and 2300 °C, respectively, and the limit of detection and characteristic mass were 30 pg and 43 pg, respectively. Accuracy and precision of the method have been evaluated using microwave-assisted acid digestion of the samples with subsequent determination by HR-CS GF AAS and ICP-MS; the results were in agreement (95% confidence level) with those of the proposed method. Copyright © 2015 Elsevier B.V. All rights reserved.

Effects of positive results for Mycobacterium avium subsp paratuberculosis as determined by microbial culture of feces or antibody ELISA on results of caudal fold tuberculin test and interferon-gamma assay for tuberculosis in cattle.

PubMed

Dunn, John R; Kaneene, John B; Grooms, Daniel L; Bolin, Steven R; Bolin, Carole A; Bruning-Fann, Colleen S

2005-02-01

To determine whether cattle testing positive for Mycobacterium avium subsp paratuberculosis as determined by microbial culture of feces or antibody ELISA were more likely to have false-positive responses on the caudal fold tuberculin (CFT) test or interferon-gamma (IFN-gamma) assay for Mycobacterium bovis than cattle testing negative for M paratuberculosis. 1043 cattle from 10 herds in Michigan. Feces and blood samples for plasma were collected from cattle > or =24 months old on the day the CFT test was read. Fecal samples were submitted for microbial culture for M paratuberculosis. Plasma samples were tested for antibody against M paratuberculosis, and IFN-gamma after stimulation with purified protein derivative tuberculin from M bovis or M avium. Of 1043 cattle, 180 (17.3%) had positive CFT test results (suspects) and 8 (0.8%) had positive IFN-gamma assay results after stimulation with purified protein derivative tuberculin from M bovis. Forty-five (4.3%) and 115 (11.0%) cattle tested positive for M paratuberculosis as determined by microbial culture of feces and antibody ELISA, respectively. Cattle with positive responses for M paratuberculosis appeared to have an increased likelihood of false-positive results on the CFT test, although this association was not significant. No significant association was detected among cattle testing positive for M paratuberculosis as determined by microbial culture of feces and antibody ELISA and positive CFT test and IFN-gamma assay results for M bovis.

Assessment of the contamination problems resulting from the use of stainless steel needles in liver biopsies by total reflection X-ray fluorescence and inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Varga, Imre

2006-11-01

Percutaneous human liver biopsies taken from living patients could not be repeated; therefore considerable contamination was indirectly disproved. In the present study, the possible contamination of biopsy samples during sample collection was determined using a porcine liver model. Portions of porcine liver were cut by a quartz blade and treated the same as the steel needle biopsy samples. Concentrations determined in samples taken by a quartz device represented the non-contaminated values and were used to determine reproducibility of measurement and intra-individual variations. Additionally, multiple samples taken from a human liver of a patient suffering steatosis during autopsy were used to determine intra-individual variation of element concentrations. Concentration data of non-contaminated samples were compared to data of steel needle biopsy samples. To investigate the possible release of elements from the steel needles the samples were allowed to contact with the needle for different time in a refrigerator at 4 °C. Total reflection X-ray fluorescence spectrometry (TXRF) and inductively coupled plasma-mass spectrometry (ICP-MS) were applied for simultaneous determination of Cr, Mn, Fe, Co, Ni, Cu, Zn, Rb, Mo and Pb because of the very low sample demand of the two selected techniques. Although the steel needles in the present study could not be substituted by polypropylene or Teflon utensils, it was demonstrated that the application of needle biopsy sampling in the reported analysis does not involve measurable contamination if contact time is kept to several minutes as usual in the clinical practice.

Exploration of attenuated total reflectance mid-infrared spectroscopy and multivariate calibration to measure immunoglobulin G in human sera.

PubMed

Hou, Siyuan; Riley, Christopher B; Mitchell, Cynthia A; Shaw, R Anthony; Bryanton, Janet; Bigsby, Kathryn; McClure, J Trenton

2015-09-01

Immunoglobulin G (IgG) is crucial for the protection of the host from invasive pathogens. Due to its importance for human health, tools that enable the monitoring of IgG levels are highly desired. Consequently there is a need for methods to determine the IgG concentration that are simple, rapid, and inexpensive. This work explored the potential of attenuated total reflectance (ATR) infrared spectroscopy as a method to determine IgG concentrations in human serum samples. Venous blood samples were collected from adults and children, and from the umbilical cord of newborns. The serum was harvested and tested using ATR infrared spectroscopy. Partial least squares (PLS) regression provided the basis to develop the new analytical methods. Three PLS calibrations were determined: one for the combined set of the venous and umbilical cord serum samples, the second for only the umbilical cord samples, and the third for only the venous samples. The number of PLS factors was chosen by critical evaluation of Monte Carlo-based cross validation results. The predictive performance for each PLS calibration was evaluated using the Pearson correlation coefficient, scatter plot and Bland-Altman plot, and percent deviations for independent prediction sets. The repeatability was evaluated by standard deviation and relative standard deviation. The results showed that ATR infrared spectroscopy is potentially a simple, quick, and inexpensive method to measure IgG concentrations in human serum samples. The results also showed that it is possible to build a united calibration curve for the umbilical cord and the venous samples. Copyright © 2015 Elsevier B.V. All rights reserved.

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

Streets, W.E.

As the need for rapid and more accurate determinations of gamma-emitting radionuclides in environmental and mixed waste samples grows, there is continued interest in the development of theoretical tools to eliminate the need for some laboratory analyses and to enhance the quality of information from necessary analyses. In gamma spectrometry the use of theoretical self-absorption coefficients (SACs) can eliminate the need to determine the SAC empirically by counting a known source through each sample. This empirical approach requires extra counting time and introduces another source of counting error, which must be included in the calculation of results. The empirical determinationmore » of SACs is routinely used when the nuclides of interest are specified; theoretical determination of the SAC can enhance the information for the analysis of true unknowns, where there may be no prior knowledge about radionuclides present in a sample. Determination of an exact SAC does require knowledge about the total composition of a sample. In support of the Department of Energy`s (DOE) Environmental Survey Program, the Analytical Chemistry Laboratory (ACL) at Argonne National Laboratory developed theoretical self-absorption models to estimate SACs for the determination of non-specified radionuclides in samples of unknown, widely-varying, compositions. Subsequently, another SAC model, in a different counting geometry and for specified nuclides, was developed for another application. These two models are now used routinely for the determination of gamma-emitting radionuclides in a wide variety of environmental and mixed waste samples.« less

Uptake of explosives from contaminated soil by vegetation at the Joliet Army Ammunition Plant

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

Schneider, J.F.; Tomczyk, N.A.; Zellmer, S.D.

1994-06-01

This study examines the uptake of explosives by vegetation growing on soils contaminated by 2,4,6-trinitrotoluene (TNT) in Group 61 at the Joliet Army Ammunition Plant (JAAP). Plant materials and soil from the root zone were sampled and analyzed to determine TNT uptake under natural field conditions. Standard USATHAMA methods were used to determine concentrations of explosives, their derivatives, and metabolites in the soil samples. No- explosives were detected in the aboveground portion of any plant sample. However, results indicate that TNT, 2-aminodinitrotoluene (2-ADNT), and/or 4-ADNT were present in some root samples. The presence of 2-ADNT and 4-ADNT increases the likelihoodmore » that explosives were taken up by plant roots, as opposed to their presence resulting from external soil contamination.« less

Influence of various water quality sampling strategies on load estimates for small streams

USGS Publications Warehouse

Robertson, Dale M.; Roerish, Eric D.

1999-01-01

Extensive streamflow and water quality data from eight small streams were systematically subsampled to represent various water‐quality sampling strategies. The subsampled data were then used to determine the accuracy and precision of annual load estimates generated by means of a regression approach (typically used for big rivers) and to determine the most effective sampling strategy for small streams. Estimation of annual loads by regression was imprecise regardless of the sampling strategy used; for the most effective strategy, median absolute errors were ∼30% based on the load estimated with an integration method and all available data, if a regression approach is used with daily average streamflow. The most effective sampling strategy depends on the length of the study. For 1‐year studies, fixed‐period monthly sampling supplemented by storm chasing was the most effective strategy. For studies of 2 or more years, fixed‐period semimonthly sampling resulted in not only the least biased but also the most precise loads. Additional high‐flow samples, typically collected to help define the relation between high streamflow and high loads, result in imprecise, overestimated annual loads if these samples are consistently collected early in high‐flow events.

Determinations of rare earth element abundance and U-Pb age of zircons using multispot laser ablation-inductively coupled plasma mass spectrometry.

PubMed

Yokoyama, Takaomi D; Suzuki, Toshihiro; Kon, Yoshiaki; Hirata, Takafumi

2011-12-01

We have developed a new calibration technique for multielement determination and U-Pb dating of zircon samples using laser ablation-inductively coupled plasma mass spectrometry (ICPMS) coupled with galvanometric optics. With the galvanometric optics, laser ablation of two or more sample materials could be achieved in very short time intervals (~10 ms). The resulting sample aerosols released from different ablation pits or different solid samples were mixed and homogenized within the sample cell and then transported into the ICP ion source. Multiple spot laser ablation enables spiking of analytes or internal standard elements directly into the solid samples, and therefore the standard addition calibration method can be applied for the determination of trace elements in solid samples. In this study, we have measured the rare earth element (REE) abundances of two zircon samples (Nancy 91500 and Prešovice) based on the standard addition technique, using a direct spiking of analytes through a multispot laser ablation of the glass standard material (NIST SRM612). The resulting REE abundance data show good agreement with previously reported values within analytical uncertainties achieved in this study (10% for most elements). Our experiments demonstrated that nonspectroscopic interferences on 14 REEs could be significantly reduced by the standard addition technique employed here. Another advantage of galvanometric devices is the accumulation of sample aerosol released from multiple spots. In this study we have measured the U-Pb age of a zircon sample (LMR) using an accumulation of sample aerosols released from 10 separate ablation pits of low diameters (~8 μm). The resulting (238)U-(206)Pb age data for the LMR zircons was 369 ± 64 Ma, which is in good agreement with previously reported age data (367.6 ± 1.5 Ma). (1) The data obtained here clearly demonstrate that the multiple spot laser ablation-ICPMS technique can become a powerful approach for elemental and isotopic ratio measurements in solid materials.

A comparison of Thellier-type and multispecimen paleointensity determinations on Pleistocene and historical lava flows from Lanzarote (Canary Islands, Spain)

NASA Astrophysics Data System (ADS)

Calvo-Rathert, Manuel; Morales-Contreras, Juan; Carrancho, Ángel; Goguitchaichvili, Avto

2016-09-01

Sixteen Miocene, Pleistocene, and historic lava flows have been sampled in Lanzarote (Canary Islands) for paleointensity analysis with both the Coe and multispecimen methods. Besides obtaining new data, the main goal of the study was the comparison of paleointensity results determined with two different techniques. Characteristic Remanent Magnetization (ChRM) directions were obtained in 15 flows, and 12 were chosen for paleointensity determination. In Thellier-type experiments, a selection of reliable paleointensity determinations (43 of 78 studied samples) was performed using sets of criteria of different stringency, trying to relate the quality of results to the strictness of the chosen criteria. Uncorrected and fraction and domain-state corrected multispecimen paleointensity results were obtained in all flows. Results with the Coe method on historical flows either agree with the expected values or show moderately lower ones, but multispecimen determinations display a large deviation from the expected result in one case. No relation can be detected between correct or anomalous results and paleointensity determination quality or rock-magnetic properties. However, results on historical flows suggest that agreement between both methods could be a good indicator of correct determinations. Comparison of results obtained with both methods on seven Pleistocene flows yields an excellent agreement in four and disagreements in three cases. Pleistocene determinations were only accepted if either results from both methods agreed or a result was based on a sufficiently large number (n > 4) of individual Thellier-type determinations. In most Pleistocene flows, a VADM around 5 × 1022 Am2 was observed, although two flows displayed higher values around 9 × 1022 Am2.

[Evaluation of the diagnostic performance of Xpert MTB/RIF test for the detection of Mycobacterium tuberculosis and rifampin resistance in clinical samples].

PubMed

Gürsoy, Nafia Canan; Yakupoğulları, Yusuf; Tekerekoğlu, Mehmet Sait; Otlu, Barış

2016-04-01

Rapid and accurate detection of active tuberculosis (TB) cases is one of the most important goal of tuberculosis control programme. For this purpose, new methods are being developed to isolate, serotype and determine the drug resistance of the agent. Xpert MTB/RIF test (CepheidGeneXpert® System, USA) that has been recently developed, is a real-time polymerase chain reaction-based method which detects Mycobacterium tuberculosis complex and resistance of the strain to rifampicin (RIF) from the clinical sample directly within a couple of hours. However, there are not sufficient data about the performance of that test for extrapulmonary samples and pulmonary samples other than sputum. The aims of this study were to investigate the sensitivity, specificity, positive and negative predictive values of Xpert MTB/RIF test in detection of M. tuberculosis and the performance in the determination of rifampicin resistance of the isolates from pulmonary and extrapulmonary clinical samples. A total of 2160 clinical samples, in which 1141 (52.8%) were pulmonary and 1019 (47.2%) were extrapulmonary samples, sent to our laboratory between July 2013 to December 2014, were included in the study. Sixty seven of the evaluated samples (3.1%) were positive with microscopy (acid-fast stain; AFS), 116 samples (5.1%) were positive with culture and 98 samples (4.5%) were positive with Xpert MTB/RIF test. When the culture was considered as the reference method, the sensitivity and specificity of Xpert MTB/RIF test were determined as 73.3% and 99.3%, respectively for all samples; 77.5% and 99.5%, respectively for pulmonary samples and 63.9% and 99.2%, respectively for extrapulmonary samples. Among AFS positive samples, the sensitivity was 100% and specificity was 66.7%; whereas among AFS negative samples those values were 40.4% and 99.4%, respectively. Among all the samples involved in the study, RIF resistance was determined only in three samples with Xpert MTB/ RIF test and that was also proved phenotypically (100% concordance). According to mycobacterial culture results, positive and negative predictive values of Xpert MTB/RIF test were determined as 86.7% and 98.5%, respectively for all samples. Those were determined as 92.5% and 98.3%, respectively for extrapulmonary samples and were determined as 74.2 and 98.7%, respectively for pulmonary samples. According to the results obtained in our study, sensitivity of Xpert MTB/RIF test for extrapulmonary samples was found to be at moderate level; sensitivity of the test was found to be decreased especially in AFS negative samples with less bacilli load. Nonetheless, specificity of Xpert MTB/RIF test to the agent in all samples was found to be extremely high. In our study, although RIF-resistant strains were detected in few of the samples, Xpert MTB/ RIF test could differentiate all resistant and sensitive strains. Additionally, detection of M. tuberculosis and RIF resistance in our laboratory takes approximately 20.96 days with culture, this period decreases to a couple of hours with Xpert MTB/RIF test. Because of the advantages such as being practical, rapid and requiring minimal safety measures, it was concluded that Xpert MTB/RIF test may contribute to rapid diagnosis of TB also in extrapulmonary samples, with the confirmation of culture method.

Sample size determination for mediation analysis of longitudinal data.

PubMed

Pan, Haitao; Liu, Suyu; Miao, Danmin; Yuan, Ying

2018-03-27

Sample size planning for longitudinal data is crucial when designing mediation studies because sufficient statistical power is not only required in grant applications and peer-reviewed publications, but is essential to reliable research results. However, sample size determination is not straightforward for mediation analysis of longitudinal design. To facilitate planning the sample size for longitudinal mediation studies with a multilevel mediation model, this article provides the sample size required to achieve 80% power by simulations under various sizes of the mediation effect, within-subject correlations and numbers of repeated measures. The sample size calculation is based on three commonly used mediation tests: Sobel's method, distribution of product method and the bootstrap method. Among the three methods of testing the mediation effects, Sobel's method required the largest sample size to achieve 80% power. Bootstrapping and the distribution of the product method performed similarly and were more powerful than Sobel's method, as reflected by the relatively smaller sample sizes. For all three methods, the sample size required to achieve 80% power depended on the value of the ICC (i.e., within-subject correlation). A larger value of ICC typically required a larger sample size to achieve 80% power. Simulation results also illustrated the advantage of the longitudinal study design. The sample size tables for most encountered scenarios in practice have also been published for convenient use. Extensive simulations study showed that the distribution of the product method and bootstrapping method have superior performance to the Sobel's method, but the product method was recommended to use in practice in terms of less computation time load compared to the bootstrapping method. A R package has been developed for the product method of sample size determination in mediation longitudinal study design.

Determination of fat and total protein content in milk using conventional digital imaging.

PubMed

Kucheryavskiy, Sergey; Melenteva, Anastasiia; Bogomolov, Andrey

2014-04-01

The applicability of conventional digital imaging to quantitative determination of fat and total protein in cow's milk, based on the phenomenon of light scatter, has been proved. A new algorithm for extracting features from digital images of milk samples has been developed. The algorithm takes into account spatial distribution of light, diffusely transmitted through a sample. The proposed method has been tested on two sample sets prepared from industrial raw milk standards, with variable fat and protein content. Partial Least-Squares (PLS) regression on the features calculated from images of monochromatically illuminated milk samples resulted in models with high prediction performance when analysed the sets separately (best models with cross-validated R(2)=0.974 for protein and R(2)=0.973 for fat content). However when analysed the sets jointly with the obtained results were significantly worse (best models with cross-validated R(2)=0.890 for fat content and R(2)=0.720 for protein content). The results have been compared with previously published Vis/SW-NIR spectroscopic study of similar samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Determination of trichloroanisole and trichlorophenol in wineries' ambient air by passive sampling and thermal desorption-gas chromatography coupled to tandem mass spectrometry.

PubMed

Camino-Sánchez, F J; Bermúdez-Peinado, R; Zafra-Gómez, A; Ruíz-García, J; Vílchez-Quero, J L

2015-02-06

The present paper describes the calibration of selected passive samplers used in the quantitation of trichlorophenol and trichloroanisole in wineries' ambient air, by calculating the corresponding sampling rates. The method is based on passive sampling with sorbent tubes and involves thermal desorption-gas chromatography-triple quadrupole mass spectrometry analysis. Three commercially available sorbents were tested using sampling cartridges with a radial design instead of axial ones. The best results were found for Tenax TA™. Sampling rates (R-values) for the selected sorbents were determined. Passive sampling was also used for accurately determining the amount of compounds present in the air. Adequate correlation coefficients between the mass of the target analytes and exposure time were obtained. The proposed validated method is a useful tool for the early detection of trichloroanisole and its precursor trichlorophenol in wineries' ambient air while avoiding contamination of wine or winery facilities. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination colchicine content in aquadest-extracted Gloriosa superba seed from Sukoharjo and Gunung Kidul

NASA Astrophysics Data System (ADS)

Rahmawati, S. I.; Susilowati, A.; Yunus, A.; Widyastuti, Y.

2018-03-01

Colchicine is a toxic alkaloid compound from the Colchicum autumnale plant. Colchicine can be used in agriculture as anti-mitosis in the procurement of plants with polyploid cells. Gloriosa superba is an herb contains colchicine as a mutagen (polyploid) potential in its parts, especially in the seeds. The aims of this research were to determine colchicine content from aquadest-extracted Gloriosa superba seed obtained from Sukoharjo and Gunung Kidul. Gloriosa superba seed samples were obtained naturally in January - April 2017. Samples were divided into immature seed samples from Mulur, Sukoharjo, Central Java and old seed samples from Krakal Beach, Gunung Kidul, Yogyakarta. Extraction seeds of Gloriosa superba using the maceration method with aquadest solvent (1: 1). Determination content of colchicine extract using TLC-Densitometry method. The results indicated that colchicine content of old seed Gloriosa superba samples 37,6 μg/μl (± 6,63) higher than colchicine content of immature seed Gloriosa superba samples 12,84 μg/μl (± 2,88)

Strontium-90 measurement after the Chernobyl accident in Romanian samples without chemical separation

NASA Astrophysics Data System (ADS)

Cosma, C.

2000-07-01

This paper presents a method for measuring 90Sr from soil and sediments without a preliminary chemical separation of strontium from samples. The measurements were done using a Geiger-Müller proportional radiation detector of VA-Z-520 type, an RFT-20026 monochannel analyser and aluminium plates of two thicknesses determined in this way to select the 1500-2281-keV energy range for the 90Y measurement and to avoid the 106Rh interference. The results obtained with this method were compared with those using chemical separation. This method was used to determine the strontium content in four samples, which were collected in Cluj-Napoca and three other Romanian towns (Transylvania region) after the Chernobyl disaster. The obtained values for these samples are in the 40-75-Bq/g range for 90Sr. The 90Sr/ 137Cs ratio is approximately 1:8, close to the ratio 1:10 determined in samples from Bucharest area and Japanese samples measured during 1988.

[Determination of lead in microemulsified rapeseed oil and bio-diesel oil by GFAAS].

PubMed

Li, Sheng-qing; He, Xiao-min; Du, Ping; Wang, Min; Chen, Hao; Wu, Mou-cheng

2008-10-01

Bio-diesel oil has attracted much attention as a substitutable energy sources for its renewable and eco-friendly property. However, problems of lead contamination in fuel are also emphasized increasingly at present. So it was of quite significance to determine the contents of lead in bio-diesel oil and its raw material rapeseed oil. An effective method was developed for the rapid determination of lead in rapeseed oil and bio-diesel oil by graphite furnace atomic absorption spectrometry (GFAAS) after their stabilization as microemulsions. In this research work, polyethyleneglycol octyl phenyl ether and n-butanol were used for emulsifier and auxiliary emulsifying agent, respectively. For Pb, efficient thermal stabilization was obtained using NH4H2PO4 as matrix modifier. Sample stabilization was necessary because of evident analyte losses that occurred immediately after sampling. Excellent long-term sample stabilization and the influence of the microemulsion composition on the GFAAS response were observed by mixing different organic solvents. The ashing and atomization temperature and ramp rate influenced the sensitivity obtained for Ph. Take this into account, the optimum conditions of the graphite furnace atomic absorption spectrometric determination of Pb in rapeseed oil and bio-diesel oil samples were investigated. The results showed that the microemulsion was quite stable when the value of V(20% polyethyleneglycol octyl phenyl ether), V(n-butanol), V(oil) and V(water) was 0.1: 8.9: 0.5: 0.5, without matrix interference effect. The determination limit of the proposed method was 126.2 microg x L(-1) for Pb, comfortably below the values found in the analyzed samples. The recoveries were from 81.8% to 109.0%, which performed using the addition of different concentrations of lead to bio-diesel oil, rapeseed oil and petrochemical diesel samples. The relative standard deviation of determination was 5.84%. This work showed the great efficiency of the microemulsion, indicating that it is possible to extract lead from the oil phase. The method was applied to the determination of lead in oil samples with satisfactory results.

Comparison of VFA titration procedures used for monitoring the biogas process.

PubMed

Lützhøft, Hans-Christian Holten; Boe, Kanokwan; Fang, Cheng; Angelidaki, Irini

2014-05-01

Titrimetric determination of volatile fatty acids (VFAs) contents is a common way to monitor a biogas process. However, digested manure from co-digestion biogas plants has a complex matrix with high concentrations of interfering components, resulting in varying results when using different titration procedures. Currently, no standardized procedure is used and it is therefore difficult to compare the performance among plants. The aim of this study was to evaluate four titration procedures (for determination of VFA-levels of digested manure samples) and compare results with gas chromatographic (GC) analysis. Two of the procedures are commonly used in biogas plants and two are discussed in literature. The results showed that the optimal titration results were obtained when 40 mL of four times diluted digested manure was gently stirred (200 rpm). Results from samples with different VFA concentrations (1-11 g/L) showed linear correlation between titration results and GC measurements. However, determination of VFA by titration generally overestimated the VFA contents compared with GC measurements when samples had low VFA concentrations, i.e. around 1 g/L. The accuracy of titration increased when samples had high VFA concentrations, i.e. around 5 g/L. It was further found that the studied ionisable interfering components had lowest effect on titration when the sample had high VFA concentration. In contrast, bicarbonate, phosphate and lactate had significant effect on titration accuracy at low VFA concentration. An extended 5-point titration procedure with pH correction was best to handle interferences from bicarbonate, phosphate and lactate at low VFA concentrations. Contrary, the simplest titration procedure with only two pH end-points showed the highest accuracy among all titration procedures at high VFA concentrations. All in all, if the composition of the digested manure sample is not known, the procedure with only two pH end-points should be the procedure of choice, due to its simplicity and accuracy. Copyright © 2014 Elsevier Ltd. All rights reserved.

Annual radiological environmental operating report, Browns Ferry Nuclear Plant, 1987

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

Not Available

1988-04-01

This report describes the environmental radiological monitoring programs conducted by TVA in the vicinity of Browns Ferry Nuclear Plant in 1987. The program includes the collection of samples from the environment and the determination of the concentrations of radioactive materials in the samples. Samples are taken from stations in the general area of the plant and from areas not influenced by plant operations. Station locations are selected after careful consideration of the weather patterns and projected radiation doses to the various areas around the plant. Material sampled includes air, water, milk, foods, vegetation, soil, fish, sediment, and direct radiation levels.more » Results from stations near the plant are compared with concentrations from control stations and with preoperational measurements to determine potential impacts of plant operations. The vast majority of the exposures calculated from environmental samples were contributed by naturally occurring radioactive materials or from materials commonly found in the environment as a result of atmospheric nuclear weapons fallout. Small amounts of Co-60 were found in sediment samples downstreams from the plant. This activity in stream sediment would result in no measurable increase over background in the dose to the general public. 3 refs., 2 figs., 34 tabs.« less

Browns Ferry Nuclear Plant annual radiological environmental operating report, 1990

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

Not Available

1991-04-01

This report describes the environmental radiological monitoring program conducted by TVA in the vicinity of Browns Ferry Nuclear Plant in 1990. The program includes the collection of samples from the environment and the determination of the concentrations of radioactive materials in the samples. Samples are taken from stations in the general area of the plant and from areas not influenced by plant operations. Station locations are selected after careful consideration of the weather patterns and projected radiation doses to the various areas around the plant. Material sampled includes air, water, milk, foods, vegetation, soil, fish, sediment, and direct radiation levels.more » Results from stations near the plant are compared with concentrations from control stations and with preoperational measurements to determine potential impacts of plant operations. The vast majority of the exposures calculated from environmental samples were contributed by naturally occurring radioactive materials or from materials commonly found in the environment as a result of atmospheric nuclear weapons fallout. Small amounts of Co-60 were found in sediment samples downstream from the plant. This activity in stream sediment would result in no measurable increase over background in the dose to the general public. 4 refs., 2 figs., 2 tabs.« less

Annual radiological environmental operating report, Browns Ferry Nuclear Plant, 1989

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

Not Available

1990-04-01

This report describes the environmental radiological monitoring program conducted by TVA in the vicinity of Browns Ferry Nuclear Plant (BFN) in 1989. The program includes the collection of samples from the environment and the determination of the concentrations of radioactive materials in the samples. Samples are taken from stations in the general area of the plant and from areas not influenced by plant operations. Station locations are selected after careful consideration of the weather patterns and projected radiation doses to the various areas around the plant. Material sampled includes air, water, milk, foods, vegetation, soil, fish, sediment, and direct radiationmore » levels. Results from stations near the plant are compared with concentrations from control stations and with preoperational measurements to determine potential impacts if plant operations. The vast majority of the exposures calculated from environmental samples were contributed by naturally occurring radioactive materials or from materials commonly found in the environment as a result of atmospheric nuclear weapons fallout. Small amounts of Co-60 were found in sediment samples downstream from the plant. This activity in river sediment would result in no measurable increase over background in the dose to the general public. 4 refs., 2 figs., 2 tabs.« less

Annual radiological environmental operating report, Browns Ferry Nuclear Plant, 1988

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

Not Available

1989-04-01

This report describes the environmental radiological monitoring program conducted by TVA in the vicinity of Browns Ferry Nuclear Plant in 1988. The program includes the collection of samples from the environment and the determination of the concentrations of radioactive materials in the samples. Samples are taken from stations in the general area of the plant and from areas not influenced by plant operations. Station locations are selected after careful consideration of the weather patterns and projected radiation doses to the various areas around the plant. Material sampled includes air, water, milk, foods, vegetation, soil, fish, sediment, and direct radiation levels.more » Results from stations near the plant are compared with concentrations from control stations and with preoperational measurements to determine potential impacts of plant operations. The vast majority of the exposures calculated from environmental samples were contributed by naturally occurring radioactive materials or from materials commonly found in the environment as a result of atmospheric nuclear weapons fallout. Small amounts of Co-60 were found in sediment samples downstream from the plant. This activity in stream sediment would result in no measurable increase over background in the dose to the general public. 3 refs., 2 figs., 2 tabs.« less

Collaborative study using common samples to evaluate the performance of anti-drug antibody assays constructed by different companies.

PubMed

Niimi, Shingo; Nishimiya, Kazuhiro; Nishidate, Masanobu; Saito, Tetsu; Minoura, Kyoko; Kadotsuji, Kenta; Shimakura, Jin; Shigemizu, Hiroko; Hosogi, Jun; Adachi, Maiko; Hashimoto, Tsutomu; Mori, Tamiki; Harada, Hideki; Yamamoto, Ken-Ichi; Nakamura, Takahiro; Nomura, Tatsuki; Yamaguchi, Itadaki; Sonehara, Kazuhiko; Ishii-Watabe, Akiko; Kawasaki, Nana

2018-04-01

This study was undertaken to evaluate the performance of anti-drug antibody (ADA) assays constructed by each participating company using common samples including ADA, drug and human serum. The ADA assays constructed by each company showed good sensitivity and precision for evaluation of ADA. Cut points for screening and confirmatory assays and assay selectivity were determined by various calculation methods. In evaluations of blind ADA samples, nearly similar results were obtained by the study companies in determinations of whether samples were positive or negative except at the lowest sample concentration (5 ng/mL). In measurement of drug tolerance, for almost samples containing ADA and drugs, more positive results were obtained in assays using acid dissociation compared to those without acid dissociation. Overall, the performance of ADA assays constructed by the 10 companies participating in this study was acceptable in terms of sensitivity and reproducibility for detection and evaluation of immunogenicity in both patients and healthy subjects. On the other hand, based on results for samples containing ADA and drugs, validity of results for ADA assays conducted without acid dissociation was less meaningful and more difficult to evaluate. Thus, acid dissociation was confirmed to be useful for improving drug tolerance. Copyright © 2018 The Japanese Society for the Study of Xenobiotics. Published by Elsevier Ltd. All rights reserved.

Optimum sample size allocation to minimize cost or maximize power for the two-sample trimmed mean test.

PubMed

Guo, Jiin-Huarng; Luh, Wei-Ming

2009-05-01

When planning a study, sample size determination is one of the most important tasks facing the researcher. The size will depend on the purpose of the study, the cost limitations, and the nature of the data. By specifying the standard deviation ratio and/or the sample size ratio, the present study considers the problem of heterogeneous variances and non-normality for Yuen's two-group test and develops sample size formulas to minimize the total cost or maximize the power of the test. For a given power, the sample size allocation ratio can be manipulated so that the proposed formulas can minimize the total cost, the total sample size, or the sum of total sample size and total cost. On the other hand, for a given total cost, the optimum sample size allocation ratio can maximize the statistical power of the test. After the sample size is determined, the present simulation applies Yuen's test to the sample generated, and then the procedure is validated in terms of Type I errors and power. Simulation results show that the proposed formulas can control Type I errors and achieve the desired power under the various conditions specified. Finally, the implications for determining sample sizes in experimental studies and future research are discussed.

Spectrophotometric determination of L-cysteine by using polyvinylpyrrolidone-stabilized silver nanoparticles in the presence of barium ions.

PubMed

Bamdad, Farzad; Khorram, Fateme; Samet, Maryam; Bamdad, Kourosh; Sangi, Mohammad Reza; Allahbakhshi, Fateme

2016-05-15

In this article a simple and selective colorimetric probe for cysteine determination using silver nano particles (AgNPS) is described. The determination process was based upon the surface plasmon resonance properties of polyvinylpyrrolidone-stabilized AgNPS. Interaction of AgNPS with cysteine molecules in the presence of barium ions induced a red shift in the surface plasmon resonance (SPR) maximum of AgNPs, as a result of nanoparticle aggregation. Consequently, yellow color of AgNP solution was changed to pink. The linear range for the determination of cysteine was 3.2-8.2 μM (R=0.9965) with a limit of detection equal to 2.8 μM (3σ). The proposed method was successfully applied to the determination of cysteine in human plasma samples. Acceptable recovery results of the spiked samples confirmed the validity of the proposed method. Copyright © 2016 Elsevier B.V. All rights reserved.

Spectrophotometric determination of L-cysteine by using polyvinylpyrrolidone-stabilized silver nanoparticles in the presence of barium ions

NASA Astrophysics Data System (ADS)

Bamdad, Farzad; Khorram, Fateme; Samet, Maryam; Bamdad, Kourosh; Sangi, Mohammad Reza; Allahbakhshi, Fateme

2016-05-01

In this article a simple and selective colorimetric probe for cysteine determination using silver nano particles (AgNPS) is described. The determination process was based upon the surface plasmon resonance properties of polyvinylpyrrolidone-stabilized AgNPS. Interaction of AgNPS with cysteine molecules in the presence of barium ions induced a red shift in the surface plasmon resonance (SPR) maximum of AgNPs, as a result of nanoparticle aggregation. Consequently, yellow color of AgNP solution was changed to pink. The linear range for the determination of cysteine was 3.2-8.2 μM (R = 0.9965) with a limit of detection equal to 2.8 μM (3σ). The proposed method was successfully applied to the determination of cysteine in human plasma samples. Acceptable recovery results of the spiked samples confirmed the validity of the proposed method.

Comparison of Thellier-type and multispecimen absolute paleointensities obtained on Miocene to historical lava flows from Lanzarote (Canary Islands, Spain)

NASA Astrophysics Data System (ADS)

Calvo-Rathert, M.; Morales, J.; Carrancho, Á.; Gogichaishvili, A.

2015-12-01

A paleomagnetic, rock-magnetic and paleointensity study has been carried out on 16 Miocene, Pleistocene, Quaternary and historical lava flows from Lanzarote (Canary Islands, Spain) with two main goals: (i) Compare paleointensity results obtained with two different techniques (Thellier-type and multispecimen) and (ii) obtain new paleointensity data. Initial rock-magnetic experiments on selected samples from each site were carried out to find out the carriers of remanence and to determine their thermal stability and grain size. They included the measurement of thermomagnetic curves, hysteresis parameters and IRM acquisition curves. Mostly reversible but also non-reversible curves were recorded in thermomagnetic experiments, with low-Ti titanomagnetite being the main carrier of remanence in most studied flows. Paleomagnetic analysis showed in most cases a single component and a characteristic component could be determined in 15 flows, all displaying normal-polarity. 83 samples from 13 flows were chosen for paleointensity experiments. In order to compare paleointensity results from exactly the same samples, they were cut into smaller specimens so that in each case a specimen was available to be used for a Thellier-type paleointensity determination, another one for a multispecimen paleointensity experiment and another one for rock-magnetic experiments. Thermomagnetic curves could be therefore measured on all samples subjected to paleointensity experiments. Thellier-type paleointensity determinations were performed with the Coe method between room temperature and 581°C on small (0.9 cm diameter and 1 to 2.5 cm length) specimens. After heating, samples were left cooling down naturally during several hours. Multispecimen paleointensity determinations were carried out using the method of Dekkers and Böhnel. The aforementioned sub-samples were cut into 8 specimens and pressed into salt pellets in order to obtain standard cylindrical specimens. A set of eight experiments was performed using laboratory fields from 10 to 80 μT, with increments of 10 μT. Samples were oriented in such a way that the NRM directions of each sub specimen lay parallel to the axis of the heating chamber and were heated at a temperature of 450°C. Results obtained with both methods are compared and discussed.

Quality of wet deposition in the Grand Calumet River watershed, northwestern Indiana, October 17, 1995-November 12, 1996

USGS Publications Warehouse

Willoughby, Timothy C.

2000-01-01

In June 1992, a wet-deposition collection site was established at the Gary (Indiana) Regional Airport to monitor the quantity and chemical quality of wet deposition. During the first phase of sampling, 48 wet-deposition samples were collected between June 30, 1992, and August 31, 1993. A second phase of sampling began in October 1995. During the second phase of sampling, 40 wet-deposition samples were collected between October 17, 1995, and November 12, 1996. This report presents the findings for the second phase of sampling and compares those results to the first phase of sampling. Northwestern Indiana is a heavily industrialized area. Steel production and petroleum refining are two of the area?s predominant industries. 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 northwestern Indiana and Lake Michigan. Wet-deposition samples collected during the first and second phases of sampling were analyzed for pH, specific conductance, and selected major ions and trace metals. Forty weekly wet-deposition samples were collected at the Gary (Indiana) Regional Airport during the second phase of sampling. Approximately 1.2 times as much wet deposition was collected during the second phase of sampling compared to the first phase. Statistically significant increases (at the 5-percent significance level) in concentrations of potassium, iron, lead, and zinc were determined for samples collected during the second phase of sampling when compared to the first. No statistically significant differences were determined in constituent concentrations between samples collected during warm weather (April 1 through October 31) and during cold weather (November 1 through March 31). Annual loadings for the second phase of sampling were greater than 2 times the loadings determined during the first phase of sampling for silica, iron, potassium, lead, and zinc.

The effect of pathological processes on absorption and scattering spectra of samples of bile and pancreatic juice

NASA Astrophysics Data System (ADS)

Giraev, K. M.; Ashurbekov, N. A.; Magomedov, M. A.; Murtazaeva, A. A.; Medzhidov, R. T.

2015-07-01

Spectra of optical transmission coefficients and optical reflectance for bile and pancreatic juice samples were measured experimentally for different forms of pathologies of the pancreas within the range of 250-2500 nm. The absorption and scattering spectra, as well as the spectrum of the anisotropy factor of scattering, were determined based on the results obtained using the reverse Monte Carlo method. The surface morphology for the corresponding samples of the biological media was studied employing electron microscopy. The dynamics of the optical properties of the biological media was determined depending on the stage of the pathology. It has been demonstrated that the results of the study presented are in a good agreement with pathophysiological data and could supplement and broaden the results of conventional methods for diagnostics of the pancreas.

Probing the microscopic environment of 23 Na ions in brain tissue by MRI: On the accuracy of different sampling schemes for the determination of rapid, biexponential T2* decay at low signal-to-noise ratio.

PubMed

Lommen, Jonathan M; Flassbeck, Sebastian; Behl, Nicolas G R; Niesporek, Sebastian; Bachert, Peter; Ladd, Mark E; Nagel, Armin M

2018-08-01

To investigate and to reduce influences on the determination of the short and long apparent transverse relaxation times ( T2,s*, T2,l*) of 23 Na in vivo with respect to signal sampling. The accuracy of T2* determination was analyzed in simulations for five different sampling schemes. The influence of noise in the parameter fit was investigated for three different models. A dedicated sampling scheme was developed for brain parenchyma by numerically optimizing the parameter estimation. This scheme was compared in vivo to linear sampling at 7T. For the considered sampling schemes, T2,s* / T2,l* exhibit an average bias of 3% / 4% with a variation of 25% / 15% based on simulations with previously published T2* values. The accuracy could be improved with the optimized sampling scheme by strongly averaging the earliest sample. A fitting model with constant noise floor can increase accuracy while additional fitting of a noise term is only beneficial in case of sampling until late echo time > 80 ms. T2* values in white matter were determined to be T2,s* = 5.1 ± 0.8 / 4.2 ± 0.4 ms and T2,l* = 35.7 ± 2.4 / 34.4 ± 1.5 ms using linear/optimized sampling. Voxel-wise T2* determination of 23 Na is feasible in vivo. However, sampling and fitting methods have to be chosen carefully to retrieve accurate results. Magn Reson Med 80:571-584, 2018. © 2018 International Society for Magnetic Resonance in Medicine. © 2018 International Society for Magnetic Resonance in Medicine.

Simultaneous determination of inorganic and organic ions in plant parts of Betula pendula from two different types of ecosystems (Wielkopolski National Park and Chemical Plant in Luboń, Poland).

PubMed

Frankowski, Marcin

2016-06-01

The results of inorganic and organic anion concentrations in samples of soils and plant parts of Betula pendula (tap roots, lateral roots, stem, twigs, leaves), in the bioavailable fraction, are presented in this study. An ion chromatography method was applied for the first time in the simultaneous determination of inorganic and organic anions, as an effective tool for qualitative and quantitative analysis of samples with different matrix. A linear gradient elution with potassium hydroxide allowed for the separation of both inorganic and organic ions such as: F(-), CH3COO(-), HCOO(-), Cl(-), NO2 (-), Br(-) and NO3 (-), SO4 (2-), CH2(COO)2 (2-), C2O4 (2-), PO4 (3-) and C3H5O(COO)3 (3-). The samples of soils and plant parts of B. pendula from the area of the Wielkopolski National Park (WNP) and the Chemical Plant in Luboń (LU; protected vs. contaminated area) were selected for the study. The obtained results indicated that such inorganic ions as: F(-), Cl(-), NO3 (-) and PO4 (3-) are quite easily transported from soil to leaves. In contrast, the mechanism of migration could not be clearly defined for SO4 (2-) because the ion was retained in roots of many of the analysed samples. Significantly higher bioavailability of inorganic ions was observed for samples collected from the area of the WNP. Phosphates were the only ions which showed no variation in their concentrations between the two sampling sites, both for soils and plant parts of B. pendula. None of the organic anions was detected in soil samples. The acetate, formate, malonate, oxalate and citrate ions were detected in all leaf samples. The statistical analysis allowed the author to determine the mechanism of ion migration and accumulation in leaves and, additionally, determine the variation in the occurrence of inorganic and organic ions depending on the sampling site (WNP vs. LU). The results of the statistical analysis were confirmed by the bioacumulation (BF) and translocation (TF) factors.

Determination of furfural and hydroxymethylfurfural from baby formula using headspace solid phase microextraction based on nanostructured polypyrrole fiber coupled with ion mobility spectrometry.

PubMed

Kamalabadi, Mahdie; Ghaemi, Elham; Mohammadi, Abdorreza; Alizadeh, Naader

2015-08-15

Furfural (Fu) and hydroxymethylfurfural (HMFu) are extracted using a dodecylbenzenesulfonate-doped polypyrrole coating as a fiber for headspace solid phase microextraction (HS-SPME) method in baby formula samples and detected using ion mobility spectrometry (IMS). Sample pH, salt effect, extraction time and temperature were investigated and optimized as effective parameters in HS-SPME. The calibration curves were linear in the range of 20-300 ng g(-1) (R(2)>0.99). Limits of detection for Fu and HMFu were 6 ng g(-1) and 5 ng g(-1), respectively. The RSD% of Fu and HMFu for five analyses was 4.4 and 4.9, respectively. The proposed method was successfully applied to determine of Fu and HMFu in the different baby formula samples with satisfactory result. The results were in agreement with those obtained using HPLC analysis. The HS-SPME-IMS is precise, selective and sensitive analytical method for determination of Fu and HMFu in baby formula samples, without any derivatization process. Copyright © 2015 Elsevier Ltd. All rights reserved.

Determination of benzylpenicillin in pharmaceuticals by capillary zone electrophoresis

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

Hoyt, A.M. Jr.; Sepaniak, M.J.

A rapid and direct method is described for the determination of benzylpenicillin (penicillin G) in pharmaceutical preparations. The method involves very little sample preparation and total analysis time for duplicate results is less 30 minutes per sample. The method takes advantage of the speed and separating power of capillary zone electrophoresis (CZE). Detection of penicillin is by absorption at 228 nm. An internal standard is employed to reduce sample injection error. The method was applied successfully to both tablets and injectable preparations. 14 refs., 5 figs., 3 tabs.

Slurry sampling high-resolution continuum source electrothermal atomic absorption spectrometry for direct beryllium determination in soil and sediment samples after elimination of SiO interference by least-squares background correction.

PubMed

Husáková, Lenka; Urbanová, Iva; Šafránková, Michaela; Šídová, Tereza

2017-12-01

In this work a simple, efficient, and environmentally-friendly method is proposed for determination of Be in soil and sediment samples employing slurry sampling and high-resolution continuum source electrothermal atomic absorption spectrometry (HR-CS-ETAAS). The spectral effects originating from SiO species were identified and successfully corrected by means of a mathematical correction algorithm. Fractional factorial design has been employed to assess the parameters affecting the analytical results and especially to help in the development of the slurry preparation and optimization of measuring conditions. The effects of seven analytical variables including particle size, concentration of glycerol and HNO 3 for stabilization and analyte extraction, respectively, the effect of ultrasonic agitation for slurry homogenization, concentration of chemical modifier, pyrolysis and atomization temperature were investigated by a 2 7-3 replicate (n = 3) design. Using the optimized experimental conditions, the proposed method allowed the determination of Be with a detection limit being 0.016mgkg -1 and characteristic mass 1.3pg. Optimum results were obtained after preparing the slurries by weighing 100mg of a sample with particle size < 54µm and adding 25mL of 20% w/w glycerol. The use of 1μg Rh and 50μg citric acid was found satisfactory for the analyte stabilization. Accurate data were obtained with the use of matrix-free calibration. The accuracy of the method was confirmed by analysis of two certified reference materials (NIST SRM 2702 Inorganics in Marine Sediment and IGI BIL-1 Baikal Bottom Silt) and by comparison of the results obtained for ten real samples by slurry sampling with those determined after microwave-assisted extraction by inductively coupled plasma time of flight mass spectrometry (TOF-ICP-MS). The reported method has a precision better than 7%. Copyright © 2017 Elsevier B.V. All rights reserved.

[Exploration of rapidly determining quality of traditional Chinese medicines by (NIR) spectroscopy based on internet sharing mode].

PubMed

Ni, Li-Jun; Luan, Shao-Rong; Zhang, Li-Guo

2016-10-01

Because of the numerous varieties of herbal species and active ingredients in the traditional Chinese medicine(TCM),the traditional methods employed could hardly satisfy the current determination requirements of TCM.The present work proposed an idea to realize rapid determination of the quality of TCM based on near infrared(NIR)spectroscopy and internet sharing mode. Low cost and portable multi-source composite spectrometer was invented by our group for in-site fast measurement of spectra of TCM samples. The database could be set up by sharing spectra and quality detection data of TCM samples among TCM enterprises based on the internet platform.A novel method called as keeping same relationship between X and Y space based on K nearest neighbors(KNN-KSR for short)was applied to predict the contents of effective compounds of the samples. In addition,a comparative study between KNN-KSR and partial least squares(PLS)was conducted. Two datasets were applied to validate above idea:one was about 58 Ginkgo Folium samples samples measured with four near-infrared spectroscopy instruments and two multi-source composite spectrometers,another one was about 80 corn samples available online measured with three NIR instruments. The results show that the KNN-KSR method could obtain more reliable outcomes without correcting spectrum.However transforming the PLS models to other instruments could hardly acquire better predictive results until spectral calibration is performed. Meanwhile,the similar analysis results of total flavonoids and total lactones of Ginkgo Folium samples are achieved on the multi-source composite spectrometers and near-infrared spectroscopy instruments,and the prediction results of KNN-KSR are better than PLS. The idea proposed in present study is in urgent need of more samples spectra, and then to be verified by more case studies. Copyright© by the Chinese Pharmaceutical Association.

Determination of As, Cd, Hg and Pb in herbs using slurry sampling electrothermal vaporisation inductively coupled plasma mass spectrometry.

PubMed

Lin, Mei-Ling; Jiang, Shiuh-Jen

2013-12-01

Inductively coupled plasma mass spectrometry coupled with ultrasonic slurry sampling electrothermal vaporisation (USS-ETV-ICP-MS) has been applied to determine As, Cd, Hg and Pb in 0.5% m/v slurries of several herb samples. 1% m/v 8-Hydroxyquinoline was used as the modifier to enhance the ion signals. The influences of instrument operating conditions, slurry preparation and interferences on the ion signals were reported. This method has been applied to the determination of As, Cd, Hg and Pb in NIST SRM 1547 peach leaves and SRM 1573a tomato leaves reference materials and three herb samples purchased from the local market and ground to 150 μm. The analysis results of the standard reference materials agreed with the certified values which are at sub μg g(-1) levels. Precision between sample replicates was better than 4% for all the determinations. The method detection limits estimated from standard addition curves were about 0.3, 0.1, 0.1 and 0.2 ng g(-1) for As, Cd, Hg and Pb, respectively, in original herb samples. Copyright © 2013 Elsevier Ltd. All rights reserved.

Solid phase extraction of amoxicillin using dibenzo-18-crown-6 modified magnetic-multiwalled carbon nanotubes prior to its spectrophotometric determination.

PubMed

Ahmadi, Mazaher; Madrakian, Tayyebeh; Afkhami, Abbas

2016-01-01

This work reports on a method for selective extraction and sensitive determination of amoxicillin drug (AMX). The method is based on solid phase extraction of AMX by a novel modified magnetic nanoadsorbent prior to spectrophotometric determination of AMX using a procedure based on formation a colored azo-derivative of the investigated drug. The nanoadsorbent has been synthesized by modification of magnetic-multiwalled carbon nanotube with dibenzo-18-crown-6 moieties. The synthesized nanoparticles were characterized using TEM, XRD and FT-IR measurements. At the next step, various factors that could potentially affect adsorption and desorption efficiencies of AMX, have been optimized. The results showed that under the optimized conditions, sensitive and selective determination of the investigated drug in concentration range of 5.0-1000.0 ng mL(-1) with the limit of detection of 3.0 ng mL(-1) was achievable. Furthermore, the real sample analysis (i.e. amoxicillin capsules and human urine samples) results indicated that a reliable promising candidate method has been developed for the determination of AMX in the investigated real samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Antimicrobial effect of sour pomegranate sauce on Escherichia coli O157:H7 and Staphylococcus aureus.

PubMed

Kışla, Duygu; Karabıyıklı, Şeniz

2013-05-01

Pomegranate sauce is one of the most popular pomegranate products produced in Turkey. This study was conducted to determine the minimum inhibitory concentrations (MICs) of both traditional and commercial sour pomegranate sauce samples on Staphylococcus aureus (ATCC 25923) and Escherichia coli O157:H7 (ATCC 43895). The initial microflora of the pomegranate sauce samples was determined by performing the enumerations of total aerobic mesophilic bacteria, yeast and mold, S. aureus, E. coli, and the determination of Salmonella spp. MIC tests were applied to the neutralized and the original (unneutralized) sour pomegranate sauce samples in order to put forth the inhibition effect depending on low pH value. It was found that inhibitory effect of the traditional and the commercial samples, except one sample, on pathogens was not only due to the acidity of the products. The results of MIC tests indicated that although both traditional and commercial samples showed a considerable inhibitory effect on test microorganisms, the traditional pomegranate sauce samples were more effective than the commercial ones. © 2013 Institute of Food Technologists®

Direct spectral analysis of tea samples using 266 nm UV pulsed laser-induced breakdown spectroscopy and cross validation of LIBS results with ICP-MS.

PubMed

Gondal, M A; Habibullah, Y B; Baig, Umair; Oloore, L E

2016-05-15

Tea is one of the most common and popular beverages spanning vast array of cultures all over the world. The main nutritional benefits of drinking tea are its anti-oxidant properties, presumed protection against certain cancers, inhibition of inflammation and possible protective effects against diabetes. Laser induced breakdown spectrometer (LIBS) was assembled as a powerful tool for qualitative and quantitative analysis of various brands of tea samples using 266 nm pulsed UV laser. LIBS spectra for six brands of tea samples in the wavelength range of 200-900 nm was recorded and all elements present in our tea samples were identified. The major toxic elements detected in several brands of tea samples were bromine, chromium and minerals like iron, calcium, potassium and silicon. The spectral assignment was conducted prior to the determination of concentration of each element. For quantitative analysis, calibration curves were drawn for each element using standard samples prepared in known concentration in the tea matrix. The plasma parameters (electron temperature and electron density) were also determined prior to the tea samples spectroscopic analysis. The concentration of iron, chromium, potassium, bromine, copper, silicon and calcium detected in all tea samples was between 378-656, 96-124, 1421-6785, 99-1476, 17-36, 2-11 and 92-130 mg L(-1) respectively. The limits of detection estimated for Fe, Cr, K, Br, Cu, Si, Ca in tea samples were 22, 12, 14, 11, 6, 1 and 12 mg L(-1) respectively. To further confirm the accuracy of our LIBS results, we determined the concentration of each element present in tea samples by using standard analytical technique like ICP-MS. The concentrations detected with our LIBS system are in excellent agreement with ICP-MS results. The system assembled for spectral analysis in this work could be highly applicable for testing the quality and purity of food and also pharmaceuticals products. Copyright © 2016 Elsevier B.V. All rights reserved.

Measurements of induced radioactivity in some LDEF samples

NASA Technical Reports Server (NTRS)

Moss, C. E.; Reedy, R. C.

1992-01-01

Twenty-six stainless steel trunnion samples, five aluminum end support retainer plate samples, two aluminum keel plate samples, and two titanium clips were analyzed. The shielded high purity germanium detectors used had efficiencies of 33, 54, and 80 percent at 1332 keV. Detector efficiencies as a function of energy and corrections for self-absorption in the samples were determined with calibrated sources and unactivated control samples. Several measurements were made on most samples. In the trunnion samples, Mn-54 and Co-57 were seen and limits were obtained for other isotopes. The results agree well with 1-D activation calculations for an anisotropic trapped proton model. In the aluminum and titanium samples, Na-22 was detected. Other results are presented.

Measurements of induced radioactivity in some LDEF samples

NASA Technical Reports Server (NTRS)

Moss, C. E.; Reedy, R. C.

1991-01-01

Twenty-six stainless steel trunnion samples, five aluminum end support retainer plate samples, two aluminum keel plate samples, and two titanium clips were analyzed. The shielded high purity germanium detectors used had efficiencies of 33, 54, and 80 pcts. at 1332 keV. Detector efficiencies as a function of energy and corrections for self absorption in the samples were determined with calibrated sources, unactivated control samples, and calculations. Several measurements were made on most samples. In the trunnion samples, Mn-54 and Co-57 were seen and limits were obtained for other isotopes. The results agree well with 1-D activation calculations for an anisotropic trapped proton model. In the aluminum samples, Na-22 and Be-7 were seen. Other results are presented.

Determination of Zn/Cu ratio and oligoelements in serum samples by total reflection X-ray fluorescence spectrometry for cancer diagnosis

NASA Astrophysics Data System (ADS)

Marcó P., L. M.; Jiménez, E.; Hernández C., E. A.; Rojas, A.; Greaves, E. D.

2001-11-01

The method of quantification using the Compton peak as an internal standard, developed in a previous work, was applied to the routine determination of Fe, Cu, Zn and Se in serum samples from normal individuals and cancer patients by total reflection X-ray fluorescence spectrometry. Samples were classified according to age and sex of the donor, in order to determine reference values for normal individuals. Results indicate that the Zn/Cu ratio and the Cu concentration could prove to be useful tools for cancer diagnosis. Significant differences in these parameters between the normal and cancer group were found for all age ranges. The multielemental character of the technique, coupled with the small amounts of sample required and the short analysis time make it a valuable tool in clinical analysis.

Biomass Thermogravimetric Analysis: Uncertainty Determination Methodology and Sampling Maps Generation

PubMed Central

Pazó, Jose A.; Granada, Enrique; Saavedra, Ángeles; Eguía, Pablo; Collazo, Joaquín

2010-01-01

The objective of this study was to develop a methodology for the determination of the maximum sampling error and confidence intervals of thermal properties obtained from thermogravimetric analysis (TG), including moisture, volatile matter, fixed carbon and ash content. The sampling procedure of the TG analysis was of particular interest and was conducted with care. The results of the present study were compared to those of a prompt analysis, and a correlation between the mean values and maximum sampling errors of the methods were not observed. In general, low and acceptable levels of uncertainty and error were obtained, demonstrating that the properties evaluated by TG analysis were representative of the overall fuel composition. The accurate determination of the thermal properties of biomass with precise confidence intervals is of particular interest in energetic biomass applications. PMID:20717532

Emperical Tests of Acceptance Sampling Plans

NASA Technical Reports Server (NTRS)

White, K. Preston, Jr.; Johnson, Kenneth L.

2012-01-01

Acceptance sampling is a quality control procedure applied as an alternative to 100% inspection. A random sample of items is drawn from a lot to determine the fraction of items which have a required quality characteristic. Both the number of items to be inspected and the criterion for determining conformance of the lot to the requirement are given by an appropriate sampling plan with specified risks of Type I and Type II sampling errors. In this paper, we present the results of empirical tests of the accuracy of selected sampling plans reported in the literature. These plans are for measureable quality characteristics which are known have either binomial, exponential, normal, gamma, Weibull, inverse Gaussian, or Poisson distributions. In the main, results support the accepted wisdom that variables acceptance plans are superior to attributes (binomial) acceptance plans, in the sense that these provide comparable protection against risks at reduced sampling cost. For the Gaussian and Weibull plans, however, there are ranges of the shape parameters for which the required sample sizes are in fact larger than the corresponding attributes plans, dramatically so for instances of large skew. Tests further confirm that the published inverse-Gaussian (IG) plan is flawed, as reported by White and Johnson (2011).

Determination of vitamins D2 and D3 in selected food matrices by online high-performance liquid chromatography-gas chromatography-mass spectrometry (HPLC-GC-MS).

PubMed

Nestola, Marco; Thellmann, Andrea

2015-01-01

An online normal-phase liquid chromatography-gas chromatography-mass spectrometry (HPLC-GC-MS) method was developed for the determination of vitamins D2 and D3 in selected food matrices. Transfer of the sample from HPLC to GC was realized by large volume on-column injection; detection was performed with a time-of-flight mass spectrometer (TOF-MS). Typical GC problems in the determination of vitamin D such as sample degradation or sensitivity issues, previously reported in the literature, were not observed. Determination of total vitamin D content was done by quantitation of its pyro isomer based on an isotopically labelled internal standard (ISTD). Extracted ion traces of analyte and ISTD showed cross-contribution, but non-linearity of the calibration curve was not determined inside the chosen calibration range by selection of appropriate quantifier ions. Absolute limits of detection (LOD) and quantitation (LOQ) for vitamins D2 and D3 were calculated as approximately 50 and 150 pg, respectively. Repeatability with internal standard correction was below 2 %. Good agreement between quantitative results of an established high-performance liquid chromatography with UV detection (HPLC-UV) method and HPLC-GC-MS was found. Sterol-enriched margarine was subjected to HPLC-GC-MS and HPLC-MS/MS for comparison, because HPLC-UV showed strong matrix interferences. HPLC-GC-MS produced comparable results with less manual sample cleanup. In summary, online hyphenation of HPLC and GC allowed a minimization in manual sample preparation with an increase of sample throughput.

Validating a refractometer to evaluate immunoglobulin G concentration in Jersey colostrum and the effect of multiple freeze-thaw cycles on evaluating colostrum quality.

PubMed

Morrill, K M; Robertson, K E; Spring, M M; Robinson, A L; Tyler, H D

2015-01-01

The objectives of this study were to (1) validate a method using refractometry to rapidly and accurately determine immunoglobulin (IgG) concentration in Jersey colostrum, (2) determine whether there should be different refractive index (nD) and %Brix cut points for Jersey colostrum, and (3) evaluate the effect of multiple freeze-thaw (FT) cycles on radial immunodiffusion (RID) and a digital refractometer to determine IgG concentration in Jersey colostrum. Samples (n=58; 3L) of colostrum were collected from a dairy in northwestern Iowa. Samples were analyzed within 2h of collection for IgG concentration by RID, %Brix, and nD by refractometer and an estimate of IgG by colostrometer. Samples were frozen, placed on dry ice, and transported to the laboratory at Iowa State University (Ames). Samples arrived frozen and were placed in a -20°C manual-defrost freezer until further analysis. On d 7 (1FT), d 14 (2FT), and 1yr (3FT) all samples were thawed, analyzed for IgG by RID, %Brix, nD by refractometer, and IgG estimate by colostrometer, and frozen until reanalysis at the next time point. Fresh colostrum had a mean (±SD) IgG concentration of 72.91 (±33.53) mg/mL, 21.24% (±4.43) Brix, and nD 1.3669 (±0.0074). Multiple FT cycles did affect IgG as determined by RID and colostrometer reading. The IgG concentrations were greater in fresh and 1FT samples as compared with 2FT and 3FT samples (72.91, 75.38, 67.20, and 67.31mg of IgG/mL, respectively). The colostrometer reading was lower in 1FT samples compared with fresh and 2FT samples. Multiple FT cycles had no effect on nD or %Brix reading. In fresh samples, IgG concentration was moderately correlated with nD (r=0.79), %Brix (r=0.79), and colostrometer reading (r=0.79). Diagnostic test characteristics using the recommended cut point of 1.35966 nD resulted in similar sensitivities for 1FT and 2 FT samples (94.87 and 94.74%, respectively). Cut points of 18 and 19% Brix resulted in the greatest sensitivities (92.31 and 84.62%) and specificity (94.74 and 94.74%, respectively). The 18% Brix cut point resulted in 94.83% of the samples being correctly classified based on IgG concentration. These data support the use of digital refractometer to accurately and rapidly determine IgG concentration in fresh Jersey colostrum. Additionally, these data suggest that IgG concentration determined by RID is affected by multiple FT cycles, whereas estimates obtained by refractometer are not affected by multiple FT cycles. Copyright © 2015 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Analysis of particulate contamination on tape lift samples from the VETA optical surfaces

NASA Technical Reports Server (NTRS)

Germani, Mark S.

1992-01-01

Particulate contamination analysis was carried out on samples taken from the Verification Engineering Test Article (VETA) x-ray detection system. A total of eighteen tape lift samples were taken from the VETA optical surfaces. Initially, the samples were tested using a scanning electron microscope. Additionally, particle composition was determined by energy dispersive x-ray spectrometry. Results are presented in terms of particle loading per sample.

Simultaneous Determination of Iron, Copper and Cobalt in Food Samples by CCD-diode Array Detection-Flow Injection Analysis with Partial Least Squares Calibration Model

NASA Astrophysics Data System (ADS)

Mi, Jiaping; Li, Yuanqian; Zhou, Xiaoli; Zheng, Bo; Zhou, Ying

2006-01-01

A flow injection-CCD diode array detection spectrophotometry with partial least squares (PLS) program for simultaneous determination of iron, copper and cobalt in food samples has been established. The method was based on the chromogenic reaction of the three metal ions and 2- (5-Bromo-2-pyridylazo)-5-diethylaminophenol, 5-Br-PADAP in acetic acid - sodium acetate buffer solution (pH5) with Triton X-100 and ascorbic acid. The overlapped spectra of the colored complexes were collected by charge-coupled device (CCD) - diode array detector and the multi-wavelength absorbance data was processed using partial least squares (PLS) algorithm. Optimum reaction conditions and parameters of flow injection analysis were investigated. The samples of tea, sesame, laver, millet, cornmeal, mung bean and soybean powder were determined by the proposed method. The average recoveries of spiked samples were 91.80%~100.9% for Iron, 92.50%~108.0% for Copper, 93.00%~110.5% for Cobalt, respectively with relative standard deviation (R.S.D) of 1.1%~12.1%. The sampling rate is 45 samples h-1. The determination results of the food samples were in good agreement between the proposed method and ICP-AES.

Determination of variables in the prediction of strontium distribution coefficients for selected sediments

USGS Publications Warehouse

Pace, M.N.; Rosentreter, J.J.; Bartholomay, R.C.

2001-01-01

Idaho State University and the US Geological Survey, in cooperation with the US Department of Energy, conducted a study to determine and evaluate strontium distribution coefficients (Kds) of subsurface materials at the Idaho National Engineering and Environmental Laboratory (INEEL). The Kds were determined to aid in assessing the variability of strontium Kds and their effects on chemical transport of strontium-90 in the Snake River Plain aquifer system. Data from batch experiments done to determine strontium Kds of five sediment-infill samples and six standard reference material samples were analyzed by using multiple linear regression analysis and the stepwise variable-selection method in the statistical program, Statistical Product and Service Solutions, to derive an equation of variables that can be used to predict strontium Kds of sediment-infill samples. The sediment-infill samples were from basalt vesicles and fractures from a selected core at the INEEL; strontium Kds ranged from ???201 to 356 ml g-1. The standard material samples consisted of clay minerals and calcite. The statistical analyses of the batch-experiment results showed that the amount of strontium in the initial solution, the amount of manganese oxide in the sample material, and the amount of potassium in the initial solution are the most important variables in predicting strontium Kds of sediment-infill samples.

Recovery and Determination of Adsorbed Technetium on Savannah River Site Charcoal Stack Samples

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

Lahoda, Kristy G.; Engelmann, Mark D.; Farmer, Orville T.

2008-03-01

Experimental results are provided for the sample analyses for technetium (Tc) in charcoal samples placed in-line with a Savannah River Site (SRS) processing stack effluent stream as a part of an environmental surveillance program. The method for Tc removal from charcoal was based on that originally developed with high purity charcoal. Presented is the process that allowed for the quantitative analysis of 99Tc in SRS charcoal stack samples with and without 97Tc as a tracer. The results obtained with the method using the 97Tc tracer quantitatively confirm the results obtained with no tracer added. All samples contain 99Tc at themore » pg g-1 level.« less

Determination of flavanol and procyanidin (by degree of polymerization 1-10) content of chocolate, cocoa liquors, powder(s), and cocoa flavanol extracts by normal phase high-performance liquid chromatography: collaborative study.

PubMed

Robbins, Rebecca J; Leonczak, Jadwiga; Li, Julia; Johnson, J Christopher; Collins, Tom; Kwik-Uribe, Catherine; Schmitz, Harold H

2012-01-01

An international collaborative study was conducted on an HPLC method with fluorescent detection (FLD) for the determination of flavanols and procyanidins in materials containing chocolate and cocoa. The sum of the oligomeric fractions with degree of polymerization 1-10 was the determined content value. Sample materials included dark and milk chocolates, cocoa powder, cocoa liquors, and cocoa extracts. The content ranged from approximately 2 to 500 mg/g (defatted basis). Thirteen laboratories representing commercial, industrial, and academic institutions in six countries participated in the study. Fourteen samples were sent as blind duplicates to the collaborators. Results from 12 laboratories yielded repeatability relative standard deviation (RSDr) values that were below 10% for all materials analyzed, ranging from 4.17 to 9.61%. The reproducibility relative standard deviation (RSD(R)) values ranged from 5.03 to 12.9% for samples containing 8.07 to 484.7 mg/g. In one sample containing a low content of flavanols and procyanidins (approximately 2 mg/g), the RSD(R) was 17.68%. Based on these results, the method is recommended for Official First Action for the determination of flavanols and procyanidins in chocolate, cocoa liquors, powder(s), and cocoa extracts.

2-Naphthalenthiol derivatization followed by dispersive liquid-liquid microextraction as an efficient and sensitive method for determination of acrylamide in bread and biscuit samples using high-performance liquid chromatography.

PubMed

Faraji, Mohammad; Hamdamali, Mohammadrezza; Aryanasab, Fezzeh; Shabanian, Meisam

2018-07-13

In this research, an ultrasonic-assisted extraction followed by 2-naphthalenthiol derivatization and dispersive liquid-liquid microextraction of acrylamide (AA) was developed as simple and sensitive sample preparation method for AA in bread and biscuit samples using high performance liquid chromatography. Influence of derivatization and microextraction parameters were evaluated and optimized. Results showed that the derivatization of AA leads to improve its hydrophobicity and chromatographic behavior. Under optimum conditions of derivatization and microextraction, the method yielded a linear calibration curve ranging from 10 to 1000 μg L -1 with a determination coefficient (R 2 ) of 0.9987. Limit of detection (LOD) and limit of quantification (LOQ) were 3.0 and 9.0 μg L -1 , respectively. Intra-day (n = 6) and inter-day (n = 3) precisions based on relative standard deviation percent (RSD%) for extraction and determination of AA at 50 and 500 μg L -1 levels were less than 9.0%. Finally, the performance of proposed method was investigated for determination of AA in some bread and biscuit samples, and satisfactory results were obtained (relative recovery ≥ 90%). Copyright © 2018. Published by Elsevier B.V.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of antimony by automated-hydride atomic absorption spectrophotometry

USGS Publications Warehouse

Brown, G.E.; McLain, B.J.

1994-01-01

The analysis of natural-water samples for antimony by automated-hydride atomic absorption spectrophotometry is described. Samples are prepared for analysis by addition of potassium and hydrochloric acid followed by an autoclave digestion. After the digestion, potassium iodide and sodium borohydride are added automatically. Antimony hydride (stibine) gas is generated, then swept into a heated quartz cell for determination of antimony by atomic absorption spectrophotometry. Precision and accuracy data are presented. Results obtained on standard reference water samples agree with means established by interlaboratory studies. Spike recoveries for actual samples range from 90 to 114 percent. Replicate analyses of water samples of varying matrices give relative standard deviations from 3 to 10 percent.

Method of Analysis by the U.S. Geological Survey California District Sacramento Laboratory?Determination of Trihalomethane Formation Potential, Method Validation, and Quality-Control Practices

USGS Publications Warehouse

Crepeau, Kathryn L.; Fram, Miranda S.; Bush, Noel

2004-01-01

An analytical method for the determination of the trihalomethane formation potential of water samples has been developed. The trihalomethane formation potential is measured by dosing samples with chlorine under specified conditions of pH, temperature, incubation time, darkness, and residual-free chlorine, and then analyzing the resulting trihalomethanes by purge and trap/gas chromatography equipped with an electron capture detector. Detailed explanations of the method and quality-control practices are provided. Method validation experiments showed that the trihalomethane formation potential varies as a function of time between sample collection and analysis, residual-free chlorine concentration, method of sample dilution, and the concentration of bromide in the sample.

Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Elements in Whole-Water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry

USGS Publications Warehouse

Garbarino, John R.; Struzeski, Tedmund M.

1998-01-01

Inductively coupled plasma-optical emission spectrometry (ICP-OES) and inductively coupled plasma-mass spectrometry (ICP-MS) can be used to determine 26 elements in whole-water digests. Both methods have distinct advantages and disadvantages--ICP-OES is capable of analyzing samples with higher elemental concentrations without dilution, however, ICP-MS is more sensitive and capable of determining much lower elemental concentrations. Both techniques gave accurate results for spike recoveries, digested standard reference-water samples, and whole-water digests. Average spike recoveries in whole-water digests were 100 plus/minus 10 percent, although recoveries for digests with high dissolved-solid concentrations were lower for selected elements by ICP-MS. Results for standard reference-water samples were generally within 1 standard deviation of hte most probable values. Statistical analysis of the results from 43 whole-water digest indicated that there was no significant difference among ICP-OES, ICP-MS, and former official methods of analysis for 24 of the 26 elements evaluated.

Method and apparatus for determining pressure-induced frequency-shifts in shock-compressed materials

DOEpatents

Moore, David S.; Schmidt, Stephen C.

1985-01-01

A method and an apparatus for conducting coherent anti-Stokes Raman scattering spectroscopy in shock-compressed materials are disclosed. The apparatus includes a sample vessel having an optically transparent wall and an opposing optically reflective wall. Two coherent laser beams, a pump beam and a broadband Stokes beam, are directed through the window and focused on a portion of the sample. In the preferred embodiment, a projectile is fired from a high-pressure gas gun to impact the outside of the reflective wall, generating a planar shock wave which travels through the sample toward the window. The pump and Stokes beams result in the emission from the shock-compressed sample of a coherent anti-Stokes beam, which is emitted toward the approaching reflective wall of the vessel and reflected back through the window. The anti-Stokes beam is folded into a spectrometer for frequency analysis. The results of such analysis are useful for determining chemical and physical phenomena which occur during the shock-compression of the sample.

A comparative study of neutron activation analysis and proton-induced X-ray emission analysis for the determination of heavy metals in estuarine sediments

NASA Astrophysics Data System (ADS)

Randle, K.; Al-Jundi, J.; Mamas, C. J. V.; Sokhi, R. S.; Earwaker, L. G.

1993-06-01

Our work on heavy metals in the estuarine environment has involved the use of two multielement techniques: neutron activation analysis (NAA) and proton-induced X-ray emission (PIXE) analysis. As PIXE is essentially a surface analytical technique problems may arise due to sample inhomogeneity and surface roughness. In order to assess the contribution of these effects we have compared the results from PIXE analysis with those from a technique which analyzes a larger bulk sample rather than just the surface. An obvious method was NAA. A series of sediment samples containing particles of variable diameter were compared. Pellets containing a few mg of sediment were prepared from each sample and analyzed by the PIXE technique using both an absolute and a comparitive method. For INAA the rest of the sample was then irradiated with thermal neutrons and element concentrations determined from analyses of the subsequent gamma-ray spectrum. Results from the two methods are discussed.

Method and apparatus for determining pressure-induced frequency-shifts in shock-compressed materials

DOEpatents

Moore, D.S.; Schmidt, S.C.

1983-12-16

A method and an apparatus for conducting coherent anti-Stokes Raman scattering spectroscopy in shock-compressed materials are disclosed. The apparatus includes a sample vessel having an optically transparent wall and an opposing optically reflective wall. Two coherent laser beams, a pump beam and a broadband Stokes beam, are directed through the window and focused on a portion of the sample. In the preferred embodiment, a projectile is fired from a high-pressure gas gun to impact the outside of the reflective wall, generating a planar shock wave which travels through the sample toward the window. The pump and Stokes beams result in the emission from the shock-compressed sample of a coherent anti-Stokes beam, which is emitted toward the approaching reflective wall of the vessel and reflected back through the window. The anti-Stokes beam is folded into a spectrometer for frequency analysis. The results of such analysis are useful for determining chemical and physical phenomena which occur during the shock-compression of the sample.

Mineralogy of ash of some American coals: variations with temperature and source

USGS Publications Warehouse

Mitchell, R.S.; Gluskoter, H.J.

1976-01-01

Ten samples of mineral-matter residue were obtained by the radio-frequency low-temperature ashing of subbituminous and bituminous coals. The low-temperature ash samples were then heated progressively from 400 ??C to 1400 ??C at 100 ??C intervals. Mineral phases present at each temperature interval were determined by X-ray diffraction analyses. The minerals originally present in the coals (quartz, kaolinite, illite, pyrite, calcite, gypsum, dolomite, and sphalerite) were all altered to higher temperature phases. Several of these phases, including kaolinite, metakaolinite, mullite, anhydrite, and anorthite, were found only in limited temperature ranges. Therefore the temperature of formation of the ashes in which they occur may be determined. Mineralogical differences were observed between coal samples from the Rocky Mountain Province, the Illinois Basin, and the Appalachians; and as a result of these mineralogical differences, different high-temperature phases resulted as the samples were heated. However, regional generalizations cannot be made until a greater number of samples have been studied. ?? 1976.

Annual radiological environmental operating report: Browns Ferry Nuclear Plant, 1992. Operations Services/Technical Programs

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

Not Available

1993-04-01

This report describes the environmental radiological monitoring program conducted by TVA in the vicinity of Browns Ferry Nuclear Plant (BFN) in 1992. The program includes the collection of samples from the environment and the determination of the concentrations of radioactive materials in the samples. Samples are taken from stations in the general area of the plant and from areas not influenced by plant operations. Station locations are selected after careful consideration of the weather patterns and projected radiation doses to the various areas around the plant. Material sampled includes air, water, milk, foods, vegetation, soil, fish, sediment, and direct radiationmore » levels. Results from stations near the plant are compared with concentrations from control stations and with preoperational measurements to determine potential impacts of plant operations. Small amounts of Co-60 and Cs-134 were found in sediment samples downstream from the plant. This activity in stream sediment would result in no measurable increase over background in the dose to the general public.« less

Integrated luminometer for the determination of trace metals in seawater using fluorescence, phosphorescence and chemiluminescence detection

PubMed Central

Achterberg, E. P.; Bowie, A. R.; Cannizzaro, V.; Charles, S.; Costa, J. M.; Dubois, F.; Pereiro, R.; San Vicente, B.; Sanz-Medel, A.; Vandeloise, R.; Donckt, E. Vander; Wollast, P.; Yunus, S.

2002-01-01

The paper describes an integrated luminometer able to perform fluorescence (FL), room temperature phosphorescence (RTP) and chemiluminescence (CL) measurements on seawater samples. The technical details of the instrumentation are presented together with flow injection (FI) manifolds for the determination of cadmium and zinc (by FL), lead (RTP) and cobalt (CL). The analytical figures of merit are given for each manifold and results are presented for the determination of the four trace metals in seawater reference materials (NASS-5, SLEW-2) and Scheldt estuarine water samples. PMID:18924742

Determination of the molar mass of argon from high-precision acoustic comparisons

NASA Astrophysics Data System (ADS)

Feng, X. J.; Zhang, J. T.; Moldover, M. R.; Yang, I.; Plimmer, M. D.; Lin, H.

2017-06-01

This article describes the accurate determination of the molar mass M of a sample of argon gas used for the determination of the Boltzmann constant. The method of one of the authors (Moldover et al 1988 J. Res. Natl. Bur. Stand. 93 85-144) uses the ratio of the square speed of sound in the gas under analysis and in a reference sample of known molar mass. A sample of argon that was isotopically-enriched in 40Ar was used as the reference, whose unreactive impurities had been independently measured. The results for three gas samples are in good agreement with determinations by gravimetric mass spectrometry; (  -  1)  =  (-0.31  ±  0.69)  ×  10-6, where the indicated uncertainty is one standard deviation that does not account for the uncertainties from the acoustic and mass-spectroscopy references.

Determination of uranium in tap water by ICP-MS.

PubMed

El Himri, M; Pastor, A; de la Guardia, M

2000-05-01

A fast and accurate procedure has been developed for the determination of uranium at microg L(-1) level in tap and mineral water. The method is based on the direct introduction of samples, without any chemical pre-treatment, into an inductively coupled plasma mass spectrometer (ICP-MS). Uranium was determined at the mass number 238 using Rh as internal standard. The method provides a limit of detection of 2 ng L(-1) and a good repeatability with relative standard deviation values (RSD) about 3% for five independent analyses of samples containing 73 microg L(-1) of uranium. Recovery percentage values found for the determination of uranium in spiked natural samples varied between 91% and 106%. Results obtained are comparable with those found by radiochemical methods for natural samples and of the same order for the certified content of a reference material, thus indicating the accuracy of the ICP-MS procedure without the need of using isotope dilution. A series of mineral and tap waters from different parts of Spain and Morocco were analysed.

Determination of Inorganic Ion Profiles of Illicit Drugs by Capillary Electrophoresis.

PubMed

Evans, Elizabeth; Costrino, Carolina; do Lago, Claudimir L; Garcia, Carlos D; Roux, Claude; Blanes, Lucas

2016-11-01

A portable capillary electrophoresis instrument with dual capacitively coupled contactless conductivity detection (C 4 D) was used to determine the inorganic ionic profiles of three pharmaceutical samples and precursors of two illicit drugs (contemporary samples of methylone and para-methoxymethamphetamine). The LODs ranged from 0.10 μmol/L to 1.25 μmol/L for the 10 selected cations, and from 0.13 μmol/L to 1.03 μmol/L for the eight selected anions. All separations were performed in less than 6 min with migration times and peak area RSD values ranging from 2 to 7%. The results demonstrate the potential of the analysis of inorganic ionic species to aid in the identification and/or differentiation of unknown tablets, and real samples found in illicit drug manufacture scenarios. From the resulting ionic fingerprint, the unknown tablets and samples can be further classified. © 2016 American Academy of Forensic Sciences.

Determination of sulphite in wine by coulometric titration.

PubMed

Lowinsohn, D; Bertotti, M

2001-09-01

A method for the determination of both free and bound S(IV) in white wine samples by coulometric titration with electrogenerated iodine is described, the S(IV) speciation being performed by extracting SO2 from samples acidified wiith hydrochloric acid. Titrations of samples treated with NaOH led to the total S(IV) concentration, the results being in agreement with the ones obtained by the distillation procedure as well as by using the classical Monier-Williams method. An average recovery of 97% was obtained for samples spiked with S(IV) in the range 0.4-1.2 mM, which demonstrated the validity of the proposed procedure. The repeatability was 1.3% and the limit of detection was estimated as 0.01 mM. Results from direct titrations of wine added to the electrochemical cell are reported, which give indications of the stability of adducts towards the reaction with iodine.

Problems of comparing blood glucose molality and molarity determined with an Omni, an EML 105 and an Ebio analyser.

PubMed

Haeckel, Rainer; Hänecke, Petra

2003-07-01

The comparability between glucose concentrations measured in various sample systems is still a matter of debate. Decision limits are usually determined in venous plasma and then converted to either blood or to the aqueous compartment (activity). The conversion factors recommended have not yet been generally accepted. In the present study, glucose concentrations were determined in blood and plasma with an Ebio analyser (molarity) and in the aqueous compartment with both an EML 105 and an Omni (molality). All analytical results were referred to the same aqueous standard solution. The Ebio results agreed with reference method values in control materials. Concentrations determined in the various sample systems from patients (molarity) correlated well with the molality values measured either with the EML or the Omni. However, the mean values of the EML were not consistent with those derived theoretically by considering the different water content. With the Omni, only molality values in whole blood appeared plausible, but not in plasma, although the two sample systems should provide identical molality values. The EML results were almost identical in whole blood and plasma. Theoretically, glucose molality would be the ideal diagnostic quantity. However, no diagnostic advantage of molality determined in whole blood with the Omni vs. molarity values could be detected in a group of 40 non-diabetic and 27 diabetic subjects.

Determination of Silicon in Hydrazine

NASA Technical Reports Server (NTRS)

McClure, Mark B.; Mast, Dion; Greene, Ben; Maes, Miguel J.

2006-01-01

Inductively coupled plasma-mass spectrometry (ICP-MS) is a highly sensitive technique sometimes used for the trace determination of silicon at a mass-to-charge (m/z) ratio of 28, the most abundant natural isotope of silicon. Unfortunately, ICP-MS is unable to differentiate between other sources of m/z 28 and false positive results for silicon will result when other sources of m/z 28 are present. Nitrogen was a major source of m/z 28 and contributes to the m/z 28 signal when hydrazine sample or nitric acid preservative is introduced into the plasma. Accordingly, this work was performed to develop a sample preparation step coupled with an ICP-MS analysis that minimized non-silicon sources of m/z 28. In the preparatory step of this method, the hydrazine sample was first decomposed predominately to nitrogen gas and water with copper-catalyzed hydrogen peroxide. In the analysis step, ICP-MS was used without nitric acid preservative in samples or standards. Glass, a potential source of silicon contamination, was also avoided where possible. The method was sensitive, accurate, and reliable for the determination of silicon in monopropellant grade hydrazine (MPH) in AF-E-332 elastomer leaching tests. Results for silicon in MPH were comparable to those reported in the literature for other studies.

Personal Breathing Zone Exposures among Hot-Mix Asphalt Paving Workers; Preliminary Analysis for Trends and Analysis of Work Practices That Resulted in the Highest Exposure Concentrations

PubMed Central

Osborn, Linda V.; Snawder, John E.; Kriech, Anthony J.; Cavallari, Jennifer M.; McClean, Michael D.; Herrick, Robert F.; Blackburn, Gary R.; Olsen, Larry D.

2015-01-01

An exposure assessment of hot-mix asphalt (HMA) paving workers was conducted to determine which of four exposure scenarios impacted worker exposure and dose. Goals of this report are to present the personal-breathing zone (PBZ) data, discuss the impact of substituting the releasing/cleaning agent, and discuss work practices that resulted in the highest exposure concentration for each analyte. One-hundred-seven PBZ samples were collected from HMA paving workers on days when diesel oil was used as a releasing/cleaning agent. An additional 36 PBZ samples were collected on days when B-100 (100% biodiesel, containing no petroleum-derived products) was used as a substitute releasing/cleaning agent. Twenty-four PBZ samples were collected from a reference group of concrete workers, who also worked in outdoor construction but had no exposure to asphalt emissions. Background and field blank samples were also collected daily. Total particulates and the benzene soluble fraction were determined gravimetrically. Total organic matter was determined using gas chromatography (GC) with flame ionization detection and provided qualitative information about other exposure sources contributing to worker exposure besides asphalt emissions. Thirty-three individual polycyclic aromatic compounds (PACs) were determined using GC with time-offlight mass spectrometry; results were presented as either the concentration of an individual PAC or a summation of the individual PACs containing either 2- to 3-rings or 4- to 6-rings. Samples were also screened for PACs containing 4- to 6-rings using fluorescence spectroscopy. Arithmetic means, medians, and box plots of the PBZ data were used to evaluate trends in the data. Box plots illustrating the diesel oil results were more variable than the B-100. Also, the highest diesel oil results were much higher in concentration than the highest B-100 results. An analysis of the highest exposure results and field notes revealed a probable association between these exposures and the use of diesel oil, use of a diesel-powered screed, elevated HMA paving application temperatures, lubricating and working on broken-down equipment, and operation of a broom machine. PMID:24195533

Personal breathing zone exposures among hot-mix asphalt paving workers; preliminary analysis for trends and analysis of work practices that resulted in the highest exposure concentrations.

PubMed

Osborn, Linda V; Snawder, John E; Kriech, Anthony J; Cavallari, Jennifer M; McClean, Michael D; Herrick, Robert F; Blackburn, Gary R; Olsen, Larry D

2013-01-01

An exposure assessment of hot-mix asphalt (HMA) paving workers was conducted to determine which of four exposure scenarios impacted worker exposure and dose. Goals of this report are to present the personal-breathing zone (PBZ) data, discuss the impact of substituting the releasing/cleaning agent, and discuss work practices that resulted in the highest exposure concentration for each analyte. One-hundred-seven PBZ samples were collected from HMA paving workers on days when diesel oil was used as a releasing/cleaning agent. An additional 36 PBZ samples were collected on days when B-100 (100% biodiesel, containing no petroleum-derived products) was used as a substitute releasing/cleaning agent. Twenty-four PBZ samples were collected from a reference group of concrete workers, who also worked in outdoor construction but had no exposure to asphalt emissions. Background and field blank samples were also collected daily. Total particulates and the benzene soluble fraction were determined gravimetrically. Total organic matter was determined using gas chromatography (GC) with flame ionization detection and provided qualitative information about other exposure sources contributing to worker exposure besides asphalt emissions. Thirty-three individual polycyclic aromatic compounds (PACs) were determined using GC with time-of-flight mass spectrometry; results were presented as either the concentration of an individual PAC or a summation of the individual PACs containing either 2- to 3-rings or 4- to 6-rings. Samples were also screened for PACs containing 4- to 6-rings using fluorescence spectroscopy. Arithmetic means, medians, and box plots of the PBZ data were used to evaluate trends in the data. Box plots illustrating the diesel oil results were more variable than the B-100. Also, the highest diesel oil results were much higher in concentration than the highest B-100 results. An analysis of the highest exposure results and field notes revealed a probable association between these exposures and the use of diesel oil, use of a diesel-powered screed, elevated HMA paving application temperatures, lubricating and working on broken-down equipment, and operation of a broom machine.

[Determination of podophyllotoxin and total lignans in Sinopodophyllum emodi].

PubMed

Huang, Kun; Jiang, Wei; Zhao, Jifeng; Wang, Changhua; Liu, Xiang; Zhang, Zhiwei; Qin, Songyun; Zhong, Guoyue

2012-05-01

To determine the content of podophyllotoxin and total lignans in Sinopodophyllum emodi Ying from different areas and evaluate the resource utilization of this endangered medicinal plant. HPLC and UV spectrophotometry were used to determine the content of podophyllotoxin and total lignans in 126 samples from different habitats and the total lignans content was determined by the reference wavelength method. According to the results, the highest content was determined from the samples from Yongdeng Nature Reserve in Gansu province, and the lowest ones was found in the samples from Tibet. The former's podophyllotoxin and total lignans contents were 7.40% and 20.66%, respectively, which were 19 times and 4 times more than those of the latter. The content of podophyllotoxin and total lignans in S. emodi were significantly positively related, meanwhile, samples from both low altitude and high latitude showed the higher content. The two determination methods are simple, rapid, accurate and repeatable. It is more scientific and rational to evaluate the resource utilization of S. emodi with two indicators, those are the content of podophyllotoxin and the content of total lignans. This paper is instructive to the collection of wild resources and the establishment of production bases.

A method for the determination of vanadium and iron oxidation states in naturally occurring oxides and silicates

USGS Publications Warehouse

Wanty, R.B.; Goldhaber, M.B.

1985-01-01

A valence-specific analytical method for determining V3+ in ore minerals has been developed that involves two steps: dissolution of a mineral sample without disturbing the V3+/Vtot ratio, followed by determination of V3+ in the presence of V4+. The samples are dissolved in a mixture of hydrofluoric and sulphuric acids at 100?? in Teflon-lined reaction vessels. Tervalent vanadium is then determined colorimetrically by formation of a V3+-thiocyanate complex in aqueous-acetone medium. Fe3+ is measured semi-quantitatively in the same solution. The method has been tested with two naturally occurring samples containing vanadium and iron. The results obtained were supported by those obtained by other methods, including electron spin resonance spectroscopy, thermogravimetric analysis, and Mo??ssbauer spectroscopy. ?? 1985.

The late Neandertal supraorbital fossils from Vindija Cave, Croatia: a biased sample?

PubMed

Ahern, James C M; Lee, Sang-Hee; Hawks, John D

2002-09-01

The late Neandertal sample from Vindija (Croatia) has been described as transitional between the earlier Central European Neandertals from Krapina (Croatia) and modern humans. However, the morphological differences indicating this transition may rather be the result of different sex and/or age compositions between the samples. This study tests the hypothesis that the metric differences between the Krapina and Vindija supraorbital samples are due to sampling bias. We focus upon the supraorbital region because past studies have posited this region as particularly indicative of the Vindija sample's transitional nature. Furthermore, the supraorbital region varies significantly with both age and sex. We analyzed four chords and two derived indices of supraorbital torus form as defined by Smith & Ranyard (1980, Am. J. phys. Anthrop.93, pp. 589-610). For each variable, we analyzed relative sample bias of the Krapina and Vindija samples using three sampling methods. In order to test the hypothesis that the Vindija sample contains an over-representation of females and/or young while the Krapina sample is normal or also female/young biased, we determined the probability of drawing a sample of the same size as and with a mean equal to or less than Vindija's from a Krapina-based population. In order to test the hypothesis that the Vindija sample is female/young biased while the Krapina sample is male/old biased, we determined the probability of drawing a sample of the same size as and with a mean equal or less than Vindija's from a generated population whose mean is halfway between Krapina's and Vindija's. Finally, in order to test the hypothesis that the Vindija sample is normal while the Krapina sample contains an over-representation of males and/or old, we determined the probability of drawing a sample of the same size as and with a mean equal to or greater than Krapina's from a Vindija-based population. Unless we assume that the Vindija sample is female/young and the Krapina sample is male/old biased, our results falsify the hypothesis that the metric differences between the Krapina and Vindija samples are due to sample bias.

TECHNOLOGIES FORM MONITORING AND ...

EPA Pesticide Factsheets

A demonstration of technologies for determining the presence of dioxin and dioxin-like compounds in soil and sediment was conducted under EPA's Superfund Innovative Technology Evaluation Program in Saginaw, Michigan in April 2004. This report describes the evaluation of Wako Pure Chemical Industries's Dioxin ELISA Kit. The kit is an immunoassay technique that reports toxicity equivalents (TEQ) of dioxin/furans. The sample units are in pg/g 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) equivalents (EQ). The technology results were compared to high resolution mass spectrometry (HRMS) TEQ results generated using EPA Method 1613B.The Wako results were biased both positively and negatively relative to HRMS results. The technologys estimated method detection limit was 83-201 pg/g 2,3,7,8-TCDD EQ, but this should be considered a rough estimate. Results from this demonstration suggest that the Wako kit could be an effective screening tool for determining sample results above and below 20 pg/g TEQ, and even more effective as a screen for samples above and below 50 pg/g TEQ, particularly considering the cost to analyze the 209 demonstration samples was significantly less than that of the reference laboratory ($150,294 vs. $213,580), and all samples were analyzed on-site in 9 days (in comparison to the reference laboratory which took 8 months). The objective of this program is to promote the acceptance and use of innovative field technologies by providing well-documented per

Comparison of individual, pooled, and composite fecal sampling methods for detection of Salmonella on U.S. dairy operations

USDA-ARS?s Scientific Manuscript database

The objectives of this study were to estimate the prevalence of Salmonella for individual, pooled, and composite fecal samples and to compare culture results from each sample type for determining herd Salmonella infection status and identifying Salmonella serotype(s). The USDA’s National Animal Hea...

Estimating removal rates of bacteria from poultry carcasses using two whole-carcass rinse volumes

USDA-ARS?s Scientific Manuscript database

Rinse sampling is a common method for determining the level of microbial contamination on poultry carcasses. One of the advantages of rinse sampling, over other carcass sampling methods, is that the results can be used for both process control applications and to estimate the total microbial level o...

Application of Advanced Nondestructive Evaluation Techniques for Cylindrical Composite Test Samples

NASA Technical Reports Server (NTRS)

Martin, Richard E.; Roth, Donald J.; Salem, Jonathan A.

2013-01-01

Two nondestructive methods were applied to composite cylinder samples pressurized to failure in order to determine manufacturing quality and monitor damage progression under load. A unique computed tomography (CT) image processing methodology developed at NASA Glenn Research was used to assess the condition of the as-received samples while acoustic emission (AE) monitoring was used to identify both the extent and location of damage within the samples up to failure. Results show the effectiveness of both of these methods in identifying potentially critical fabrication issues and their resulting impact on performance.

Language Sampling for Preschoolers With Severe Speech Impairments

PubMed Central

Ragsdale, Jamie; Bustos, Aimee

2016-01-01

Purpose The purposes of this investigation were to determine if measures such as mean length of utterance (MLU) and percentage of comprehensible words can be derived reliably from language samples of children with severe speech impairments and if such measures correlate with tools that measure constructs assumed to be related. Method Language samples of 15 preschoolers with severe speech impairments (but receptive language within normal limits) were transcribed independently by 2 transcribers. Nonparametric statistics were used to determine which measures, if any, could be transcribed reliably and to determine if correlations existed between language sample measures and standardized measures of speech, language, and cognition. Results Reliable measures were extracted from the majority of the language samples, including MLU in words, mean number of syllables per utterance, and percentage of comprehensible words. Language sample comprehensibility measures were correlated with a single word comprehensibility task. Also, language sample MLUs and mean length of the participants' 3 longest sentences from the MacArthur–Bates Communicative Development Inventory (Fenson et al., 2006) were correlated. Conclusion Language sampling, given certain modifications, may be used for some 3-to 5-year-old children with normal receptive language who have severe speech impairments to provide reliable expressive language and comprehensibility information. PMID:27552110

Slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of Cr, Cd and Pb in plastics.

PubMed

Li, Po-Chien; Jiang, Shiuh-Jen

2006-07-01

Ultrasonic slurry sampling electrothermal vaporization dynamic reaction cell inductively coupled plasma mass spectrometry (USS-ETV-DRC-ICP-MS) for the determination of Cr, Cd and Pb in several plastic samples, using NH4NO3 as the modifier, is described. The influences of the instrumental operating conditions and the slurry preparation technique on the ion signals are investigated. A reduction in the intensity of the background at signals corresponding to chromium masses (arising from matrix elements) was achieved by using NH3 as the reaction cell gas in the DRC. The method was applied to determine Cr, Cd and Pb in two polystyrene (PS) samples and a polyvinyl chloride (PVC) sample using two different calibration methods, namely standard addition and isotope dilution. The results were in good agreement with those for digested samples analyzed by ultrasonic nebulization DRC-ICP-MS. The precision between sample replicates was better than 17% with the USS-ETV-DRC-ICP-MS method. The method detection limits, estimated from standard addition curves, were about 6-9, 1-2 and 8-11 ng g(-1) for Cr, Cd and Pb, respectively, in the original plastic samples.

Evaluation of the Architect HIV Ag/Ab Combo Assay in a low-prevalence setting: The role of samples with a low S/CO ratio.

PubMed

Alonso, Roberto; Pérez-García, Felipe; Gijón, Paloma; Collazos, Ana; Bouza, Emilio

2018-06-01

The Architect HIV Ag/Ab Combo Assay, a fourth-generation ELISA, has proven to be highly reliable for the diagnosis of HIV infection. However, its high sensitivity may lead to false-positive results. To evaluate the diagnostic performance of Architect in a low-prevalence population and to assess the role of the sample-to-cutoff ratio (S/CO) in reducing the frequency of false-positive results. We conducted a retrospective study of samples analyzed by Architect between January 2015 and June 2017. Positive samples were confirmed by immunoblot (RIBA) or nucleic acid amplification tests (NAATs). Different S/CO thresholds (1, 2.5, 10, 25, and 100) were analyzed to determine sensitivity, specificity, and negative and positive predictive values (NPV, PPV). ROC analysis was used to determine the optimal S/CO. A total of 69,471 samples were analyzed. 709 (1.02%) were positive by Architect. Of these, 63 (8.89%) were false-positive results. Most of them (93.65%) were in samples with S/CO < 100. However, most confirmations by NAATs (12 out of 19 cases) were also recorded for these samples. The optimal S/CO was 2.5, which provided the highest area under the ROC curve (0.9998) and no false-negative results. With this S/CO, sensitivity and specificity were 100.0%, and PPV and NPV were 95.8% and 100.0%, respectively. In addition, the frequency of false-positive results decreased significantly to 4.15%. Although Architect generates a relatively high number of false-positive results, raising the S/CO limit too much to increase specificity can lead to false-negative results, especially in newly infected individuals. Copyright © 2018 Elsevier B.V. All rights reserved.

A Study to Determine if a Difference Exists Among the Cumulative Incidence of Acute Respiratory Disease Hospital Admissions of Three Groups of Army Basic Trainees as Defined by the Design of Barracks in Which They Are Housed

DTIC Science & Technology

1989-08-01

number) Using chi-square tests of homogeneity, a selected sample of Army Basic Trainees at Ft. Jackso was studied to determine if there was a...Period of training for sample soldiers was January to May 1985. Results of testing for the female trainees indicated no significant difference in incidence...of ARD among three barracks groups. Results of testing for male trainees indicated statistically significant dif -erences of ARD among each of three

Validation of the Explorer® 2.0 test coupled to e-Reader® for the screening of antimicrobials in muscle from different animal species.

PubMed

Mata, Luis; Sanz, David; Razquin, Pedro

2014-01-01

The Explorer(®) 2.0 tube test is a microbial inhibition test for the screening of antimicrobial residues in food samples. The new e-Reader(®) device coupled to Explorer(®) 2.0 operates by incubation at a selected temperature, determination of the endpoint of the assay and interpretation to generate results. This system was validated for muscle samples according to the European Commission Decision 2002/657/EC. Sensitivity towards 25 substances from several groups of antimicrobials was investigated in a first step. Detection capabilities for six substances representing the six major antimicrobial groups were also determined in bovine muscle. The detection capabilities for amoxicillin (10 µg l(-1)), cefalexin (200 µg l(-1)), doxycyclin (100 µg l(-1)), sulfamethazine (100 µg l(-1)), tylosin (100 µg l(-1)) and neomycin (200 µg l(-1)) were in all cases at or below the maximum residue limit (MRL). Specificity and applicability of the test were demonstrated with muscle samples from four animal species (bovine, porcine, ovine and poultry) and results were found to be satisfactory. Ruggedness was evaluated on negative and spiked samples with sulfamethazine as a representative antimicrobial. Neither false-positives nor false-negatives were detected when varying the sample volume, the time of pre-incubation, the temperature of incubation and the batch of the test. These results prove that Explorer(®) 2.0 coupled to e-Reader(®) is a valuable tool for the screening of a broad range of antimicrobials in muscle. This new methodology simplifies the analysis and increases the accuracy of interpretation of the test results since the endpoint of the assay is automatically determined and results are interpreted objectively.

Sample Results From Tank 48H Samples HTF-48-14-158, -159, -169, and -170

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

Peters, T.; Hang, T.

2015-04-28

Savannah River National Laboratory (SRNL) analyzed samples from Tank 48H in support of determining the cause for the unusually high dose rates at the sampling points for this tank. A set of two samples was taken from the quiescent tank, and two additional samples were taken after the contents of the tank were mixed. The results of the analyses of all the samples show that the contents of the tank have changed very little since the analysis of the previous sample in 2012. The solids are almost exclusively composed of tetraphenylborate (TPB) salts, and there is no indication of accelerationmore » in the TPB decomposition. The filtrate composition shows a moderate increase in salt concentration and density, which is attributable to the addition of NaOH for the purposes of corrosion control. An older modeling simulation of the TPB degradation was updated, and the supernate results from a 2012 sample were run in the model. This result was compared to the results from the 2014 recent sample results reported in this document. The model indicates there is no change in the TPB degradation from 2012 to 2014. SRNL measured the buoyancy of the TPB solids in Tank 48H simulant solutions. It was determined that a solution of density 1.279 g/mL (~6.5M sodium) was capable of indefinitely suspending the TPB solids evenly throughout the solution. A solution of density 1.296 g/mL (~7M sodium) caused a significant fraction of the solids to float on the solution surface. As the experiments could not include the effect of additional buoyancy elements such as benzene or hydrogen generation, the buoyancy measurements provide an upper bound estimate of the density in Tank 48H required to float the solids.« less

From picture to porosity of river bed material using Structure-from-Motion with Multi-View-Stereo

NASA Astrophysics Data System (ADS)

Seitz, Lydia; Haas, Christian; Noack, Markus; Wieprecht, Silke

2018-04-01

Common methods for in-situ determination of porosity of river bed material are time- and effort-consuming. Although mathematical predictors can be used for estimation, they do not adequately represent porosities. The objective of this study was to assess a new approach for the determination of porosity of frozen sediment samples. The method is based on volume determination by applying Structure-from-Motion with Multi View Stereo (SfM-MVS) to estimate a 3D volumetric model based on overlapping imagery. The method was applied on artificial sediment mixtures as well as field samples. In addition, the commonly used water replacement method was applied to determine porosities in comparison with the SfM-MVS method. We examined a range of porosities from 0.16 to 0.46 that are representative of the wide range of porosities found in rivers. SfM-MVS performed well in determining volumes of the sediment samples. A very good correlation (r = 0.998, p < 0.0001) was observed between the SfM-MVS and the water replacement method. Results further show that the water replacement method underestimated total sample volumes. A comparison with several mathematical predictors showed that for non-uniform samples the calculated porosity based on the standard deviation performed better than porosities based on the median grain size. None of the predictors were effective at estimating the porosity of the field samples.

An empirical comparison of isolate-based and sample-based definitions of antimicrobial resistance and their effect on estimates of prevalence.

PubMed

Humphry, R W; Evans, J; Webster, C; Tongue, S C; Innocent, G T; Gunn, G J

2018-02-01

Antimicrobial resistance is primarily a problem in human medicine but there are unquantified links of transmission in both directions between animal and human populations. Quantitative assessment of the costs and benefits of reduced antimicrobial usage in livestock requires robust quantification of transmission of resistance between animals, the environment and the human population. This in turn requires appropriate measurement of resistance. To tackle this we selected two different methods for determining whether a sample is resistant - one based on screening a sample, the other on testing individual isolates. Our overall objective was to explore the differences arising from choice of measurement. A literature search demonstrated the widespread use of testing of individual isolates. The first aim of this study was to compare, quantitatively, sample level and isolate level screening. Cattle or sheep faecal samples (n=41) submitted for routine parasitology were tested for antimicrobial resistance in two ways: (1) "streak" direct culture onto plates containing the antimicrobial of interest; (2) determination of minimum inhibitory concentration (MIC) of 8-10 isolates per sample compared to published MIC thresholds. Two antibiotics (ampicillin and nalidixic acid) were tested. With ampicillin, direct culture resulted in more than double the number of resistant samples than the MIC method based on eight individual isolates. The second aim of this study was to demonstrate the utility of the observed relationship between these two measures of antimicrobial resistance to re-estimate the prevalence of antimicrobial resistance from a previous study, in which we had used "streak" cultures. Boot-strap methods were used to estimate the proportion of samples that would have tested resistant in the historic study, had we used the isolate-based MIC method instead. Our boot-strap results indicate that our estimates of prevalence of antimicrobial resistance would have been considerably lower in the historic study had the MIC method been used. Finally we conclude that there is no single way of defining a sample as resistant to an antimicrobial agent. The method used greatly affects the estimated prevalence of antimicrobial resistance in a sampled population of animals, thus potentially resulting in misleading results. Comparing methods on the same samples allows us to re-estimate the prevalence from other studies, had other methods for determining resistance been used. The results of this study highlight the importance of establishing what the most appropriate measure of antimicrobial resistance is, for the proposed purpose of the results. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparison of preprocessing methods and storage times for touch DNA samples

PubMed Central

Dong, Hui; Wang, Jing; Zhang, Tao; Ge, Jian-ye; Dong, Ying-qiang; Sun, Qi-fan; Liu, Chao; Li, Cai-xia

2017-01-01

Aim To select appropriate preprocessing methods for different substrates by comparing the effects of four different preprocessing methods on touch DNA samples and to determine the effect of various storage times on the results of touch DNA sample analysis. Method Hand touch DNA samples were used to investigate the detection and inspection results of DNA on different substrates. Four preprocessing methods, including the direct cutting method, stubbing procedure, double swab technique, and vacuum cleaner method, were used in this study. DNA was extracted from mock samples with four different preprocessing methods. The best preprocess protocol determined from the study was further used to compare performance after various storage times. DNA extracted from all samples was quantified and amplified using standard procedures. Results The amounts of DNA and the number of alleles detected on the porous substrates were greater than those on the non-porous substrates. The performances of the four preprocessing methods varied with different substrates. The direct cutting method displayed advantages for porous substrates, and the vacuum cleaner method was advantageous for non-porous substrates. No significant degradation trend was observed as the storage times increased. Conclusion Different substrates require the use of different preprocessing method in order to obtain the highest DNA amount and allele number from touch DNA samples. This study provides a theoretical basis for explorations of touch DNA samples and may be used as a reference when dealing with touch DNA samples in case work. PMID:28252870

The Impact of Soil Sampling Errors on Variable Rate Fertilization

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

R. L. Hoskinson; R C. Rope; L G. Blackwood

2004-07-01

Variable rate fertilization of an agricultural field is done taking into account spatial variability in the soil’s characteristics. Most often, spatial variability in the soil’s fertility is the primary characteristic used to determine the differences in fertilizers applied from one point to the next. For several years the Idaho National Engineering and Environmental Laboratory (INEEL) has been developing a Decision Support System for Agriculture (DSS4Ag) to determine the economically optimum recipe of various fertilizers to apply at each site in a field, based on existing soil fertility at the site, predicted yield of the crop that would result (and amore » predicted harvest-time market price), and the current costs and compositions of the fertilizers to be applied. Typically, soil is sampled at selected points within a field, the soil samples are analyzed in a lab, and the lab-measured soil fertility of the point samples is used for spatial interpolation, in some statistical manner, to determine the soil fertility at all other points in the field. Then a decision tool determines the fertilizers to apply at each point. Our research was conducted to measure the impact on the variable rate fertilization recipe caused by variability in the measurement of the soil’s fertility at the sampling points. The variability could be laboratory analytical errors or errors from variation in the sample collection method. The results show that for many of the fertility parameters, laboratory measurement error variance exceeds the estimated variability of the fertility measure across grid locations. These errors resulted in DSS4Ag fertilizer recipe recommended application rates that differed by up to 138 pounds of urea per acre, with half the field differing by more than 57 pounds of urea per acre. For potash the difference in application rate was up to 895 pounds per acre and over half the field differed by more than 242 pounds of potash per acre. Urea and potash differences accounted for almost 87% of the cost difference. The sum of these differences could result in a $34 per acre cost difference for the fertilization. Because of these differences, better analysis or better sampling methods may need to be done, or more samples collected, to ensure that the soil measurements are truly representative of the field’s spatial variability.« less

Potentiometric detection in UPLC as an easy alternative to determine cocaine in biological samples.

PubMed

Daems, Devin; van Nuijs, Alexander L N; Covaci, Adrian; Hamidi-Asl, Ezat; Van Camp, Guy; Nagels, Luc J

2015-07-01

The analytical methods which are often used for the determination of cocaine in complex biological matrices are a prescreening immunoassay and confirmation by chromatography combined with mass spectrometry. We suggest an ultra-high-pressure liquid chromatography combined with a potentiometric detector, as a fast and practical method to detect and quantify cocaine in biological samples. An adsorption/desorption model was used to investigate the usefulness of the potentiometric detector to determine cocaine in complex matrices. Detection limits of 6.3 ng mL(-1) were obtained in plasma and urine, which is below the maximum residue limit (MRL) of 25 ng mL(-1). A set of seven plasma samples and 10 urine samples were classified identically by both methods as exceeding the MRL or being inferior to it. The results obtained with the UPLC/potentiometric detection method were compared with the results obtained with the UPLC/MS method for samples spiked with varying cocaine concentrations. The intraclass correlation coefficient was 0.997 for serum (n =7) and 0.977 for urine (n =8). As liquid chromatography is an established technique, and as potentiometry is very simple and cost-effective in terms of equipment, we believe that this method is potentially easy, inexpensive, fast and reliable. Copyright © 2014 John Wiley & Sons, Ltd.

External quality-assurance results for the National Atmospheric Deposition Program/National Trends Network, 1997-99

USGS Publications Warehouse

Gordon, John D.; Latysh, Natalie E.; Lindholm, Sandy J.

2003-01-01

Five external quality-assurance programs were operated by the U.S. Geological Survey for the National Atmospheric Deposition Program/ National Trends Network (NADP/NTN) during 1997 through 1999: the intersite-comparison program, the blind-audit program, the field- audit program, the interlaboratory-comparison program, and the collocated-sampler program. The intersite-comparison program assesses the accuracy of pH and specific-conductance determinations made by NADP/NTN site operators. In two 1997 intersite-comparison studies, 83.7 and 85.8 percent of the pH determinations met the NADP/NTN accuracy goals, whereas 97.3 and 92.4 percent of the specific-conductance determinations met the NADP/NTN accuracy goals. The percentage of pH and specific-conductance determinations that met the accuracy goals in 1998 were, for the most part, higher than in 1997. In two 1998 studies, 90.9 and 90.3 percent of the pH determinations met the accuracy goals compared to 94.7 and 96.0 percent of the specific- conductance measurements meeting the accuracy goals. In one 1999 intersite-comparison study, 89.5 percent and 99.4 percent of pH and specific- conductance determinations, respectively, met the NADP/NTN accuracy goals. The blind-audit program evaluates the effects of routine sample handling, processing, and shipping on the analytical bias and precision of weekly precipitation samples. A portion of the blind-audit sample subject to the normal onsite handling and processing of a weekly precipitation sample is referred to as the bucket portion, whereas the portion receiving only minimal handling is referred to as the bottle portion. Positive bias in regard to blind-audit results indicates that the bucket portion has a higher concentration than the bottle portion. The paired t-test for the 1997 through 1999 blind- audit data indicates that routine sample handling, processing, and shipping introduced a positive bias (a=0.05) for calcium and chloride and a negative bias (cz=0.05) for hydrogen ion. During 1997 through 1999, the median paired differences between the bucket and bottle portions ranged from 0.00 milligram per liter for nitrate and ammonium to +0.010 milligram per liter for both chloride and sulfate. The median paired difference between the bucket and bottle portions for hydrogen ion was -1.086 microequivalents per liter, whereas for specific conductance, the median paired difference between the bucket and bottle portions was -0.200 microsiemen per centimeter during 1997 through 1999. Surface-chemistry effects due to variable amounts of precipitation contacting prewashed sample-collection and shipping-container surfaces were studied in the blind-audit program by using three different sample volumes. The sample- collection and shipping containers used for the blind-audit study were obtained from the site operator's supply and could have been used for precipitation samples. Results of a Kruskal-Wallis analysis of variance test of the relation between paired blind-audit sample differences in units of concentration and sample volume were statistically significant for magnesium, chloride, sulfate, and hydrogen ion during 1997 through 1999. Before 1994, at least 5 of the 10 analytes displayed a statistically significant difference between paired blind-audit differences in units of concentration and sample volume, supporting the premise that chemical reactions between the 13-liter bucket shipping container (primarily the butadiene o-ring lid of the shipping container) and the sample, which resulted in an increasing loss of hydrogen ion with increasing volume, have been eliminated by the new l-liter bottle sample- shipping protocol. The field-audit program measures the effects of field exposure, handling, and processing on the chemistry of NADP/NTN precipitation samples. In the field-audit program, the site operator is instructed to process and submit a quality- control sample following a standard 7-day, Tuesday-to-Tuesday sampling period with no

Characterization of Volatiles Loss from Soil Samples at Lunar Environments

NASA Technical Reports Server (NTRS)

Kleinhenz, Julie; Smith, Jim; Roush, Ted; Colaprete, Anthony; Zacny, Kris; Paulsen, Gale; Wang, Alex; Paz, Aaron

2017-01-01

Resource Prospector Integrated Thermal Vacuum Test Program A series of ground based dirty thermal vacuum tests are being conducted to better understand the subsurface sampling operations for RP Volatiles loss during sampling operations Hardware performance Sample removal and transfer Concept of operationsInstrumentation5 test campaigns over 5 years have been conducted with RP hardware with advancing hardware designs and additional RP subsystems Volatiles sampling 4 years Using flight-forward regolith sampling hardware, empirically determine volatile retention at lunar-relevant conditions Use data to improve theoretical predictions Determine driving variables for retention Bound water loss potential to define measurement uncertainties. The main goal of this talk is to introduce you to our approach to characterizing volatiles loss for RP. Introduce the facility and its capabilities Overview of the RP hardware used in integrated testing (most recent iteration) Summarize the test variables used thus farReview a sample of the results.

A new device for dynamic sampling of radon in air

NASA Astrophysics Data System (ADS)

Lozano, J. C.; Escobar, V. Gómez; Tomé, F. Vera

2000-08-01

A new system is proposed for the active sampling of radon in air, based on the well-known property of activated charcoal to retain radon. Two identical carbon-activated cartridges arranged in series remove the radon from the air being sampled. The air passes first through a desiccant cell and then the carbon cartridges for short sampling times using a low-flow pump. The alpha activity for each cartridge is determined by a liquid scintillation counting system. The cartridge is placed in a holder into a vial that also contains the appropriate amount of scintillation cocktail, in a way that avoids direct contact between cocktail and charcoal. Once dynamic equilibrium between the phases has been reached, the vials can be counted. Optimum sampling conditions concerning flow rates and sampling times are determined. Using those conditions, the method was applied to environmental samples, straightforwardly providing good results for very different levels of activity.

Selective Laser Melting of Metal Powder Of Steel 3161

NASA Astrophysics Data System (ADS)

Smelov, V. G.; Sotov, A. V.; Agapovichev, A. V.; Tomilina, T. M.

2016-08-01

In this article the results of experimental study of the structure and mechanical properties of materials obtained by selective laser melting (SLM), metal powder steel 316L was carried out. Before the process of cultivation of samples as the input control, the morphology of the surface of the powder particles was studied and particle size analysis was carried out. Also, 3D X-ray quality control of the grown samples was carried out in order to detect hidden defects, their qualitative and quantitative assessment. To determine the strength characteristics of the samples synthesized by the SLM method, static tensile tests were conducted. To determine the stress X-ray diffraction analysis was carried out in the material samples.

Determination of thorium by fluorescent x-ray spectrometry

USGS Publications Warehouse

Adler, I.; Axelrod, J.M.

1955-01-01

A fluorescent x-ray spectrographic method for the determination of thoria in rock samples uses thallium as an internal standard. Measurements are made with a two-channel spectrometer equipped with quartz (d = 1.817 A.) analyzing crystals. Particle-size effects are minimized by grinding the sample components with a mixture of silicon carbide and aluminum and then briquetting. Analyses of 17 samples showed that for the 16 samples containing over 0.7% thoria the average error, based on chemical results, is 4.7% and the maximum error, 9.5%. Because of limitations of instrumentation, 0.2% thoria is considered the lower limit of detection. An analysis can be made in about an hour.

Combined radiochemical procedure for determination of plutonium, americium and strontium-90 in the soil samples from SNTS

NASA Astrophysics Data System (ADS)

Kazachevskii, I. V.; Lukashenko, S. N.; Chumikov, G. N.; Chakrova, E. T.; Smirin, L. N.; Solodukhin, V. P.; Khayekber, S.; Berdinova, N. M.; Ryazanova, L. A.; Bannyh, V. I.; Muratova, V. M.

1999-01-01

The results of combined radiochemical procedure for the determination of plutonium, americium and90Sr (via measurement of90Y) in the soil samples from SNTS are presented. The processes of co-precipitation of these nuclides with calcium fluoride in the strong acid solutions have been investigated. The conditions for simultaneous separation of americium and yttrium using extraction chromatography have been studied. It follows from analyses of real soil samples that the procedure developed provides the chemical recovery of plutonium and yttrium in the range of 50-95% and 60-95%, respectively. The execution of the procedure requires 3.5 working days including a sample decomposition study.

Monitoring Environmental Recovery at Terminated Produced Water Discharge Sites in Coastal Louisiana Waters

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

Continental Shelf Associates, Inc.

1999-08-16

This report presents the results of a study of terminated produced water discharge sites in the coastal waters of Louisiana. Environmental recovery at the sites is documented by comparing pre-termination and post-termination (six months and one year) data. Produced water, sediments, and sediment interstitial water samples were analyzed for radionuclides, metals, and hydrocarbons. Benthic infauna were identified from samples collected in the vicinity of the discharge and reference sites. Radium isotope activities were determined in fish and crustacean samples. In addition, an environmental risk assessment is made on the basis of the concentrations of metals and hydrocarbons determined in themore » samples.« less

Determination of total mercury in fillets of sport fishes collected from Folsom Reservoir, California, 2006

USGS Publications Warehouse

May, Thomas W.; Brumbaugh, William G.

2007-01-01

This report presents the results of a study by the U.S. Geological Survey, done in cooperation with the U.S. Bureau of Reclamation, to determine mercury concentrations in selected sport fishes from Folsom Reservoir in California. Fillets were collected from each fish sample, and after homogenization and lyophilization of fish fillets, mercury concentrations were determined with a direct mercury analyzer utilizing the process of thermal combustion-gold amalgamation atomic absorption spectroscopy. Mercury concentrations in fillets ranged from 0.031 to 0.20 micrograms per gram wet weight in rainbow trout (Oncorhynchus mykiss) samples and 0.071 to 0.16 micrograms per gram wet weight in bluegill (Lepomis macrochirus) samples. Mercury concentration was 0.98 microgram per gram wet weight in a single spotted bass (Micropterus punctulatus) sample, which was the only one in the sample set which exceeded the U.S. Environmental Protection Agency's fish consumption advisory of 0.30 microgram per gram wet weight.

High-throughput analysis of lipid hydroperoxides in edible oils and fats using the fluorescent reagent diphenyl-1-pyrenylphosphine.

PubMed

Santas, Jonathan; Guzmán, Yeimmy J; Guardiola, Francesc; Rafecas, Magdalena; Bou, Ricard

2014-11-01

A fluorometric method for the determination of hydroperoxides (HP) in edible oils and fats using the reagent diphenyl-1-pyrenylphosphine (DPPP) was developed and validated. Two solvent media containing 100% butanol or a mixture of chloroform/methanol (2:1, v/v) can be used to solubilise lipid samples. Regardless of the solvent used to solubilise the sample, the DPPP method was precise, accurate, sensitive and easy to perform. The HP content of 43 oil and fat samples was determined and the results were compared with those obtained by means of the AOCS Official Method for the determination of peroxide value (PV) and the ferrous oxidation-xylenol orange (FOX) method. The proposed method not only correlates well with the PV and FOX methods, but also presents some advantages such as requiring low sample and solvent amounts and being suitable for high-throughput sample analysis. Copyright © 2014 Elsevier Ltd. All rights reserved.

Atomic-absorption spectrometric determination of cobalt, nickel, and copper in geological materials with matrix masking and chelation-extraction

USGS Publications Warehouse

Sanzolone, R.F.; Chao, T.T.; Crenshaw, G.L.

1979-01-01

An atomic-absorption spectrometric method is reported for the determination of cobalt, nickel, and copper in a variety of geological materials including iron- and manganese-rich, and calcareous samples. The sample is decomposed with HP-HNO3 and the residue is dissolved in hydrochloric acid. Ammonium fluoride is added to mask iron and 'aluminum. After adjustment to pH 6, cobalt, nickel, and copper are chelated with sodium diethyl-dithiocarbamate and extracted into methyl isobutyl ketone. The sample is set aside for 24 h before analysis to remove interferences from manganese. For a 0.200-g sample, the limits of determination are 5-1000 ppm for Co, Ni, and Cu. As much as 50% Fe, 25% Mn or Ca, 20% Al and 10% Na, K, or Mg in the sample either individually or in various combinations do not interfere. Results obtained on five U.S. Geological Survey rock standards are in general agreement with values reported in the literature. ?? 1979.

Determination of pesticides and toxic potency of rainwater samples in western Greece.

PubMed

Rouvalis, Angela; Karadima, Constantina; Zioris, Ioannis V; Sakkas, Vasilios A; Albanis, Triantafyllos; Iliopoulou-Georgudaki, Joan

2009-03-01

Rainwater samples from four municipalities located in Achaia Prefecture, Greece, were collected from March to September 2006. The toxic potency of pollutants present in 36 rainwater samples was tested using Daphnia pulex. The pesticide determination was conducted with GC-MS. Only phosphamidon was detected, which appeared in 52% and 13% of the rural and urban areas, respectively. The toxicity of rainwater was determined in 52% and 46.7% of the rural and urban area samples, respectively. Chemical analyses showed that in rural areas, the PO(4)(3-) ions had higher concentrations than in urban areas. On the other hand, the SO(4)(2-), NO(-)(3), and NO(-)(2) anions are more highly concentrated in urban areas. Correlation analysis proved that the toxicity of the rainwater samples is moderate, affected by the presence of the insecticide only in the rural areas. The results indicated that toxicity can be directly assessed via bioassays, even when unknown pollutants are present.

Developmental Validation of Short Tandem Repeat Reagent Kit for Forensic DNA Profiling of Canine Biological Materials

PubMed Central

Dayton, Melody; Koskinen, Mikko T; Tom, Bradley K; Mattila, Anna-Maria; Johnston, Eric; Halverson, Joy; Fantin, Dennis; DeNise, Sue; Budowle, Bruce; Smith, David Glenn; Kanthaswamy, Sree

2009-01-01

Aim To develop a reagent kit that enables multiplex polymerase chain reaction (PCR) amplification of 18 short tandem repeats (STR) and the canine sex-determining Zinc Finger marker. Methods Validation studies to determine the robustness and reliability in forensic DNA typing of this multiplex assay included sensitivity testing, reproducibility studies, intra- and inter-locus color balance studies, annealing temperature and cycle number studies, peak height ratio determination, characterization of artifacts such as stutter percentages and dye blobs, mixture analyses, species-specificity, case type samples analyses and population studies. Results The kit robustly amplified domesticated dog samples and consistently generated full 19-locus profiles from as little as 125 pg of dog DNA. In addition, wolf DNA samples could be analyzed with the kit. Conclusion The kit, which produces robust, reliable, and reproducible results, will be made available for the forensic research community after modifications based on this study’s evaluation to comply with the quality standards expected for forensic casework. PMID:19480022

Electroanalysis and laccase-based biosensor on the determination of phenolic content and antioxidant power of honey samples.

PubMed

de Oliveira Neto, Jerônimo Raimundo; Rezende, Stefani Garcia; Lobón, Gérman Sanz; Garcia, Telma Alves; Macedo, Isaac Yves Lopes; Garcia, Luane Ferreira; Alves, Virgínia Farias; Torres, Ieda Maria Sapateiro; Santiago, Mariângela Fontes; Schmidt, Fernando; de Souza Gil, Eric

2017-12-15

Honey is a functional food widely consumed. Thus, the evaluation of honey samples to determine its phenolic content and antioxidant capacity (AOC) is relevant to determine its quality. Usually AOC is performed by spectrophotometric methods, which lacks reproducibility and practicality. In this context, the electroanalytical methods offer higher simplicity and accuracy. Hence, the aim of this work was to use of electroanalytical tools and laccase based biosensor on the evaluation of AOC and total phenol content (TPC) of honey samples from different countries. The antioxidant power established by electrochemical index presented good correlation with the spectrophotometric FRAP (Ferric Reducing Ability of Plasma) and DPPH (2,2-Diphenyl-1-Picrylhydrazyl) radical scavenging assays. Also, TPC results obtained by the biosensor agreed with the Folin-Ciocalteu (FC) assay. In addition to the semi quantitative results, the electroanalysis offered qualitative parameters, which were useful to indicate the nature of major phenolic compounds. Copyright © 2017 Elsevier Ltd. All rights reserved.

Rapid RHD Zygosity Determination Using Digital PCR.

PubMed

Sillence, Kelly A; Halawani, Amr J; Tounsi, Wajnat A; Clarke, Kirsty A; Kiernan, Michele; Madgett, Tracey E; Avent, Neil D

2017-08-01

Paternal zygosity testing is used for determining homo- or hemizygosity of RHD in pregnancies that are at a risk of hemolytic disease of the fetus and newborn. At present, this is achieved by using real-time PCR or the Rhesus box PCR, which can be difficult to interpret and unreliable, particularly for black African populations. DNA samples extracted from 53 blood donors were analyzed using 2 multiplex reactions for RHD -specific targets against a reference ( AGO1 ) 2 to determine gene dosage by digital PCR. Results were compared with serological data, and the correct genotype for 2 discordant results was determined by long-range PCR (LR-PCR), next-generation sequencing, and conventional Sanger sequencing. The results showed clear and reliable determination of RHD zygosity using digital PCR and revealed that 4 samples did not match the serologically predicted genotype. Sanger sequencing and long-range PCR followed by next-generation sequencing revealed that the correct genotypes for samples 729M and 351D, which were serologically typed as R 1 R 2 (DCe/DcE), were R 2 r' (DcE/dCe) for 729M and R 1 r″ (DCe/dcE), R 0 r y (Dce/dCE), or R Z r (DCE/dce) for 351D, in concordance with the digital PCR data. Digital PCR provides a highly accurate method to rapidly define blood group zygosity and has clinical application in the analysis of Rh phenotyped or genotyped samples. The vast majority of current blood group genotyping platforms are not designed to define zygosity, and thus, this technique may be used to define paternal RH zygosity in pregnancies that are at a risk of hemolytic disease of the fetus and newborn and can distinguish between homo- and hemizygous RHD -positive individuals. © 2017 American Association for Clinical Chemistry.

The MISSE 7 Flexural Stress Effects Experiment After 1.5 Years of Wake Space Exposure

NASA Technical Reports Server (NTRS)

Snow, Kate E.; De Groh, Kim K.; Banks, Bruce A.

2017-01-01

Low Earth orbit space environment conditions, including ultraviolet radiation, thermal cycling, and atomic oxygen exposure, can cause degradation of exterior spacecraft materials over time. Radiation and thermal exposure often results in bond- breaking and embrittlement of polymers, reducing mechanical strength and structural integrity. An experiment called the Flexural Stress Effects Experiment (FSEE) was flown with the objective of determining the role of space environmental exposure on the degradation of polymers under flexural stress. The FSEE samples were flown in the wake orientation on the exterior of International Space Station for 1.5 years. Twenty-four samples were flown: 12 bent over a 0.375 in. mandrel and 12 were over a 0.25 in. mandrel. This was designed to simulate flight configurations of insulation blankets on spacecraft. The samples consisted of assorted polyimide and fluorinated polymers with various coatings. Half the samples were designated for bend testing and the other half will be tensile tested. A non-standard bend-test procedure was designed to determine the surface strain at which embrittled polymers crack. All ten samples designated for bend testing have been tested. None of the control samples' polymers cracked, even under surface strains up to 19.7%, although one coating cracked. Of the ten flight samples tested, seven show increased embrittlement through bend-test induced cracking at surface strains from 0.70%to 11.73%. These results show that most of the tested polymers are embrittled due to space exposure, when compared to their control samples. Determination of the extent of space induced embrittlement of polymers is important for designing durable spacecraft.

A geochemical sampling technique for use in areas of active alpine glaciation: an application from the central Alaska Range

USGS Publications Warehouse

Stephens, G.C.; Evenson, E.B.; Detra, D.E.

1990-01-01

In mountainous regions containing extensive glacier systems there is a lack of suitable material for conventional geochemical sampling. As a result, in most geochemical sampling programs a few stream-sediment samples collected at, or near, the terminus of valley glaciers are used to evaluate the mineral potential of the glaciated area. We have developed and tested a technique which utilizes the medial moraines of valley glaciers for systematic geochemical exploration of the glacial catchment area. Moraine sampling provides geochemical information that is site-specific in that geochemical anomalies can be traced directly up-ice to bedrock sources. Traverses were made across the Trident and Susitna glaciers in the central Alaska Range where fine-grained (clay to sand size) samples were collected from each medial moraine. These samples were prepared and chemically analyzed to determine the concentration of specific elements. Fifty pebbles were collected at each moraine for archival purposes and for subsequent lithologic identification. Additionally, fifty cobbles and fifty boulders were examined and described at each sample site to determine the nature and abundance of lithologies present in the catchment area, the extent and nature of visible mineralization, the presence and intensity of hydrothermal alteration and the existence of veins, dikes and other minor structural features. Results from the central Alaska Range have delineated four distinct multi-element anomalies which are a response to potential mineralization up-ice from the medial moraine traverse. By integrating the lithologic, mineralogical and geochemical data the probable geological setting of the geochemical anomalies is determined. ?? 1990.

Characterization of nonstarch polysaccharides content from different edible organs of some vegetables, determined by GC and HPLC: comparative study.

PubMed

Villanueva-Suárez, M J; Redondo-Cuenca, A; Rodríguez-Sevilla, M D; de las Heras Martínez, M

2003-09-24

Content and composition of dietary fiber as nonstarch polysaccharides (NSP) was determined in vegetables belonging to different types of edible organs, using GC and HPLC. Samples analyzed were subterranean organs (radish and leek), leaves (celery, swiss chard, and lettuce), stalks (celery, swiss chard, and asparagus), inflorescence (broccoli), and fruits (tomato, green pepper, and marrow). The results indicate that though the monomeric profile is similar in all these samples quantitative differences were found for neutral sugars and uronic acids among samples of the same type of vegetal organ. The NSP values determined using CG method were in good agreement with HPLC method (R(2) = 0.9005). However, arabinose, mannose, and galactose plus rhamnose are more influenced by the analytical method used than the rest of the monomers in nearly all the samples analyzed. Final values of NSP depend on the method used in celery stalks, broccoli, and green pepper.

Antimicrobial agent-free hybrid cationic starch/sodium alginate polyelectrolyte films for food packaging materials.

PubMed

Şen, Ferhat; Uzunsoy, İrem; Baştürk, Emre; Kahraman, Memet Vezir

2017-08-15

This study aimed to develop polyelectrolyte structured antimicrobial food packaging materials that do not contain any antimicrobial agents. Cationic starch was synthesized and characterized by FT-IR spectroscopy and 1 H NMR spectroscopy. Its nitrogen content was determined by Kjeldahl method. Polyelectrolyte structured antimicrobial food packaging materials were prepared using starch, cationic starch and sodium alginate. Antimicrobial activity of materials was defined by inhibition zone method (disc diffusion method). Thermal stability of samples was evaluated by TGA and DSC. Hydrophobicity of samples was determined by contact angle measurements. Surface morphology of samples was investigated by SEM. Moreover, gel contents of samples were determined. The obtained results prove that produced food packaging materials have good thermal, antimicrobial and surface properties, and they can be used as food packaging material in many industries. Copyright © 2017 Elsevier Ltd. All rights reserved.

Analysis of bromate in drinking water using liquid chromatography-tandem mass spectrometry without sample pretreatment.

PubMed

Kosaka, Koji; Asami, Mari; Takei, Kanako; Akiba, Michihiro

2011-01-01

An analytical method for determining bromate in drinking water was developed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The (18)O-enriched bromate was used as an internal standard. The limit of quantification (LOQ) of bromate was 0.2 µg/L. The peak of bromate was separated from those of coexisting ions (i.e., chloride, nitrate and sulfate). The relative and absolute recoveries of bromate in two drinking water samples and in a synthesized ion solution (100 mg/L chloride, 10 mg N/L nitrate, and 100 mg/L sulfate) were 99-105 and 94-105%, respectively. Bromate concentrations in 11 drinking water samples determined by LC-MS/MS were <0.2-2.3 µg/L. The results of the present study indicated that the proposed method was suitable for determining bromate concentrations in drinking water without sample pretreatment.

Determination of ash in coals unusually high in calcite and pyrite

USGS Publications Warehouse

Rees, O.W.; Selvig, W.A.

1942-01-01

The preliminary hearth heating method (A and E) gave results within the A. S. T. M. tolerances for all duplicates obtained in the same laboratory. Checks between different laboratories within A. S. T. M. tolerances were obtained for coals containing up to about 3.6 per cent mineral carbon dioxide, but these ashes contained larger amounts of retained sulfur. The determination of ash by the cold furnace method (B and F) gave duplicate results within A. S. T. M. tolerances for all samples in the U. S. Bureau of Mines laboratory and for samples up to about 1.6 per cent mineral carbon dioxide content in the Illinois Geological Survey laboratory. Checks between average values from the two laboratories were within A. S. T. M. tolerances for all samples.

The diagnostic significance of lactate dehydrogenase isoenzymes in urinary cytology.

PubMed Central

Nishikawa, A.; Tanaka, T.; Takeuchi, T.; Fujihiro, S.; Mori, H.

1991-01-01

Lactate dehydrogenase (LDH) isoenzyme distribution was examined in 106 urine samples being tested cytologically for evidence of bladder cancer; the samples were selected to have less than 20 leucocytes and erythrocytes per high power field and the LDH pattern determined by electrophoresis. The Papanicolaou stained-smears showed 68 negative, 17 suspicious and 21 positive. The LDH M-fraction of the urinary supernatant in cytologically positive cases was significantly greater than in negative cases, although the latter included a few false negative samples. Some of the false negatives gave positive results for the LDH M-fraction; these results suggest that the determination of LDH isoenzymes in the urine is useful in diagnosing urinary tract cancers, including early stage, and for follow-up of patients with bladder cancers after surgical resection. PMID:2039708

Plasma creatinine in dogs: intra- and inter-laboratory variation in 10 European veterinary laboratories

PubMed Central

2011-01-01

Background There is substantial variation in reported reference intervals for canine plasma creatinine among veterinary laboratories, thereby influencing the clinical assessment of analytical results. The aims of the study was to determine the inter- and intra-laboratory variation in plasma creatinine among 10 veterinary laboratories, and to compare results from each laboratory with the upper limit of its reference interval. Methods Samples were collected from 10 healthy dogs, 10 dogs with expected intermediate plasma creatinine concentrations, and 10 dogs with azotemia. Overlap was observed for the first two groups. The 30 samples were divided into 3 batches and shipped in random order by postal delivery for plasma creatinine determination. Statistical testing was performed in accordance with ISO standard methodology. Results Inter- and intra-laboratory variation was clinically acceptable as plasma creatinine values for most samples were usually of the same magnitude. A few extreme outliers caused three laboratories to fail statistical testing for consistency. Laboratory sample means above or below the overall sample mean, did not unequivocally reflect high or low reference intervals in that laboratory. Conclusions In spite of close analytical results, further standardization among laboratories is warranted. The discrepant reference intervals seem to largely reflect different populations used in establishing the reference intervals, rather than analytical variation due to different laboratory methods. PMID:21477356

Determination of maximal amount of minor gases adsorbed in a shale sample by headspace gas chromatography.

PubMed

Zhang, Chun-Yun; Hu, Hui-Chao; Chai, Xin-Sheng; Pan, Lei; Xiao, Xian-Ming

2014-02-07

In this paper, we present a novel method for determining the maximal amount of ethane, a minor gas species, adsorbed in a shale sample. The method is based on the time-dependent release of ethane from shale samples measured by headspace gas chromatography (HS-GC). The study includes a mathematical model for fitting the experimental data, calculating the maximal amount gas adsorbed, and predicting results at other temperatures. The method is a more efficient alternative to the isothermal adsorption method that is in widespread use today. Copyright © 2013 Elsevier B.V. All rights reserved.

Determination of naturally occurring radionuclides in soil samples of Ayranci, Turkey

NASA Astrophysics Data System (ADS)

Agar, Osman; Eke, Canel; Boztosun, Ismail; Emin Korkmaz, M.

2015-04-01

The specific activity, radiation hazard index and the annual effective dose of the naturally occurring radioactive elements (238U, 232Th and 40K) were determined in soil samples collected from 12 different locations in Ayranci region by using a NaI(Tl) gamma-ray spectrometer. The measured activity concentrations of the natural radionuclides in studied soil samples were compared with the corresponding results of different countries and the internationally reported values. From the analysis, it is found that these materials may be safely used as construction materials and do not pose significant radiation hazards.

Characterization and application of a diamine oxidase from Lathyrus sativus as component of an electrochemical biosensor for the determination of biogenic amines in wine and beer.

PubMed

Di Fusco, Massimo; Federico, Rodolfo; Boffi, Alberto; Macone, Alberto; Favero, Gabriele; Mazzei, Franco

2011-08-01

In this work, we have characterized a diamine oxidase (DAO) from Lathyrus sativus and evaluated its use, for the first time, as biocatalytic component of an electrochemical biosensor for the determination of biogenic amines index in wine and beer samples. Firstly, DAO was electrokinetically characterized free in solution by means of a platinum electrode and then immobilized by using polyazetidine prepolimer on the surface of screen-printed electrodes constituted of two gold working electrodes. The amperometric measurements were carried out by using a flow system at a fixed potential of +600 mV vs the internal silver pseudo reference in phosphate buffer solution (0.1 mol l(-1), pH = 7.4). The analysis of wine and beer samples were performed in flow injection system using the dual channel transducer providing simultaneous detection of sample and blank signal, and the resulting signal (after subtraction of the blank signal) was referred to that of putrescine. The results were compared with those obtained using a modified reference method based on gas chromatography-mass spectrometry analysis on the same samples. The results obtained in the analysis of Italian wines shows the better suitability of DAO-based biosensor in the determination of the biogenic amines (BAs) index expressed as putrescine equivalent in both red and white wines, being less efficient in beer samples where it underestimates by about 50% the BAs content.

Determination of plutonium and its isotopic ratio in marine sediment samples using quadrupole ICP-MS with the shield torch system under normal plasma conditions.

PubMed

Zheng, Jian; Yamada, Masatoshi; Wang, Zhongliang; Aono, Tatsuo; Kusakabe, Masashi

2004-06-01

An analytical method for determining (239)Pu and (240)Pu in marine sediment samples, which uses quadrupole ICP-MS, was developed in this work. A simple anion-exchange chromatography system was employed for the separation and purification of Pu from the sample matrix. A sufficient decontamination factor of 1.4 x 10(4) for U, which interferes with the determination of (239)Pu, was achieved. High sensitivity Pu determination was obtained, which led to an extremely low concentration detection limit of approximately 8 fg/ml (0.019 mBq/ml for (239)Pu; 0.071 mBq/ml for (240)Pu) in a sample solution, or an absolute detection limit of 42 fg in a 5 ml sample solution, by using the shield torch technique. Analytical results for the determination of the (239+240)Pu and the (240)Pu/(239)Pu ratio in IAEA 368 (ocean sediment) reference material indicated that the accuracy of the method was satisfactory. The method developed was successfully applied to a study of Pu behavior in the sediments from Sagami Bay, Japan. The observed high (240)Pu/(239)Pu ratio in the sediment core indicated that there was additional Pu input derived from close-in fallout in addition to the global fallout.

An integrated bioanalytical method development and validation approach: case studies.

PubMed

Xue, Y-J; Melo, Brian; Vallejo, Martha; Zhao, Yuwen; Tang, Lina; Chen, Yuan-Shek; Keller, Karin M

2012-10-01

We proposed an integrated bioanalytical method development and validation approach: (1) method screening based on analyte's physicochemical properties and metabolism information to determine the most appropriate extraction/analysis conditions; (2) preliminary stability evaluation using both quality control and incurred samples to establish sample collection, storage and processing conditions; (3) mock validation to examine method accuracy and precision and incurred sample reproducibility; and (4) method validation to confirm the results obtained during method development. This integrated approach was applied to the determination of compound I in rat plasma and compound II in rat and dog plasma. The effectiveness of the approach was demonstrated by the superior quality of three method validations: (1) a zero run failure rate; (2) >93% of quality control results within 10% of nominal values; and (3) 99% incurred sample within 9.2% of the original values. In addition, rat and dog plasma methods for compound II were successfully applied to analyze more than 900 plasma samples obtained from Investigational New Drug (IND) toxicology studies in rats and dogs with near perfect results: (1) a zero run failure rate; (2) excellent accuracy and precision for standards and quality controls; and (3) 98% incurred samples within 15% of the original values. Copyright © 2011 John Wiley & Sons, Ltd.

Rapid determination of 226Ra in environmental samples

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

Maxwell, Sherrod L.; Culligan, Brian K.

A new rapid method for the determination of {sup 228}Ra in natural water samples has been developed at the SRNL/EBL (Savannah River National Lab/ Environmental Bioassay Laboratory) that can be used for emergency response or routine samples. While gamma spectrometry can be employed with sufficient detection limits to determine {sup 228}Ra in solid samples (via {sup 228}Ac) , radiochemical methods that employ gas flow proportional counting techniques typically provide lower MDA (Minimal Detectable Activity) levels for the determination of {sup 228}Ra in water samples. Most radiochemical methods for {sup 228}Ra collect and purify {sup 228}Ra and allow for {sup 228}Acmore » daughter ingrowth for ~36 hours. In this new SRNL/EBL approach, {sup 228}Ac is collected and purified from the water sample without waiting to eliminate this delay. The sample preparation requires only about 4 hours so that {sup 228}Ra assay results on water samples can be achieved in < 6 hours. The method uses a rapid calcium carbonate precipitation enhanced with a small amount of phosphate added to enhance chemical yields (typically >90%), followed by rapid cation exchange removal of calcium. Lead, bismuth, uranium, thorium and protactinium isotopes are also removed by the cation exchange separation. {sup 228}Ac is eluted from the cation resin directly onto a DGA Resin cartridge attached to the bottom of the cation column to purify {sup 228}Ac. DGA Resin also removes lead and bismuth isotopes, along with Sr isotopes and {sup 90}Y. La is used to determine {sup 228}Ac chemical yield via ICP-MS, but {sup 133}Ba can also be used instead if ICP-MS assay is not available. Unlike some older methods, no lead or strontium holdback carriers or continual readjustment of sample pH is required.« less

Microwave-assisted extraction and mild saponification for determination of organochlorine pesticides in oyster samples.

PubMed

Carro, N; García, I; Ignacio, M-C; Llompart, M; Yebra, M-C; Mouteira, A

2002-10-01

A sample-preparation procedure (extraction and saponification) using microwave energy is proposed for determination of organochlorine pesticides in oyster samples. A Plackett-Burman factorial design has been used to optimize the microwave-assisted extraction and mild saponification on a freeze dried sample spiked with a mixture of aldrin, endrin, dieldrin, heptachlor, heptachorepoxide, isodrin, transnonachlor, p, p'-DDE, and p, p'-DDD. Six variables: solvent volume, extraction time, extraction temperature, amount of acetone (%) in the extractant solvent, amount of sample, and volume of NaOH solution were considered in the optimization process. The results show that the amount of sample is statistically significant for dieldrin, aldrin, p, p'-DDE, heptachlor, and transnonachlor and solvent volume for dieldrin, aldrin, and p, p'-DDE. The volume of NaOH solution is statistically significant for aldrin and p, p'-DDE only. Extraction temperature and extraction time seem to be the main factors determining the efficiency of extraction process for isodrin and p, p'-DDE, respectively. The optimized procedure was compared with conventional Soxhlet extraction.

Biomarker discovery study design for type 1 diabetes in The Environmental Determinants of Diabetes in the Young (TEDDY) study.

PubMed

Lee, Hye-Seung; Burkhardt, Brant R; McLeod, Wendy; Smith, Susan; Eberhard, Chris; Lynch, Kristian; Hadley, David; Rewers, Marian; Simell, Olli; She, Jin-Xiong; Hagopian, Bill; Lernmark, Ake; Akolkar, Beena; Ziegler, Anette G; Krischer, Jeffrey P

2014-07-01

The Environmental Determinants of Diabetes in the Young planned biomarker discovery studies on longitudinal samples for persistent confirmed islet cell autoantibodies and type 1 diabetes using dietary biomarkers, metabolomics, microbiome/viral metagenomics and gene expression. This article describes the details of planning The Environmental Determinants of Diabetes in the Young biomarker discovery studies using a nested case-control design that was chosen as an alternative to the full cohort analysis. In the frame of a nested case-control design, it guides the choice of matching factors, selection of controls, preparation of external quality control samples and reduction of batch effects along with proper sample allocation. Our design is to reduce potential bias and retain study power while reducing the costs by limiting the numbers of samples requiring laboratory analyses. It also covers two primary end points (the occurrence of diabetes-related autoantibodies and the diagnosis of type 1 diabetes). The resulting list of case-control matched samples for each laboratory was augmented with external quality control samples. Copyright © 2013 John Wiley & Sons, Ltd.

Novel calibration for LA-ICP-MS-based fission-track thermochronology

NASA Astrophysics Data System (ADS)

Soares, C. J.; Guedes, S.; Hadler, J. C.; Mertz-Kraus, R.; Zack, T.; Iunes, P. J.

2014-01-01

We present a novel age-equation calibration for fission-track age determinations by laser ablation inductively coupled plasma mass spectrometry. This new calibration incorporates the efficiency factor of an internal surface, [ ηq]is, which is obtained by measuring the projected fission-track length, allowing the determination of FT ages directly using the recommended spontaneous fission decay constant. Also, the uranium concentrations in apatite samples are determined using a Durango (Dur-2, 7.44 μg/g U) crystal and a Mud Tank (MT-7, 6.88 μg/g U) crystal as uranium reference materials. The use of matrix-matched reference materials allows a reduction in the uncertainty of the uranium measurements to those related to counting statistics, which are ca. 1 % taking into account that no extra source of uncertainty has to be considered. The equations as well as the matrix-matched reference materials are evaluated using well-dated samples from Durango, Fish Canyon Tuff, and Limberg as unknown samples. The results compare well with their respective published ages determined through other dating methods. Additionally, the results agree with traditional fission-track ages using both the zeta approach and the absolute approach, suggesting that the calibration presented in this work can be robustly applied in geological context. Furthermore, considering that fission-track ages can be determined without an age standard sample, the fission-track thermochronology approach presented here is assumed to be a valuable dating tool.

Evaluation of mechanical properties of Aluminum-Copper cold sprayed and alloy 625 wire arc sprayed coatings

NASA Astrophysics Data System (ADS)

Bashirzadeh, Milad

This study examines microstructural-based mechanical properties of Al-Cu composite deposited by cold spraying and wire arc sprayed nickel-based alloy 625 coating using numerical modeling and experimental techniques. The microhardness and elastic modulus of samples were determined using the Knoop hardness technique. Hardness in both transverse and longitudinal directions on the sample cross-sections has been measured. An image-based finite element simulation algorithm was employed to determine the mechanical properties through an inverse analysis. In addition mechanical tests including, tensile, bending, and nano-indentation tests were performed on alloy 625 wire arc sprayed samples. Overall, results from the experimental tests are in relatively good agreement for deposited Al-Cu composites and alloy 625 coating. However, results obtained from numerical simulation are significantly higher in value than experimentally obtained results. Examination and comparison of the results are strong indications of the influence of microstructure characteristics on the mechanical properties of thermally spray deposited coatings.

Spectral multivariate calibration without laboratory prepared or determined reference analyte values.

PubMed

Ottaway, Josh; Farrell, Jeremy A; Kalivas, John H

2013-02-05

An essential part to calibration is establishing the analyte calibration reference samples. These samples must characterize the sample matrix and measurement conditions (chemical, physical, instrumental, and environmental) of any sample to be predicted. Calibration usually requires measuring spectra for numerous reference samples in addition to determining the corresponding analyte reference values. Both tasks are typically time-consuming and costly. This paper reports on a method named pure component Tikhonov regularization (PCTR) that does not require laboratory prepared or determined reference values. Instead, an analyte pure component spectrum is used in conjunction with nonanalyte spectra for calibration. Nonanalyte spectra can be from different sources including pure component interference samples, blanks, and constant analyte samples. The approach is also applicable to calibration maintenance when the analyte pure component spectrum is measured in one set of conditions and nonanalyte spectra are measured in new conditions. The PCTR method balances the trade-offs between calibration model shrinkage and the degree of orthogonality to the nonanalyte content (model direction) in order to obtain accurate predictions. Using visible and near-infrared (NIR) spectral data sets, the PCTR results are comparable to those obtained using ridge regression (RR) with reference calibration sets. The flexibility of PCTR also allows including reference samples if such samples are available.

Analytical results for 544 water samples collected in the Attean Quartz Monzonite in the vicinity of Jackman, Maine

USGS Publications Warehouse

Ficklin, W.H.; Nowlan, G.A.; Preston, D.J.

1983-01-01

Water samples were collected in the vicinity of Jackman, Maine as a part of the study of the relationship of dissolved constituents in water to the sediments subjacent to the water. Each sample was analyzed for specific conductance, alkalinity, acidity, pH, fluoride, chloride, sulfate, phosphate, nitrate, sodium, potassium, calcium, magnesium, and silica. Trace elements determined were copper, zinc, molybdenum, lead, iron, manganese, arsenic, cobalt, nickel, and strontium. The longitude and latitude of each sample location and a sample site map are included in the report as well as a table of the analytical results.

Dried venous blood samples for the detection and quantification of measles IgG using a commercial enzyme immunoassay.

PubMed Central

Riddell, Michaela A.; Byrnes, Graham B.; Leydon, Jennie A.; Kelly, Heath A.

2003-01-01

OBJECTIVES: To determine whether samples of dried venous blood (DVB) were an acceptable alternative to serum for detecting measles-specific IgG in a commercial enzyme immunoassay. METHODS: Paired samples of serum and DVB were collected from 98 suspected cases of measles and 1153 schoolchildren in Victoria, Australia. All samples were tested using the Dade Behring Enzygnost Anti-Measles-Virus/IgG immunoassay. DVB samples were eluted using either the sample buffer provided with the kit or 5% dry milk powder in phosphate-buffered saline-Tween 20. FINDINGS: DVB samples eluted by sample buffer showed significantly better linear correlation to the serum samples than did DVB samples eluted in 5% dry milk in phosphate-buffered saline-Tween 20. To improve the comparability of serum and DVB samples an adjustment factor of 1.28 was applied to the optical density (OD) values of DVB. This adjustment also enabled quantification of the titre of measles IgG in mIU/ml directly from the OD value using the alpha calculation as specified by the kit protocol. For DVB samples stored for less than six months at 4 degrees C, the assay showed an overall sensitivity of 98.4% and a specificity of 97.2% compared with the results of serum testing. CONCLUSION: These results illustrate the potential for DVB samples to be widely used with the Dade Behring enzyme immunoassay system for determining the immunity of the individual and the population to the measles virus. PMID:14758429

Sensor-triggered sampling to determine instantaneous airborne vapor exposure concentrations.

PubMed

Smith, Philip A; Simmons, Michael K; Toone, Phillip

2018-06-01

It is difficult to measure transient airborne exposure peaks by means of integrated sampling for organic chemical vapors, even with very short-duration sampling. Selection of an appropriate time to measure an exposure peak through integrated sampling is problematic, and short-duration time-weighted average (TWA) values obtained with integrated sampling are not likely to accurately determine actual peak concentrations attained when concentrations fluctuate rapidly. Laboratory analysis for integrated exposure samples is preferred from a certainty standpoint over results derived in the field from a sensor, as a sensor user typically must overcome specificity issues and a number of potential interfering factors to obtain similarly reliable data. However, sensors are currently needed to measure intra-exposure period concentration variations (i.e., exposure peaks). In this article, the digitized signal from a photoionization detector (PID) sensor triggered collection of whole-air samples when toluene or trichloroethylene vapors attained pre-determined levels in a laboratory atmosphere generation system. Analysis by gas chromatography-mass spectrometry of whole-air samples (with both 37 and 80% relative humidity) collected using the triggering mechanism with rapidly increasing vapor concentrations showed good agreement with the triggering set point values. Whole-air samples (80% relative humidity) in canisters demonstrated acceptable 17-day storage recoveries, and acceptable precision and bias were obtained. The ability to determine exceedance of a ceiling or peak exposure standard by laboratory analysis of an instantaneously collected sample, and to simultaneously provide a calibration point to verify the correct operation of a sensor was demonstrated. This latter detail may increase the confidence in reliability of sensor data obtained across an entire exposure period.

[Study on the determination of 14 inorganic elements in coffee by inductively coupled plasma mass spectrometry].

PubMed

Nie, Xi-Du; Fu, Liang

2013-07-01

Samples of coffee were digested by microwave digestion, and inorganic elements amounts of Na, Mg, P, Ca, Cr, Mn, Fe, Co, Cu, Zn, As, Se, Mo and Pb in sample solutions were determined by inductively coupled plasma mass spectrometry (ICP-MS). HNO3 + H2O2 was used to achieve the complete decomposition of the organic matrix in a closed-vessel microwave oven. The working parameters of the instrument were optimized. The results showed that the relative standard deviation (RSD) was less than 3.84% for all the elements, and the recovery was found to be 92.00% -106.52% by adding standard recovery experiment. This method was simple, sensitive and precise and can perform simultaneous multi-elements determination of coffee, which could satisfy the sample examination request and provide scientific rationale for determining inorganic elements of coffee.

[Backgrounds for assessing occupational exposure to crystalline silica dust in Poland and worldwide].

PubMed

Maciejewska, Aleksandra

2007-01-01

Crystalline silica is an agent harmful to human health, and quite frequently present in occupational environments. Occupational groups exposed to crystalline silica dust include mostly workers of the mineral and coal mining as well as metallurgical, chemical and construction industries. In the European Union (EU), the number of those exposed to this agent is estimated at over 2 million persons. In Poland, the number of people employed under conditions of excessive silica dust exposure exceeds 50 thousand. The assessment of occupational exposure to crystalline silica comprises several steps: primarily workplace determinations, quantitative sample analyses and comparisons of the obtained results with admissible values. This work describes a set of instruments that enables direct comparison of the study results with admissible values binding in almost 40 countries. It also highlights the consequences resulting from the classification of quartz and cristobalite, the most common forms of crystalline silica, as carcinogens by the International Agency for Research on Cancer (IARC). A survey of air sampling and dust determination methods used in various countries to measure airborne dust concentrations of crystalline silica in occupational environments are presented along with relevant tables. The GESTIS data base, specifying the methods considered by EU as suitable for measuring and assessing harmful agents, was used as the selection criterion. Particular attention was paid to the methods used to determine crystalline silica; the effect of analytical methods applied, sample preparation procedures, and reference materials on the results of determinations was also analyzed. Main parameters of method validation, such as detection and determination limits, and precision of the analysis were compared.

Oregon ground-water quality and its relation to hydrogeological factors; a statistical approach

USGS Publications Warehouse

Miller, T.L.; Gonthier, J.B.

1984-01-01

An appraisal of Oregon ground-water quality was made using existing data accessible through the U.S. Geological Survey computer system. The data available for about 1,000 sites were separated by aquifer units and hydrologic units. Selected statistical moments were described for 19 constituents including major ions. About 96 percent of all sites in the data base were sampled only once. The sample data were classified by aquifer unit and hydrologic unit and analysis of variance was run to determine if significant differences exist between the units within each of these two classifications for the same 19 constituents on which statistical moments were determined. Results of the analysis of variance indicated both classification variables performed about the same, but aquifer unit did provide more separation for some constituents. Samples from the Rogue River basin were classified by location within the flow system and type of flow system. The samples were then analyzed using analysis of variance on 14 constituents to determine if there were significant differences between subsets classified by flow path. Results of this analysis were not definitive, but classification as to the type of flow system did indicate potential for segregating water-quality data into distinct subsets. (USGS)

Trace elements levels in the serum, urine, and semen of patients with infertility.

PubMed

Sağlam, Hasan Salih; Altundağ, Hüseyin; Atik, Yavuz Tarık; Dündar, Mustafa Şahin; Adsan, Öztug

2015-01-01

Studies suggest that trace elements may have an adverse impact on male reproduction, even at low levels. We tried to investigate the relationships between these metals and semen quality in various body fluids among men with infertility. A total of 255 samples of blood, semen, and urine were collected from 85 men suffering from infertility. Inductively coupled plasma-optical emission spectrometry was used for the determination of 22 trace elements. We compared the results of the semen parameters with the results of the element determinations. Because of the high proportion of samples with values lower than the limit of detection for a number of the elements, only 8 of a total 22 trace elements were determined in the samples. When the concentrations of sperm were classified according to the World Health Organization's guidelines for normospermia, oligospermia, and azoospermia, statistically significant differences were found among Zn, Ca, Al, Cu, Mg, Se, and Sr concentrations in various serum, sperm, and urine samples (P < 0.05). In the present study, we found significant correlations between concentrations of Zn, Ca, Al, Cu, Mg, Se, and Sr and semen parameters in various body fluids.

[Determination of alkylphenol and alkylphenolpolyethoxylates in brine by solid phase extraction and high performance liquid chromatography-mass spectrometry].

PubMed

Wang, Jincheng; Xiong, Li; Zhang, Haijun; Chen, Jiping

2011-12-01

A simple method based on solid phase extraction (SPE) coupled with high performance liquid chromatography-mass spectrometry (HPLC-MS) was developed for the determination of octylphenol (OP), nonylphenol (NP), octylphenol ethoxylates (OPEOs) and nonylphenol ethoxylates (NPEOs) in brine. The extraction and cleanup of brine samples were performed on C18 solid-phase extraction cartridges. The complete separation among OP, NP, OPEOs and NPEOs was achieved on a Hypersil GOLD analytical column with methanol-water as the mobile phase. The determination was achieved using HPLC-MS with electrospray ionization (ESI) in selected ion monitoring mode. The results showed that the average recoveries of target compounds were 59.6% - 104.4% and the corresponding relative standard deviations (RSDs, n = 3) were 1.0% - 13.5%. The instrumental limits of detection for the compounds were 0.08 - 3 microg/L. This method was applied to the analysis of the samples of seawater near Dalian coast. The results showed that both NP and NPEOs were detected in all samples and their concentrations in seaport and oil port were much higher than those in other sampling sites.

Microfluidic Flow Injection Analysis with Thermal Lens Microscopic Detection for Determination of NGAL

NASA Astrophysics Data System (ADS)

Radovanović, Tatjana; Liu, Mingqiang; Likar, Polona; Klemenc, Matjaž; Franko, Mladen

2015-06-01

A combined microfluidic flow injection analysis-thermal lens microscopy (FIA-TLM) system was applied for determination of neutrophil gelatinase-associated lipocalin (NGAL)—a biomarker of acute kidney injury. NGAL was determined following a commercial ELISA assay and transfer of the resulting solution into the FIA-TLM system with a 100 m deep microchannel. At an excitation power of 100 mW, the FIA-TLM provided about seven times lower limits of detection (1.5 pg as compared to a conventional ELISA test, and a sample throughput of six samples per minute, which compares favorably with sample throughput of the microtiter plate reader, which reads 96 wells in about 30 min. Comparison of results for NGAL in plasma samples from healthy individuals and for NGAL dynamics in patients undergoing coronary angiography measured with transmission mode spectrometry on a microtiter plate reader and with FIA-TLM showed good agreement. In addition to improved LOD, the high sensitivity of FIA-TLM offers possibilities of a further reduction of the total reaction time of the NGAL ELISA test by sacrificing some of the sensitivity while reducing the duration of individual incubation steps.

Development of Quantitative PCR Assays Targeting the 16S rRNA Genes of Enterococcus spp. and Their Application to the Identification of Enterococcus Species in Environmental Samples

PubMed Central

Ryu, Hodon; Henson, Michael; Elk, Michael; Toledo-Hernandez, Carlos; Griffith, John; Blackwood, Denene; Noble, Rachel; Gourmelon, Michèle; Glassmeyer, Susan

2013-01-01

The detection of environmental enterococci has been determined primarily by using culture-based techniques that might exclude some enterococcal species as well as those that are nonculturable. To address this, the relative abundances of enterococci were examined by challenging fecal and water samples against a currently available genus-specific assay (Entero1). To determine the diversity of enterococcal species, 16S rRNA gene-based group-specific quantitative PCR (qPCR) assays were developed and evaluated against eight of the most common environmental enterococcal species. Partial 16S rRNA gene sequences of 439 presumptive environmental enterococcal strains were analyzed to study further the diversity of enterococci and to confirm the specificities of group-specific assays. The group-specific qPCR assays showed relatively high amplification rates with targeted species (>98%), although some assays cross-amplified with nontargeted species (1.3 to 6.5%). The results with the group-specific assays also showed that different enterococcal species co-occurred in most fecal samples. The most abundant enterococci in water and fecal samples were Enterococcus faecalis and Enterococcus faecium, although we identified more water isolates as Enterococcus casseliflavus than as any of the other species. The prevalence of the Entero1 marker was in agreement with the combined number of positive signals determined by the group-specific assays in most fecal samples, except in gull feces. On the other hand, the number of group-specific assay signals was lower in all water samples tested, suggesting that other enterococcal species are present in these samples. While the results highlight the value of genus- and group-specific assays for detecting the major enterococcal groups in environmental water samples, additional studies are needed to determine further the diversity, distributions, and relative abundances of all enterococcal species found in water. PMID:23087032

A novel method for sex determination by detecting the number of X chromosomes.

PubMed

Nakanishi, Hiroaki; Shojo, Hideki; Ohmori, Takeshi; Hara, Masaaki; Takada, Aya; Adachi, Noboru; Saito, Kazuyuki

2015-01-01

A novel method for sex determination, based on the detection of the number of X chromosomes, was established. Current methods, based on the detection of the Y chromosome, can directly identify an unknown sample as male, but female gender is determined indirectly, by not detecting the Y chromosome. Thus, a direct determination of female gender is important because the quality (e.g., fragmentation and amelogenin-Y null allele) of the Y chromosome DNA may lead to a false result. Thus, we developed a novel sex determination method by analyzing the number of X chromosomes using a copy number variation (CNV) detection technique (the comparative Ct method). In this study, we designed a primer set using the amelogenin-X gene without the CNV region as the target to determine the X chromosome copy number, to exclude the influence of the CNV region from the comparative Ct value. The number of X chromosomes was determined statistically using the CopyCaller software with real-time PCR. All DNA samples from participants (20 males, 20 females) were evaluated correctly using this method with 1-ng template DNA. A minimum of 0.2-ng template DNA was found to be necessary for accurate sex determination with this method. When using ultraviolet-irradiated template DNA, as mock forensic samples, the sex of the samples could not be determined by short tandem repeat (STR) analysis but was correctly determined using our method. Thus, we successfully developed a method of sex determination based on the number of X chromosomes. Our novel method will be useful in forensic practice for sex determination.

Determination of microplastic polyethylene (PE) and polypropylene (PP) in environmental samples using thermal analysis (TGA-DSC).

PubMed

Majewsky, Marius; Bitter, Hajo; Eiche, Elisabeth; Horn, Harald

2016-10-15

Microplastics are increasingly detected in the environment and the consequences on water resources and ecosystems are not clear to date. The present study provides a cost-effective and straightforward method to determine the mass concentrations of polymer types using thermal analysis. Characteristic endothermic phase transition temperatures were determined for seven plastic polymer types using TGA-DSC. Based on that, extracts from wastewater samples were analyzed. Results showed that among the studied polymers, only PE and PP could be clearly identified, while the phase transition signals of the other polymers largely overlap each other. Subsequently, calibration curves were run for PE and PP for qualitative measurements. 240 and 1540mg/m(3) of solid material (12µm to 1mm) was extracted from two wastewater effluent samples of a municipal WWTP of which 34% (81mg/m(3)) and 17% (257mg/m(3)) could be assigned to PE, while PP was not detected in any of the samples. The presented application of TGA-DSC provides a complementary or alternative method to FT-IR analyses for the determination of PE and PP in environmental samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of diphacinone in sea water, vertebrates, invertebrates, and bait pellet formulations following aerial broadcast on Mokapu Island, Molokai, Hawai'i

USGS Publications Warehouse

Gale, Robert W.; Tanner, Michael; Orazio, Carl E.

2008-01-01

This report presents the results of a study to determine diphacinone concentrations in samples of sea water and in fillet samples of fish and in limpets from the ocean adjacent to Mokapu Island and from reference samples from Molokai, Hawai'i; concentrations of the active ingredient (diphacinone) were also determined in samples of the Ramik Green bait pellets used for the broadcast study. After preparation, diphacinone concentrations were determined with high-performance liquid chromatography with photodiode array detection. No detectable concentrations of diphacinone were found in the fish, limpets, or sea-water samples from Mokapu Island or from the reference sites. The limit of detection for diphacinone in sea water was 18 nanograms per milliliter (parts per billion); the limit of detection in fish fillets was 10 nanograms per gram (parts per billion); and the limit of detection in limpets was 17 nanograms per gram. The average concentration of diphacinone in the Ramik Green bait pellets was 45 micrograms per gram (parts per million), which represents 90 percent of the nominal concentration stated for the product by the manufacturer.

Preserving ground water samples with hydrochloric acid does not result in the formation of chloroform

USGS Publications Warehouse

Squillace, Paul J.; Pankow, James F.; Barbash, Jack E.; Price, Curtis V.; Zogorski, John S.

1999-01-01

Water samples collected for the determination of volatile organic compounds (VOCs) are often preserved with hydrochloric acid (HCl) to inhibit the biotransformation of the analytes of interest until the chemical analyses can he performed. However, it is theoretically possible that residual free chlorine in the HCl can react with dissolved organic carbon (DOC) to form chloroform via the haloform reaction. Analyses of 1501 ground water samples preserved with HCl from the U.S. Geological Survey's National Water-Quality Assessment Program indicate that chloroform was the most commonly detected VOC among 60 VOCs monitored. The DOC concentrations were not significantly larger in samples with detectable chloroform than in those with no delectable chloroform, nor was there any correlation between the concentrations of chloroform and DOC. Furthermore, chloroform was detected more frequently in shallow ground water in urban areas (28.5% of the wells sampled) than in agricultural areas (1.6% of the wells sampled), which indicates that its detection was more related to urban land-use activities than to sample acidification. These data provide strong evidence that acidification with HCl does not lead to the production of significant amounts of chloroform in ground water samples. To verify these results, an acidification study was designed to measure the concentrations of all trihalomethanes (THMs) that can form as a result of HCl preservation in ground water samples and to determine if ascorbic acid (C6H8O6) could inhibit this reaction if it did occur. This study showed that no THMs were formed as a result of HCl acidification, and that ascorbic acid had no discernible effect on the concentrations of THMs measured.

Micro-sampling method based on high-resolution continuum source graphite furnace atomic absorption spectrometry for calcium determination in blood and mitochondrial suspensions.

PubMed

Gómez-Nieto, Beatriz; Gismera, Mª Jesús; Sevilla, Mª Teresa; Satrústegui, Jorgina; Procopio, Jesús R

2017-08-01

A micro-sampling and straightforward method based on high resolution continuum source atomic absorption spectrometry (HR-CS AAS) was developed to determine extracellular and intracellular Ca in samples of interest in clinical and biomedical analysis. Solid sampling platforms were used to introduce the micro-samples into the graphite furnace atomizer. The secondary absorption line for Ca, located at 239.856nm, was selected to carry out the measurements. Experimental parameters such as pyrolysis and atomization temperatures and the amount of sample introduced for the measurements were optimized. Calibration was performed using aqueous standards and the approach to measure at the wings of the absorption lines was employed for the expansion of the linear response range. The limit of detection was of 0.02mgL -1 Ca (0.39ng Ca) and the upper limit of linear range was increased up to 8.0mgL -1 Ca (160ng Ca). The proposed method was used to determine Ca in mitochondrial suspensions and whole blood samples with successful results. Adequate recoveries (within 91-107%) were obtained in the tests performed for validation purposes. Copyright © 2017 Elsevier B.V. All rights reserved.

[Determination of ten photoinitiators in fruit juices and tea beverages by solid-phase micro-extraction coupled with gas chromatography/mass spectrometry].

PubMed

Liu, Pengyan; Chen, Yanjie; Zhao, Chunxia; Tian, Lei

2013-12-01

A method for the determination of ten photoinitiators (PIs), benzophenone, ethyl 4-dimethylaminobenzoate, 1-hydroxycyclohexyl-phenylketone, 4-methylbenzophenone, 2-ethylhexyl-4-dimethylaminobenzoate, 4-chlorobenzophenone, 2-chlorothioxanthone, 2-isopropylthio-xanthone, 2,2-dimethoxy-2-phenylacetophenone, methyl 2-benzoylbenzoate, in 13 kinds of fruit juice and 3 kinds of tea beverage has been established, using solid-phase micro-extraction (SPME) combined with chromatography/mass spectrometry (GC/MS). At first, the major factors of SPME, extraction time and temperature, were studied through orthogonal experiment. Then the optimal operation conditions were obtained via the refinement of various factors. After the sample was extracted by SPME, it was desorbed for target analytes in sampling inlet for 3 min, and separated on an HP-5MS column, then detected by MS in selected ion monitoring mode, and quantified through calibration curve. The working curves were obtained using sample matrix in order to eliminate the matrix interference. The linear range was from 0.3 microg/L to 60 microg/L and the detection limit range was from 3 ng/L to 16 ng/L. The samples were determined five times with four different spiked levels individually and the relative standard deviations of all the samples were less than 14.5%. This determination method was applied in 16 kinds of packed beverages with different brands and different species. Benzophenone had been detected from all the samples. 4-Methylbenzophenone, 2-ethylhexyl-4-dimethylaminobenzoate, 2-isopropylthioxanthone, 1-hydroxycyclohexyl-phenylketone and 2-chlorothioxanthone had been detected from a portion of samples. Simultaneous determination was achieved for the ten PIs. These results provide a reference to determine the PIs migrated from packing materials in beverage. This method is simple, high sensitive and non-polluting.

Non destructive multi elemental analysis using prompt gamma neutron activation analysis techniques: Preliminary results for concrete sample

NASA Astrophysics Data System (ADS)

Dahing, Lahasen@Normanshah; Yahya, Redzuan; Yahya, Roslan; Hassan, Hearie

2014-09-01

In this study, principle of prompt gamma neutron activation analysis has been used as a technique to determine the elements in the sample. The system consists of collimated isotopic neutron source, Cf-252 with HPGe detector and Multichannel Analysis (MCA). Concrete with size of 10×10×10 cm3 and 15×15×15 cm3 were analysed as sample. When neutrons enter and interact with elements in the concrete, the neutron capture reaction will occur and produce characteristic prompt gamma ray of the elements. The preliminary result of this study demonstrate the major element in the concrete was determined such as Si, Mg, Ca, Al, Fe and H as well as others element, such as Cl by analysis the gamma ray lines respectively. The results obtained were compared with NAA and XRF techniques as a part of reference and validation. The potential and the capability of neutron induced prompt gamma as tool for multi elemental analysis qualitatively to identify the elements present in the concrete sample discussed.

Resolving occlusion and segmentation errors in multiple video object tracking

NASA Astrophysics Data System (ADS)

Cheng, Hsu-Yung; Hwang, Jenq-Neng

2009-02-01

In this work, we propose a method to integrate the Kalman filter and adaptive particle sampling for multiple video object tracking. The proposed framework is able to detect occlusion and segmentation error cases and perform adaptive particle sampling for accurate measurement selection. Compared with traditional particle filter based tracking methods, the proposed method generates particles only when necessary. With the concept of adaptive particle sampling, we can avoid degeneracy problem because the sampling position and range are dynamically determined by parameters that are updated by Kalman filters. There is no need to spend time on processing particles with very small weights. The adaptive appearance for the occluded object refers to the prediction results of Kalman filters to determine the region that should be updated and avoids the problem of using inadequate information to update the appearance under occlusion cases. The experimental results have shown that a small number of particles are sufficient to achieve high positioning and scaling accuracy. Also, the employment of adaptive appearance substantially improves the positioning and scaling accuracy on the tracking results.

Sensitivity of different Trypanosoma vivax specific primers for the diagnosis of livestock trypanosomosis using different DNA extraction methods.

PubMed

Gonzales, J L; Loza, A; Chacon, E

2006-03-15

There are several T. vivax specific primers developed for PCR diagnosis. Most of these primers were validated under different DNA extraction methods and study designs leading to heterogeneity of results. The objective of the present study was to validate PCR as a diagnostic test for T. vivax trypanosomosis by means of determining the test sensitivity of different published specific primers with different sample preparations. Four different DNA extraction methods were used to test the sensitivity of PCR with four different primer sets. DNA was extracted directly from whole blood samples, blood dried on filter papers or blood dried on FTA cards. The results showed that the sensitivity of PCR with each primer set was highly dependant of the sample preparation and DNA extraction method. The highest sensitivities for all the primers tested were determined using DNA extracted from whole blood samples, while the lowest sensitivities were obtained when DNA was extracted from filter paper preparations. To conclude, the obtained results are discussed and a protocol for diagnosis and surveillance for T. vivax trypanosomosis is recommended.

Structural, magnetic and transport properties of Pb{sub 2}Cr{sub 1+x}Mo{sub 1−x}O{sub 6} (−1≤x≤1/3)

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

Zhao, H.F.; School of Mathematics and Physics, University of Science and Technology, Beijing 100083; Cao, L.P.

Pb{sub 2}Cr{sub 1+x}Mo{sub 1-x}O{sub 6} (−1≤x≤1/3) samples were synthesized via a high pressure and high temperature route. X-ray diffraction results suggest the samples crystallize in a disordered double perovskite structure (Pm-3m). X-ray photoemission spectroscopy results confirm the presence of Mo{sup 4+} for x=−1 and Mo{sup 6+} for x=1/3. The measured magnetic and electrical properties exhibit systematic change with increasing x. - Highlights: • A series of Pb{sub 2}Cr{sub 1+x}Mo{sub 1−x}O{sub 6} samples were synthesized under high pressure. • Magnetic and electrical properties of the series samples were investigated. • Valence states of Cr and Mo were determined through the analysesmore » of XRD and XPS results. • Ground state of PbMoO{sub 3} were determined through the transport study and first-principles calculations.« less

Determination of Porosity in Shale by Double Headspace Extraction GC Analysis.

PubMed

Zhang, Chun-Yun; Li, Teng-Fei; Chai, Xin-Sheng; Xiao, Xian-Ming; Barnes, Donald

2015-11-03

This paper reports on a novel method for the rapid determination of the shale porosity by double headspace extraction gas chromatography (DHE-GC). Ground core samples of shale were placed into headspace vials and DHE-GC measurements of released methane gas were performed at a given time interval. A linear correlation between shale porosity and the ratio of consecutive GC signals was established both theoretically and experimentally by comparing with the results from the standard helium pycnometry method. The results showed that (a) the porosity of ground core samples of shale can be measured within 30 min; (b) the new method is not significantly affected by particle size of the sample; (c) the uncertainties of measured porosities of nine shale samples by the present method range from 0.31 to 0.46 p.u.; and (d) the results obtained by the DHE-GC method are in a good agreement with those from the standard helium pycnometry method. In short, the new DHE-GC method is simple, rapid, and accurate, making it a valuable tool for shale gas-related research and applications.

Investigation of the "true" extraction recovery of analytes from multiple types of tissues and its impact on tissue bioanalysis using two model compounds.

PubMed

Yuan, Long; Ma, Li; Dillon, Lisa; Fancher, R Marcus; Sun, Huadong; Zhu, Mingshe; Lehman-McKeeman, Lois; Aubry, Anne-Françoise; Ji, Qin C

2016-11-16

LC-MS/MS has been widely applied to the quantitative analysis of tissue samples. However, one key remaining issue is that the extraction recovery of analyte from spiked tissue calibration standard and quality control samples (QCs) may not accurately represent the "true" recovery of analyte from incurred tissue samples. This may affect the accuracy of LC-MS/MS tissue bioanalysis. Here, we investigated whether the recovery determined using tissue QCs by LC-MS/MS can accurately represent the "true" recovery from incurred tissue samples using two model compounds: BMS-986104, a S1P 1 receptor modulator drug candidate, and its phosphate metabolite, BMS-986104-P. We first developed a novel acid and surfactant assisted protein precipitation method for the extraction of BMS-986104 and BMS-986104-P from rat tissues, and determined their recoveries using tissue QCs by LC-MS/MS. We then used radioactive incurred samples from rats dosed with 3 H-labeled BMS-986104 to determine the absolute total radioactivity recovery in six different tissues. The recoveries determined using tissue QCs and incurred samples matched with each other very well. The results demonstrated that, in this assay, tissue QCs accurately represented the incurred tissue samples to determine the "true" recovery, and LC-MS/MS assay was accurate for tissue bioanalysis. Another aspect we investigated is how the tissue QCs should be prepared to better represent the incurred tissue samples. We compared two different QC preparation methods (analyte spiked in tissue homogenates or in intact tissues) and demonstrated that the two methods had no significant difference when a good sample preparation was in place. The developed assay showed excellent accuracy and precision, and was successfully applied to the quantitative determination of BMS-986104 and BMS-986104-P in tissues in a rat toxicology study. Copyright © 2016 Elsevier B.V. All rights reserved.

Efficacy of Sex Determination from Human Dental Pulp Tissue and its Reliability as a Tool in Forensic Dentistry

PubMed Central

Khanna, Kaveri Surya

2015-01-01

Background: Sex determination is one of the primary steps in forensics. Barr body can be used as a histological method for identification of sex as it is found to be specific to female somatic cells and rare in male cells. To demarcate human dental pulp as an important identification tool of sex in forensic odontology (FO) and to evaluate the time period till which sex can be determined from pulp tissue using three stains H and E, Feulgen, and acridine - orange under fluorescence so as. Materials and Methods: 90 pulp samples (45 males and 45 females) were subjected to Barr body analysis for determination of sex using light and fluorescent microscopy. Results: Barr body was found to be positive for female samples and negative or rare in the male sample (<3%). Conclusion: Barr body from human dental pulp tissue can be used as a successful determinant of sex identification in FO. PMID:26668474

Structure determination of an integral membrane protein at room temperature from crystals in situ

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

Axford, Danny; Foadi, James; Imperial College London, London SW7 2AZ

2015-05-14

The X-ray structure determination of an integral membrane protein using synchrotron diffraction data measured in situ at room temperature is demonstrated. The structure determination of an integral membrane protein using synchrotron X-ray diffraction data collected at room temperature directly in vapour-diffusion crystallization plates (in situ) is demonstrated. Exposing the crystals in situ eliminates manual sample handling and, since it is performed at room temperature, removes the complication of cryoprotection and potential structural anomalies induced by sample cryocooling. Essential to the method is the ability to limit radiation damage by recording a small amount of data per sample from many samplesmore » and subsequently assembling the resulting data sets using specialized software. The validity of this procedure is established by the structure determination of Haemophilus influenza TehA at 2.3 Å resolution. The method presented offers an effective protocol for the fast and efficient determination of membrane-protein structures at room temperature using third-generation synchrotron beamlines.« less

Spectrophotometric determination of sulphate in automotive fuel ethanol by sequential injection analysis using dimethylsulphonazo(III) reaction.

PubMed

de Oliveira, Fabio Santos; Korn, Mauro

2006-01-15

A sensitive SIA method was developed for sulphate determination in automotive fuel ethanol. This method was based on the reaction of sulphate with barium-dimethylsulphonazo(III) leading to a decrease on the magnitude of analytical signal monitored at 665 nm. Alcohol fuel samples were previously burned up to avoid matrix effects for sulphate determinations. Binary sampling and stop-flow strategies were used to increase the sensitivity of the method. The optimization of analytical parameter was performed by response surface method using Box-Behnker and central composite designs. The proposed sequential flow procedure permits to determine up to 10.0mg SO(4)(2-)l(-1) with R.S.D. <2.5% and limit of detection of 0.27 mg l(-1). The method has been successfully applied for sulphate determination in automotive fuel alcohol and the results agreed with the reference volumetric method. In the optimized condition the SIA system carried out 27 samples per hour.

Binary Colloidal Alloy Test-5: Three-Dimensional Melt

NASA Technical Reports Server (NTRS)

Yodh, Arjun G.

2008-01-01

Binary Colloidal Alloy Test - 5: Three-Dimensional Melt (BCAT-5-3DMelt) photographs initially randomized colloidal samples in microgravity to determine their resulting structure over time. BCAT-5-3D-Melt will allow the scientists to capture the kinetics (evolution) of their samples, as well as the final equilibrium state of each sample. BCAT-5-3D-Melt will look at the mechanisms of melting using three-dimensional temperature sensitive colloidal crystals. Results will help scientists develop fundamental physics concepts previously shadowed by the effects of gravity.

Determination of total mercury in environmental and biological samples by flow injection cold vapour atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Murphy, James; Jones, Phil; Hill, Steve J.

1996-12-01

A simple and accurate method has been developed for the determination of total mercury in environmental and biological samples. The method utilises an off-line microwave digestion stage followed by analysis using a flow injection system with detection by cold vapour atomic absorption spectrometry. The method has been validated using two certified reference materials (DORM-1 dogfish and MESS-2 estuarine sediment) and the results agreed well with the certified values. A detection limit of 0.2 ng g -1 Hg was obtained and no significant interference was observed. The method was finally applied to the determination of mercury in river sediments and canned tuna fish, and gave results in the range 0.1-3.0 mg kg -1.

A simple and automated sample preparation system for subsequent halogens determination: Combustion followed by pyrohydrolysis.

PubMed

Pereira, L S F; Pedrotti, M F; Vecchia, P Dalla; Pereira, J S F; Flores, E M M

2018-06-20

A simple and automated system based on combustion followed by a pyrohydrolysis reaction was proposed for further halogens determination. This system was applied for digestion of soils containing high (90%) and also low (10%) organic matter content for further halogens determination. The following parameters were evaluated: sample mass, use of microcrystalline cellulose and heating time. For analytes absorption, a diluted alkaline solution (6 mL of 25 mmol L -1  NH 4 OH) was used in all experiments. Up to 400 mg of soil with high organic matter content and 100 mg of soil with low organic matter content (mixed with 400 mg of cellulose) could be completely digested using the proposed system. Quantitative results for all halogens were obtained using less than 12 min of sample preparation step (about 1.8 min for sample combustion and 10 min for pyrohydrolysis). The accuracy was evaluated using a certified reference material of coal and spiked samples. No statistical difference was observed between the certified values and results obtained by the proposed method. Additionally, the recoveries obtained using spiked samples were in the range of 98-103% with relative standard deviation values lower than 5%. The limits of quantification obtained for F, Cl, Br and I for soil with high (400 mg of soil) and low (100 mg of soil) organic matter were in the range of 0.01-2 μg g -1 and 0.07-59 μg g -1 , respectively. The proposed system was considered as a simple and suitable alternative for soils digestion for further halogens determination by ion chromatography and inductively coupled plasma mass spectrometry techniques. Copyright © 2018 Elsevier B.V. All rights reserved.

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.

Comparison of spectrofluorometric and HPLC methods for the characterization of fecal porphyrins in river otters.

PubMed

Taylor, C; Duffy, L K; Plumley, F G; Bowyer, R T

2000-09-01

A spectrofluorometric method (B. Grandchamp et al., 1980, Biochem. Biophys. Acta 629, 577-586) developed for the determination of amounts of uroporphyrin I (Uro I), coproporphyrin III (Copro III), and protoporphyrin IX (Proto IX) in skin fibroblasts was compared with a high-performance liquid chromatography (HPLC) method for the analysis of porphyrins in fecal samples of river otters (Lutra canadensis). Heptacarboxylate porphyrin I and coproporphyrin I, two porphyrins determined to be critical in defining the porphyrin profile in fecal samples of river otters with the HPLC method, contributed substantially to the calculation of the concentrations of Uro I and Copro III, respectively, in standard solutions of porphyrins with the spectrofluorometric method. Fluorescent components of the fecal matrix complicated the determination of the concentrations of Uro I, Copro III, and Proto IX with the spectrofluorometric method and resulted in erroneous values for the concentrations of these porphyrins compared with values determined with the HPLC method. These results indicate that the complexity of the sample, particularly with regard to the potential presence of interfering fluorescent compounds, as well as porphyrins additional to Uro I, Copro III, and Proto IX, should be considered prior to the application of the spectrofluorometric method. An alternative HPLC method developed for the rapid characterization of porphyrin profiles in fecal samples of river otters is described. Copyright 2000 Academic Press.

Cultural and Molecular Evidence of Legionella spp. Colonization in Dental Unit Waterlines: Which Is the Best Method for Risk Assessment?

PubMed

Ditommaso, Savina; Giacomuzzi, Monica; Ricciardi, Elisa; Zotti, Carla M

2016-02-06

Legionella spp. are ubiquitous in aquatic habitats and water distribution systems, including dental unit waterlines (DUWLs). The aim of the present study was to determine the prevalence of Legionella in DUWLs and tap water samples using PMA-qPCR and standard culture methods. The total viable counts (TVCs) of aerobic heterotrophic bacteria in the samples were also determined. Legionella spp. were detected and quantified using the modified ISO 11731 culture method. Extracted genomic DNA was analysed using the iQ-Check Quanti Legionella spp. kit, and the TVCs were determined according to the ISO protocol 6222. Legionella spp. were detected in 100% of the samples using the PMA-qPCR method, whereas these bacteria were detected in only 7% of the samples using the culture method. The number of colony forming units (CFUs) of the TVCs in the DUWL and tap water samples differed, with the bacterial load being significantly lower in the tap water samples (p-value = 0). The counts obtained were within the Italian standard range established for potable water in only 5% of the DUWL water samples and in 77% of the tap water samples. Our results show that the level of Legionella spp. contamination determined using the culture method does not reflect the true scale of the problem, and consequently we recommend testing for the presence of aerobic heterotrophic bacteria based on the assumption that Legionella spp. are components of biofilms.

Cultural and Molecular Evidence of Legionella spp. Colonization in Dental Unit Waterlines: Which Is the Best Method for Risk Assessment?

PubMed Central

Ditommaso, Savina; Giacomuzzi, Monica; Ricciardi, Elisa; Zotti, Carla M.

2016-01-01

Legionella spp. are ubiquitous in aquatic habitats and water distribution systems, including dental unit waterlines (DUWLs). The aim of the present study was to determine the prevalence of Legionella in DUWLs and tap water samples using PMA-qPCR and standard culture methods. The total viable counts (TVCs) of aerobic heterotrophic bacteria in the samples were also determined. Legionella spp. were detected and quantified using the modified ISO 11731 culture method. Extracted genomic DNA was analysed using the iQ-Check Quanti Legionella spp. kit, and the TVCs were determined according to the ISO protocol 6222. Legionella spp. were detected in 100% of the samples using the PMA-qPCR method, whereas these bacteria were detected in only 7% of the samples using the culture method. The number of colony forming units (CFUs) of the TVCs in the DUWL and tap water samples differed, with the bacterial load being significantly lower in the tap water samples (p-value = 0). The counts obtained were within the Italian standard range established for potable water in only 5% of the DUWL water samples and in 77% of the tap water samples. Our results show that the level of Legionella spp. contamination determined using the culture method does not reflect the true scale of the problem, and consequently we recommend testing for the presence of aerobic heterotrophic bacteria based on the assumption that Legionella spp. are components of biofilms. PMID:26861373

Detection of pyrethroid pesticides and their environmental degradation products in duplicate diet samples

EPA Science Inventory

The abstract is for an oral presentation at the Asilomar Conference on Mass Spectrometry: Mass Spectrometry in Environmental Chemistry, Toxicology, and Health. It describes analytical method development and sample results for determination of pyrethroid pesticides and environme...

Determination of rare earth elements, uranium and thorium in geological samples by ICP-MS, using an automatic fusion machine as an alkaline digestion tool.

NASA Astrophysics Data System (ADS)

Granda, Luis; Rivera, Maria; Velasquez, Colon; Barona, Diego; Carpintero, Natalia

2014-05-01

At the present time, rare earth elements deposits have became in strategic resources for extraction of raw materials in order to manufacture high tech devices (computers, LCD, cell phones, batteries for hybrid vehicles, fiber optics and wind turbines) (1).The appropriate analytical determination of the REE ( rare earth elements) in sediment and rock samples , is important to find potential deposits and to recognize geological environments for identifying possible alterations and mineral occurrences. The alkaline fusion, which aim is to move the entire sample from solid to liquid state by forming water soluble complexes of boron and lithium, as a previous procedure for the determination of these elements, usually takes a lot of time due to the complexity of the analysis phase and by the addition of other reagents (Tm and HF ) (2) to compensate the lack of strict temperature control. The objective of this work is to develop an efficient alternative to alkaline digestion using an electrical fusion machine, which allows to create temperature programs with advanced process control and supports up to 5 samples simultaneously, which generates a reproducibility of the method and results during the melting step. Additionally, this new method permits the processing of a larger number of samples in a shorter time. The samples analyzed in this method were weighed into porcelain crucibles and subjected to calcination for 4 hours at 950 ° C in order to determine the Lost on Ignition (LOI ) , that serves to adjust the analytical results and to preserve the shelf life of the platinum ware. Subsequently, a fraction of the calcined sample was weighed into platinum crucibles and mixed with ultra-pure lithium metaborate ( flux ) 1:4 . The crucible was then placed in the fusion machine, which was programmed to take the sample from room temperature to 950 ° C in five minutes, make a small ramp to 970 ° C maintain that temperature for five minutes and download the melt in a 10 % v / v nitric acid solution . After an incorporation time, a fraction of this sample was then diluted 20 times in ultrapure deionized water ( resistivity greater 18.2 megohms / cm ). The diluted sample was analized in the ICP- MS, which was setted in high sensitivity mode. The results were compared through cross samples (the same samples tested in the laboratory were sent to another international laboratory, which works under accreditation ISO 17025 ) and no major deviations (5%) was obtained by making comparisons between the two laboratories. When comparing the results and evaluated the development of the art, it is concluded that this is an alternative that allows performing samples up to 50 alkaline fusions per day with great accuracy, saving resources and time. References: (1) British Geological Survey, Natural Environment Research Council, , Minerals UK Centre of Sustainable mineral development: Rare Earth Elements, p18-22, 2011 (2) Germain Bayon, Jean Alix Barrat, Joel Etoubleau, Mathieu Benoit ,Claire Bollinger, and Sidonie Revillon: Determination of Rare Earth Elements, Sc, Y, Zr, Ba, Hf and Th in Geological Samples by ICP-MS after Tm Addition and Alkaline Fusion, Geostandards and Geoanalytical Research, vol 33-N1, p51-62, 2008

The Comparison of Detrital Zircon Ages to Point Count Provenance Analysis for the Pottsville Sandstone in the Northern Appalachian Foreland Basin Venango County, Pennsylvania

NASA Astrophysics Data System (ADS)

Loveday, S.; Harris, D. B.; Schiappa, T.; Pecha, M.

2017-12-01

The specific sources of sediments deposited in the Appalachian basin prior to and immediately following the Alleghenian orogeny has long been a topic of debate. Recent advances in U-Pb dating of detrital zircons have greatly helped to determine some of the sources of these sediments. For this study, sandstone samples were collected from the Pottsville Formation in the northern Appalachian Foreland Basin, Venango County, Pennsylvania to provide supplementary data for previous work that sought to describe the provenance of the same sediments by point counts of thin sections of the same units. Results of this previous work established that the provenance for these units was transitional recycled orogenic, including multiple recycled sediments, and that a cratonic contribution was not able to be determined clearly. The previous results suggested that the paleoenvironment was a fluvial dominated delta prograding in the northern direction. However, no geochronologic data was found during this study to confirm this interpretation. We sought to verify these results by U-Pb analysis of detrital zircons. Samples were collected from the areas where the previous research took place. U-Pb ages were found from sample at the highest elevation and lowest elevation. In the first sample, sample 17SL01 (younger sample stratigraphically), the zircons yield U-Pb age range peaks at 442-468 ma and 1037-1081 ma. The probability density plot for this specific sample displays a complete age gap from 500 ma to 811 ma. In the second sample, sample 17SL03 (older rock stratigraphically), the zircons yield U-Pb ages range peaks of 424-616 ma and 975-1057 ma. This sample doesn't show any ages younger than 424 ma and it doesn't display the sample age gap as sample 17SL01 does. The ages of zircons are consistent with thin section point counting provenance results from previous research suggesting zircon transport from the northern direction.

Elemental Analysis of Beryllium Samples Using a Microzond-EGP-10 Unit

NASA Astrophysics Data System (ADS)

Buzoverya, M. E.; Karpov, I. A.; Gorodnov, A. A.; Shishpor, I. V.; Kireycheva, V. I.

2017-12-01

Results concerning the structural and elemental analysis of beryllium samples obtained via different technologies using a Microzond-EGP-10 unit with the help of the PIXE and RBS methods are presented. As a result, the overall chemical composition and the nature of inclusions were determined. The mapping method made it possible to reveal the structural features of beryllium samples: to select the grains of the main substance having different size and chemical composition, to visualize the interfaces between the regions of different composition, and to describe the features of the distribution of impurities in the samples.

Long-term storage of salivary cortisol samples at room temperature

NASA Technical Reports Server (NTRS)

Chen, Yu-Ming; Cintron, Nitza M.; Whitson, Peggy A.

1992-01-01

Collection of saliva samples for the measurement of cortisol during space flights provides a simple technique for studying changes in adrenal function due microgravity. In the present work, several methods for preserving saliva cortisol at room temperature were investigated using radioimmunoassays for determining cortisol in saliva samples collected on a saliva-collection device called Salivettes. It was found that a pretreatment of Salivettes with citric acid resulted in preserving more than 85 percent of the salivary cortisol for as long as six weeks. The results correlated well with those for a sample stored in a freezer on an untreated Salivette.

Effect of preheat repetition on color stability of methacrylate- and silorane-based composite resins.

PubMed

Abed Kahnamouei, Mehdi; Gholizadeh, Sarah; Rikhtegaran, Sahand; Daneshpooy, Mehdi; Kimyai, Soodabeh; Alizadeh Oskoee, Parnian; Rezaei, Yashar

2017-01-01

Background. The aim of this study was to investigate the effect of preheating methacrylate- and silorane-based composite resins on their color stability up to 40 times at 55‒60°C. Methods. Seventy-six methacrylate and silorane-based composite resin samples, with a diameter of 10 mm and a height of 2 mm, were divided into 4 groups (n=19). After the samples were prepared, their color parameters were determined using a reflective spectrophotometer. The composite resin samples were separately stored in a solution of tea for 40 consecutive days. Then the samples underwent a color determination procedure again using a spectrophotometer and color changes were recorded. Finally two-way ANOVA was used to study the effect of composite temperature on its staining (P<0.05). Independent-samples t-test was used to evaluate changes in conversion rates of preheated composite resin samples compared to non-heated samples at P=0.005 and P=0.029 for silorane-based and Z250 composite resin samples, respectively. Results. Both composite resin type (P=0.014) and preheating (P<0.001) had significant effects on ΔE. Conclusion. Repeated preheating of methacrylate- and silorane-based composite resin samples, up to 55‒60°C for 40 rounds, resulted in more color changes compared with unheated composite resin samples. After storage in a solution of tea the color change rate in the composite resin samples of silorane-based was higher than the Z250 composite resin samples.

Effect of preheat repetition on color stability of methacrylate- and silorane-based composite resins

PubMed Central

Abed Kahnamouei, Mehdi; Gholizadeh, Sarah; Rikhtegaran, Sahand; Daneshpooy, Mehdi; Kimyai, Soodabeh; Alizadeh Oskoee, Parnian; Rezaei, Yashar

2017-01-01

Background. The aim of this study was to investigate the effect of preheating methacrylate- and silorane-based composite resins on their color stability up to 40 times at 55‒60°C. Methods. Seventy-six methacrylate and silorane-based composite resin samples, with a diameter of 10 mm and a height of 2 mm, were divided into 4 groups (n=19). After the samples were prepared, their color parameters were determined using a reflective spectrophotometer. The composite resin samples were separately stored in a solution of tea for 40 consecutive days. Then the samples underwent a color determination procedure again using a spectrophotometer and color changes were recorded. Finally two-way ANOVA was used to study the effect of composite temperature on its staining (P<0.05). Independent-samples t-test was used to evaluate changes in conversion rates of preheated composite resin samples compared to non-heated samples at P=0.005 and P=0.029 for silorane-based and Z250 composite resin samples, respectively. Results. Both composite resin type (P=0.014) and preheating (P<0.001) had significant effects on ΔE. Conclusion. Repeated preheating of methacrylate- and silorane-based composite resin samples, up to 55‒60°C for 40 rounds, resulted in more color changes compared with unheated composite resin samples. After storage in a solution of tea the color change rate in the composite resin samples of silorane-based was higher than the Z250 composite resin samples. PMID:29354248

Determination of aflatoxin B1 levels in organic spices and herbs.

PubMed

Tosun, Halil; Arslan, Recep

2013-01-01

Organically produced spices and herbs were analyzed for determination of aflatoxin B1 (AFB1) by ELISA using immunoaffinity column. For this purpose 93 organic spices and 37 organic herbs were randomly selected from organic markets and organic shops in Turkey. AFB1 was detected in 58 organic spice and 32 organic herb samples. Among organic spice samples, the maximum value was detected in cinnamon sample (53 μg/kg). AFB1 was not detected in thyme samples. AFB1 levels of 41 organic spice samples were above the EU regulatory limit (5 μg/kg). Among organic herb samples the highest concentration of AFB1 (52.5 μg/kg) was detected in a rosehip sample. AFB1 levels of 21 organic herb samples were above the regulatory limits of the European Union. These results showed that more stringent measures must be taken for the prevention of mold contamination in the production of organic spices and herbs.

Determination of Aflatoxin B1 Levels in Organic Spices and Herbs

PubMed Central

Tosun, Halil; Arslan, Recep

2013-01-01

Organically produced spices and herbs were analyzed for determination of aflatoxin B1 (AFB1) by ELISA using immunoaffinity column. For this purpose 93 organic spices and 37 organic herbs were randomly selected from organic markets and organic shops in Turkey. AFB1 was detected in 58 organic spice and 32 organic herb samples. Among organic spice samples, the maximum value was detected in cinnamon sample (53 μg/kg). AFB1 was not detected in thyme samples. AFB1 levels of 41 organic spice samples were above the EU regulatory limit (5 μg/kg). Among organic herb samples the highest concentration of AFB1 (52.5 μg/kg) was detected in a rosehip sample. AFB1 levels of 21 organic herb samples were above the regulatory limits of the European Union. These results showed that more stringent measures must be taken for the prevention of mold contamination in the production of organic spices and herbs. PMID:23766719

Determining bovine viral diarrhea and infectious bovine rhinotracheitis infections in dairy cattle using precolostral blood.

PubMed

Baillargeon, Paul; Arango-Sabogal, Juan C; Wellemans, Vincent; Fecteau, Gilles

2017-04-01

The objective of this study was to determine if precolostral blood samples are useful to detect apparent fetal infections with bovine viral diarrhea (BVD) and infectious bovine rhinotracheitis (IBR) viruses. A convenience sample of 317 sera from 50 Canadian herds was used in the study. Antibody level was measured using 2 commercial IBR and BVD ELISA kits. Precolostral status of sera was confirmed on 304 samples using serum gamma-glutamyl transferase activity. Postcolostral serum samples yielded a higher proportion of positive results to IBR (OR = 86; 95% CI: 17.8 to 415.7) and BVD (OR = 199.3; 95% CI: 41.7 to 952.3) than did precolostral samples. All positive precolostral serum samples ( n = 7 of 304) originated from calves born to vaccinated cows. Postcolostral positive serum samples ( n = 11 of 13) originated mostly (60%) from calves born to non-vaccinated cows. Precolostral serum sampling can detect apparent fetal infections in a herd.

Interfacial electronic structure and full spectral Hamaker constants of Si{sub 3}N{sub 4} intergranular films from VUV and SR-VEEL spectroscopy

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

French, R.H.; Scheu, C.; Duscher, G.

1995-09-01

The interfacial electronic structure, presented as the interband transition strength J{sub cv}({omega}) of the interatomic bonds, can be determined by Kramers Kronig (KK) analysis of vacuum ultraviolet (VUV) reflectance or spatially resolved valence electron energy loss (SR-VEEL) spectra. For the wetted interfaces in Si{sub 3}N{sub 4}, equilibrium thin glass films are formed whose thickness is determined by a force balance between attractive and repulsive force terms KK analysis of J{sub cv}({omega}) to yield {var_epsilon}{sub 2}({xi}) for the phases present, permits the direct calculation of the configuration-dependent Hamaker constants for the attractive vdW forces from the interfacial electronic structure. Interband transitionmore » strengths and full spectral Hamaker constants for Si{sub 3}N{sub 4}samples containing a SiYAlON glass have been determined using SR-VEELS from grains and grain boundaries and compared with results from bulk VUV spectroscopy on separate samples of glass and nitride. The A{sub 121}Hamaker constant for Si{sub 3}N{sub 4} with glass of the bulk composition is 8 zJ (zJ = 10{sup {minus}21}J) from the more established optical method. The EELS method permits the determination of vdW forces based upon actual local compositions and structure, which may differ noticeably from bulk standards. Current results show that full spectral Hamaker constants determined from VUV and SR-VEEL measurements of uniform bulk samples agree, but care must be take in the single scattering and zero loss subtraction corrections, and more work is ongoing in this area. Still the results show that for the grain boundary films present in these polycrystalline Si{sub 3}N{sub 4} samples the glass composition is of lower index of refraction. This can arise from increased oxygen content in determined in situ from the SR-VEELS of a particular grain boundary film. 45 refs.« less

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; arsenic speciation in natural-water samples using laboratory and field methods

USGS Publications Warehouse

Garbarino, John R.; Bednar, Anthony J.; Burkhardt, Mark R.

2002-01-01

Analytical methods for the determination of arsenite [As(III)], arsenate [As(V)], dimethylarsinate (DMA), monomethylarsonate (MMA), and roxarsone in filtered natural-water samples are described. Various analytical methods can be used for the determination, depending on the arsenic species being determined. Arsenic concentration is determined by using inductively coupled plasma-mass spectrometry (ICP-MS) as an arsenic-specific detector for all methods. Laboratory-speciation methods are described that use an ion chromatographic column to separate the arsenic species; the column length, column packing, and mobile phase are dependent on the species of interest. Regardless of the separation technique, the arsenic species are introduced into plasma by eithe rpneumatic nebulization or arsine generation. Analysis times range from 2 to 8 minutes and method detection limits range from 0.1 to 0.6 microgram-arsenic per liter (ug-As/L), 10 to 60 picograms absolute (for a 100-microliter injection), depending on the arsenic species determined and the analytical method used. A field-generation specciation method also is described that uses a strong anion exchange cartridge to separate As(III) from As(V) in the field. As(III) in the eluate and the As(V) in the cartridge extract are determined by direct nebulization ICP-MS. Methylated arsenic species that also are retained on the cartridge will positively bias As(V) results without further laboratory separations. The method detection limit for field speciation is 0.3 ug-As/L. The distribution of arsenic species must be preserved in the field to eliminate changes caused by photochemical oxidation or metal oxyhydroxide precipitation. Preservation techniques, such as refrigeration, the addition of acides, or the additoin of ethylene-diaminetetraacetic acid (EDTA) and the effects of ambient light were tested. Of the preservatives evaluated, EDTA was found to work best with the laboratory- and field-speciation methods for all sample matrices tested. Storing the samples in opaque polytethylene bottles eliminated the effects of photochemical oxidation. The percentage change in As(III):As(V) ratios for an EDTA-preserved acid mine drainage (AMD) sample and ground-water sample during a 3-month period was -5 percent and +3 percent, respectively. The bias and variability of the methods were evaluated by comparing results for total arsenic and As(III), As(V), DMA, and MMA concentrations in ground water, AMD, and surface water. Seventy-one ground-water, 10 AMD, and 24 surface-water samples were analyzed. Concentrations in ground-water samples reached 720 ug-As/L for As(III) and 1080 ug-As/L for As(V); AMD samples reached 12800 ug-As/L for As(III) and 7050 ug-As/L for As(V); and surface-water samples reached 5 ug-As/L for As(III) and As(V). Inorganic arsenic species distribution in the samples ranged from 0 to 90 percent As(III). DMA and MMA were present only in surface-water samples from agricultural areas where the herbicide monosodium methylarsonate was applied; concentrations never exceeded 6 ug-As/L. Statistical analyses indicated that the difference between As(III) and As(V) concentrations for samples preserved with EDTA in opaque bottles and field-speciation results were analytically insignificant at the 95-percent confidence interval. There was no significant difference among the methods tested for total arsenic concentration. Percentage recovery for field samples spiked at 50 ug-As/L and analyzed by the laboratory-speciation method (n=2) ranged from 82 to 100 percent for As(III), 97 to 102 percent for As(V), 90 to 104 percent for DMA, and 81 to 96 percent for MMA; recoveries for samples spiked at 100 ug-As/L and analyzed by the field-speciation method ranged from 102 to 107 percent for As(III) and 105 to 106 percent for As(V). Laboratory-speciation results for Environment Canada reference material SLRS-2 closely matched reported concentrations. Laboratory-speciation metho

A novel method for rapid determination of total solid content in viscous liquids by multiple headspace extraction gas chromatography.

PubMed

Xin, Li-Ping; Chai, Xin-Sheng; Hu, Hui-Chao; Barnes, Donald G

2014-09-05

This work demonstrates a novel method for rapid determination of total solid content in viscous liquid (polymer-enriched) samples. The method is based multiple headspace extraction gas chromatography (MHE-GC) on a headspace vial at a temperature above boiling point of water. Thus, the trend of water loss from the tested liquid due to evaporation can be followed. With the limited MHE-GC testing (e.g., 5 extractions) and a one-point calibration procedure (i.e., recording the weight difference before and after analysis), the total amount of water in the sample can be determined, from which the total solid contents in the liquid can be calculated. A number of black liquors were analyzed by the new method which yielded results that closely matched those of the reference method; i.e., the results of these two methods differed by no more than 2.3%. Compared with the reference method, the MHE-GC method is much simpler and more practical. Therefore, it is suitable for the rapid determination of the solid content in many polymer-containing liquid samples. Copyright © 2014 Elsevier B.V. All rights reserved.

BEVACIZUMAB LEVELS IN BREAST MILK AFTER LONG-TERM INTRAVITREAL INJECTIONS.

PubMed

McFarland, Trevor J; Rhoads, Andrew D; Hartzell, Matthew; Emerson, Geoffrey G; Bhavsar, Abdhish R; Stout, J Timothy

2015-08-01

The purpose of this study is to determine whether bevacizumab is detectable in the breast milk of nursing mothers. Breast milk samples were collected from 2 patients receiving monthly intravitreal bevacizumab injections for choroidal neovascularization over the course of 16 months. Enzyme-linked immunosorbent assay and Western blot analysis was used to determine the levels of bevacizumab in the milk samples. An enzyme-linked immunosorbent assay was developed using antibodies specific to bevacizumab in which the sensitivity threshold was 3 ng/mL. All breast milk samples assayed from the two patients actively undergoing treatment did not have detectable levels of bevacizumab. Samples collected 1.5 hours and 7 hours after an injection and 2 randomly chosen samples were negative by Western blot analysis. A sensitive assay to detect bevacizumab in breast milk samples assayed suggests that intravitreal injections do not result in detectable bevacizumab in breast milk.

Magnetostrictive resonance excitation

DOEpatents

Schwarz, Ricardo B.; Kuokkala, Veli-Tapani

1992-01-01

The resonance frequency spectrum of a magnetostrictive sample is remotely determined by exciting the magnetostrictive property with an oscillating magnetic field. The permeability of a magnetostrictive material and concomitant coupling with a detection coil varies with the strain in the material whereby resonance responses of the sample can be readily detected. A suitable sample may be a magnetostrictive material or some other material having at least one side coated with a magnetostrictive material. When the sample is a suitable shape, i.e., a cube, rectangular parallelepiped, solid sphere or spherical shell, the elastic moduli or the material can be analytically determined from the measured resonance frequency spectrum. No mechanical transducers are required and the sample excitation is obtained without contact with the sample, leading to highly reproducible results and a measurement capability over a wide temperature range, e.g. from liquid nitrogen temperature to the Curie temperature of the magnetostrictive material.

Preliminary results of investigations into the use of artificial neural networks for discriminating gas chromatograph mass spectra of remote samples

NASA Technical Reports Server (NTRS)

Geller, Harold A.; Norris, Eugene; Warnock, Archibald, III

1991-01-01

Neural networks trained using mass spectra data from the National Institute of Standards and Technology (NIST) are studied. The investigations also included sample data from the gas chromatograph mass spectrometer (GCMS) instrument aboard the Viking Lander, obtained from the National Space Science Data Center. The work performed to data and the preliminary results from the training and testing of neural networks are described. These preliminary results are presented for the purpose of determining the viability of applying artificial neural networks in discriminating mass spectra samples from remote instrumentation such as the Mars Rover Sample Return Mission and the Cassini Probe.

A survey of rapid sample return needs from Space Station Freedom and potential return systems

NASA Technical Reports Server (NTRS)

Mccandless, Ronald S.; Siegel, Bette; Charlton, Kevin

1991-01-01

Results are presented of a survey conducted among potential users of the life sciences and material sciences facilities at the Space Station Freedom (SSF) to determine the need for a special rapid sample return (RSR) mission to bring the experimental samples from the Space Station Freedom (SSF) to earth between the Space Shuttle visits. The results of the survey show that, while some experimental objectives would benefit from the RSR capability, other available cost- and mission-effective means could be used instead of the RSR proposed. Potential vehicles for transporting samples from the SSF to earth are examined in the context of the survey results.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of low-level silver by graphite furnace atomic absorption spectrophotometry

USGS Publications Warehouse

Damrau, D.L.

1993-01-01

Increased awareness of the quality of water in the United States has led to the development of a method for determining low levels (0.2-5.0 microg/L) of silver in water samples. Use of graphite furnace atomic absorption spectrophotometry provides a sensitive, precise, and accurate method for determining low-level silver in samples of low ionic-strength water, precipitation water, and natural water. The minimum detection limit determined for low-level silver is 0.2 microg/L. Precision data were collected on natural-water samples and SRWS (Standard Reference Water Samples). The overall percent relative standard deviation for natural-water samples with silver concentrations more than 0.2 microg/L was less than 40 percent throughout the analytical range. For the SRWS with concentrations more than 0.2 microg/L, the overall percent relative standard deviation was less than 25 percent throughout the analytical range. The accuracy of the results was determined by spiking 6 natural-water samples with different known concentrations of the silver standard. The recoveries ranged from 61 to 119 percent at the 0.5-microg/L spike level. At the 1.25-microg/L spike level, the recoveries ranged from 92 to 106 percent. For the high spike level at 3.0 microg/L, the recoveries ranged from 65 to 113 percent. The measured concentrations of silver obtained from known samples were within the Branch of Quality Assurance accepted limits of 1 1/2 standard deviations on the basis of the SRWS program for Inter-Laboratory studies.

A new in-situ method to determine the apparent gas diffusion coefficient of soils

NASA Astrophysics Data System (ADS)

Laemmel, Thomas; Paulus, Sinikka; Schack-Kirchner, Helmer; Maier, Martin

2015-04-01

Soil aeration is an important factor for the biological activity in the soil and soil respiration. Generally, gas exchange between soil and atmosphere is assumed to be governed by diffusion and Fick's Law is used to describe the fluxes in the soil. The "apparent soil gas diffusion coefficient" represents the proportional factor between the flux and the gas concentration gradient in the soil and reflects the ability of the soil to "transport passively" gases through the soil. One common way to determine this coefficient is to take core samples in the field and determine it in the lab. Unfortunately this method is destructive and needs laborious field work and can only reflect a small fraction of the whole soil. As a consequence insecurity about the resulting effective diffusivity on the profile scale must remain. We developed a new in-situ method using new gas sampling device, tracer gas and inverse soil gas modelling. The gas sampling device contains several sampling depths and can be easily installed into vertical holes of an auger, which allows for fast installation of the system. At the lower end of the device inert tracer gas is injected continuously. The tracer gas diffuses into the surrounding soil. The resulting distribution of the tracer gas concentrations is used to deduce the diffusivity profile of the soil. For Finite Element Modeling of the gas sampling device/soil system the program COMSOL is used. We will present the results of a field campaign comparing the new in-situ method with lab measurements on soil cores. The new sampling pole has several interesting advantages: it can be used in-situ and over a long time; so it allows following modifications of diffusion coefficients in interaction with rain but also vegetation cycle and wind.

An independent determination of the local Hubble constant

NASA Astrophysics Data System (ADS)

Fernández Arenas, David; Terlevich, Elena; Terlevich, Roberto; Melnick, Jorge; Chávez, Ricardo; Bresolin, Fabio; Telles, Eduardo; Plionis, Manolis; Basilakos, Spyros

2018-02-01

The relationship between the integrated H β line luminosity and the velocity dispersion of the ionized gas of H II galaxies and giant H II regions represents an exciting standard candle that presently can be used up to redshifts z ˜ 4. Locally it is used to obtain precise measurements of the Hubble constant by combining the slope of the relation obtained from nearby (z ≤ 0.2) H II galaxies with the zero-point determined from giant H II regions belonging to an `anchor sample' of galaxies for which accurate redshift-independent distance moduli are available. We present new data for 36 giant H II regions in 13 galaxies of the anchor sample that includes the megamaser galaxy NGC 4258. Our data are the result of the first 4 yr of observation of our primary sample of 130 giant H II regions in 73 galaxies with Cepheid determined distances. Our best estimate of the Hubble parameter is 71.0 ± 2.8(random) ± 2.1(systematic) km s- 1Mpc- 1. This result is the product of an independent approach and, although at present less precise than the latest SNIa results, it is amenable to substantial improvement.

Potential for false positive HIV test results with the serial rapid HIV testing algorithm

PubMed Central

2012-01-01

Background Rapid HIV tests provide same-day results and are widely used in HIV testing programs in areas with limited personnel and laboratory infrastructure. The Uganda Ministry of Health currently recommends the serial rapid testing algorithm with Determine, STAT-PAK, and Uni-Gold for diagnosis of HIV infection. Using this algorithm, individuals who test positive on Determine, negative to STAT-PAK and positive to Uni-Gold are reported as HIV positive. We conducted further testing on this subgroup of samples using qualitative DNA PCR to assess the potential for false positive tests in this situation. Results Of the 3388 individuals who were tested, 984 were HIV positive on two consecutive tests, and 29 were considered positive by a tiebreaker (positive on Determine, negative on STAT-PAK, and positive on Uni-Gold). However, when the 29 samples were further tested using qualitative DNA PCR, 14 (48.2%) were HIV negative. Conclusion Although this study was not primarily designed to assess the validity of rapid HIV tests and thus only a subset of the samples were retested, the findings show a potential for false positive HIV results in the subset of individuals who test positive when a tiebreaker test is used in serial testing. These findings highlight a need for confirmatory testing for this category of individuals. PMID:22429706

Evaluation of Quality-Assurance/Quality-Control Data Collected by the U.S. Geological Survey from Wells and Springs between the Southern Boundary of the Idaho National Engineering and Environmental Laboratory and the Hagerman Area, Idaho, 1989 through 1995

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

Williams, L.M.; Bartholomay, R.C.; Campbell, L.J.

1998-10-01

The U.S. Geological (USGS) and the Idaho Department of Water Resources, in cooperation with the U.S. Department of Energy, collected and analyzed water samples to monitor the water quality of the Snake River Plain aquifer from the southern boundary of the Idaho National Engineering and Environmental Laboratory to the Hagerman area, Idaho. Concurrently, replicate samples and blank samples were collected and analyzed as part of the quality-assurance/quality-control program. Samples were analyzed from inorganic constituents, gross radioactivity and radionuclides, organic constituents, and stable isotopes. To evaluate the precision of field and laboratory methods, analytical results of the water-quality and replicate samplesmore » were compared statistically for equivalence on the basis of the precision associated with each result. Statistical comparisons of the data indicated that 95 percent of the results of the replicate pairs were equivalent. Blank-sample analytical results indicated th at the inorganic blank water and volatile organic compound blank water from the USGS National Water Quality Laboratory and the distilled water from the Idaho Department of Water Resources were suitable for blanks; blank water from other sources was not. Equipment-blank analytical results were evaluated to determine if a bias had been introduced and possible sources of bias. Most equipment blanks were analyzed for trace elements and volatile organic compounds; chloroform was found in one equipment blank. Two of the equipment blanks were prepared after collection and analyses of the water-quality samples to determine whether contamination had been introduced during the sampling process. Results of one blank indicated that a hose used to divert water away from pumps and electrical equipment had contaminated the samples with some volatile organic compounds. Results of the other equipment blank, from the apparatus used to filter dissolved organic carbon samples, indicated that the filtering apparatus did not affect water-quality samples.« less

Method of Analysis by the U.S. Geological Survey California District Sacramento Laboratory-- Determination of Dissolved Organic Carbon in Water by High Temperature Catalytic Oxidation, Method Validation, and Quality-Control Practices

USGS Publications Warehouse

Bird, Susan M.; Fram, Miranda S.; Crepeau, Kathryn L.

2003-01-01

An analytical method has been developed for the determination of dissolved organic carbon concentration in water samples. This method includes the results of the tests used to validate the method and the quality-control practices used for dissolved organic carbon analysis. Prior to analysis, water samples are filtered to remove suspended particulate matter. A Shimadzu TOC-5000A Total Organic Carbon Analyzer in the nonpurgeable organic carbon mode is used to analyze the samples by high temperature catalytic oxidation. The analysis usually is completed within 48 hours of sample collection. The laboratory reporting level is 0.22 milligrams per liter.

[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.

Interference modelling, experimental design and pre-concentration steps in validation of the Fenton's reagent for pesticides determination.

PubMed

Ostra, Miren; Ubide, Carlos; Zuriarrain, Juan

2007-02-12

The determination of atrazine in real samples (commercial pesticide preparations and water matrices) shows how the Fenton's reagent can be used with analytical purposes when kinetic methodology and multivariate calibration methods are applied. Also, binary mixtures of atrazine-alachlor and atrazine-bentazone in pesticide preparations have been resolved. The work shows the way in which interferences and the matrix effect can be modelled. Experimental design has been used to optimize experimental conditions, including the effect of solvent (methanol) used for extraction of atrazine from the sample. The determination of pesticides in commercial preparations was accomplished without any pre-treatment of sample apart from evaporation of solvent; the calibration model was developed for concentration ranges between 0.46 and 11.6 x 10(-5) mol L(-1) with mean relative errors under 4%. Solid-phase extraction is used for pre-concentration of atrazine in water samples through C(18) disks, and the concentration range for determination was established between 4 and 115 microg L(-1) approximately. Satisfactory results for recuperation of atrazine were always obtained.

Proton Induced X-Ray Emission (PIXE): Determining the Concentration of Samples

NASA Astrophysics Data System (ADS)

McCarthy, Mallory; Rodriguez Manso, Alis; Pajouhafsar, Yasmin; J Yennello, Sherry

2017-09-01

We used Proton Induced X-ray Emission (PIXE) as an analysis technique to determine the composition of samples, in particular, the elemental constituents and the concentrations. Each of the samples are bombarded with protons, which in result displaces a lower level electron and causes a higher level electron to fall into its place. This displacement produces characteristic x-rays that are `fingerprints' for each element. The protons supplied for the bombardment are produced and accelerated by the K150 proton beam in the Cyclotron Institute at Texas A&M University. The products are detected by three x-ray detectors: XR-100CR Si-PIN, XR-100SDD, and XR-100T CdTe. The peaks of the spectrum are analyzed using a software analysis tool, GUPIXWIN, to determine the concentration of the known elements of each particular sample. The goals of this work are to test run the Proton Induced X-Ray Emission experimental set up at Texas A&M University (TAMU) and to determine the concentration of thin films containing KBr given by the TAMU Chemical Engineering Department.

Measurement of urinary calcium using AT89C51RD2 microcontroller.

PubMed

Neelamegam, P; Jamaludeen, A; Rajendran, A; Raghunathan, R

2009-04-01

A simple and inexpensive absorption technique for determination of calcium ion in urine samples is developed, comprising a light emitting diode (650 nm) as the light source and photodiode as the detector with AT89C51RD2 microcontroller. The design of the system and details of interface, calibration, and procedure of operation are explained in this paper. Software is developed to monitor sample processing and to display the results in liquid crystal display screen. With 15 microl sample volume, a linear output is obtained in the range of 2.5-7.5 mM calcium with a detection limit of 0.06 mM. Interferences from other cations such as monovalent ion and divalent ion are investigated in the expected range, which are normally present in clinical samples, and absorption changes over the pH range of 3-12 are also determined. This system has been demonstrated successfully for the successive assay of calcium in urine samples, with the results comparing well to those achieved and in good agreement with values obtained with the current clinical spectrophotometric method at 95% of confidence level.

Determination of Microelements in Human Milk and Infant Formula Without Digestion by ICP-OES.

PubMed

Đurović, Dijana; Milisavljević, Branka; Nedović-Vuković, Mirjana; Potkonjak, Branislav; Spasić, Snežana; Vrvić, Miroslav

2017-06-01

The concentrations of zinc (Zn), iron (Fe) and copper (Cu) in both human milk and infant formula were determined using a new sample preparation method, by inductively coupled plasma - optical emission spectometry (ICP-OES) and flame atomic absorption spectrometry (FAAS). Human milk samples were diluted in ultrapure water. The infant formula of powder samples (suitable for an infant 1-6 months of age) and standard reference material (SRM-1849) were analyzed in parallel. The results have shown that FAAS method was more sensitive for Fe determination in human milk while ICP-OES was more sensitive for both Zn and Cu detection. The limit of quantification for both Zn and Cu was 5 μg L-1 and 10 μg L-1 for Fe and the recovery for Zn, Fe and Cu was ranged from 90% to 94%, 97% to 103% and 90% to 102%, respectively. Mean concentrations of Zn, Fe, and Cu in human milk samples were 5.35, 0.47 and 0.83 mg L-1, respectively while these values in infant formula were ranged from 3.52-4.75 mg L-1, 3.37-4.56 mg L-1 and 0.28-0.41 mg L-1, respectively. Despite the sample complexity, the proposed method using dilution of milk samples with water was simple, rapid, effective and accurate. ICP-OES was a better method for Zn determination while FAAS was a better method for Fe determination. In the case of Cu both methods were comparable.

Factorial design optimization of experimental variables in the on-line separation/preconcentration of copper in water samples using solid phase extraction and ICP-OES determination.

PubMed

Escudero, Luis A; Cerutti, S; Olsina, R A; Salonia, J A; Gasquez, J A

2010-11-15

An on-line preconcentration procedure using solid phase extraction (SPE) for the determination of copper in different water samples by inductively coupled plasma optical emission spectrometry (ICP-OES) is proposed. The copper was retained on a minicolumn filled with ethyl vinyl acetate (EVA) at pH 8.0 without using any complexing reagent. The experimental optimization step was performed using a two-level full factorial design. The results showed that pH, sample loading flow rate, and their interaction (at the tested levels) were statistically significant. In order to determine the best conditions for preconcentration and determination of copper, a final optimization of the significant factors was carried out using a central composite design (CCD). The calibration graph was linear with a regression coefficient of 0.995 at levels near the detection limit up to at least 300 μg L(-1). An enrichment factor (EF) of 54 with a preconcentration time of 187.5 s was obtained. The limit of detection (3σ) was 0.26 μg L(-1). The sampling frequency for the developed methodology was about 15 samples/h. The relative standard deviation (RSD) for six replicates containing 50 μg L(-1) of copper was 3.76%. The methodology was successfully applied to the determination of Cu in tap, mineral, river water samples, and in a certified VKI standard reference material. Copyright © 2010 Elsevier B.V. All rights reserved.

Assessing representativeness of sampling methods for reaching men who have sex with men: a direct comparison of results obtained from convenience and probability samples.

PubMed

Schwarcz, Sandra; Spindler, Hilary; Scheer, Susan; Valleroy, Linda; Lansky, Amy

2007-07-01

Convenience samples are used to determine HIV-related behaviors among men who have sex with men (MSM) without measuring the extent to which the results are representative of the broader MSM population. We compared results from a cross-sectional survey of MSM recruited from gay bars between June and October 2001 to a random digit dial telephone survey conducted between June 2002 and January 2003. The men in the probability sample were older, better educated, and had higher incomes than men in the convenience sample, the convenience sample enrolled more employed men and men of color. Substance use around the time of sex was higher in the convenience sample but other sexual behaviors were similar. HIV testing was common among men in both samples. Periodic validation, through comparison of data collected by different sampling methods, may be useful when relying on survey data for program and policy development.

Determining storm sampling requirements for improving precision of annual load estimates of nutrients from a small forested watershed.

PubMed

Ide, Jun'ichiro; Chiwa, Masaaki; Higashi, Naoko; Maruno, Ryoko; Mori, Yasushi; Otsuki, Kyoichi

2012-08-01

This study sought to determine the lowest number of storm events required for adequate estimation of annual nutrient loads from a forested watershed using the regression equation between cumulative load (∑L) and cumulative stream discharge (∑Q). Hydrological surveys were conducted for 4 years, and stream water was sampled sequentially at 15-60-min intervals during 24 h in 20 events, as well as weekly in a small forested watershed. The bootstrap sampling technique was used to determine the regression (∑L-∑Q) equations of dissolved nitrogen (DN) and phosphorus (DP), particulate nitrogen (PN) and phosphorus (PP), dissolved inorganic nitrogen (DIN), and suspended solid (SS) for each dataset of ∑L and ∑Q. For dissolved nutrients (DN, DP, DIN), the coefficient of variance (CV) in 100 replicates of 4-year average annual load estimates was below 20% with datasets composed of five storm events. For particulate nutrients (PN, PP, SS), the CV exceeded 20%, even with datasets composed of more than ten storm events. The differences in the number of storm events required for precise load estimates between dissolved and particulate nutrients were attributed to the goodness of fit of the ∑L-∑Q equations. Bootstrap simulation based on flow-stratified sampling resulted in fewer storm events than the simulation based on random sampling and showed that only three storm events were required to give a CV below 20% for dissolved nutrients. These results indicate that a sampling design considering discharge levels reduces the frequency of laborious chemical analyses of water samples required throughout the year.

Monitoring of uranium concentrations in water samples collected near potentially hazardous objects in North-West Tajikistan.

PubMed

Zoriy, P; Schläger, M; Murtazaev, K; Pillath, J; Zoriy, M; Heuel-Fabianek, B

2018-01-01

The water contamination near ecologically problematic objects was investigated between 2009 and 2014 in North-West Tajikistan as a part of a joint project between Forschungszentrum Jülich and Khujand State University. The main part of this work was the determination of uranium in water samples collected near the Degmay tailings dump, the Taboshar pit lake and the Syr Darya river. More than 130 water samples were collected and analyzed to monitor the uranium concentration near the investigated areas. Two different mass spectrometers and an ion chromatograph were used for element concentration measurements. Based on the results obtained, the uranium influence of the Degmay tailings on the rivers Khoja-Bakyrgan-Say and Syr Darya and surrounding water was not found. The uranium concentration in water samples was monitored for a lengthy period at seven locations Great differences in the uranium concentration in waters collected in 2010, 2011, 2012, 2013 for each location were not observed. Drinking water samples from the region of North-West Tajikistan were analyzed and compared with the World Health Organization's guidelines. Seven out of nine drinking water samples near Taboshar exceeded the WHO guideline value for uranium concentrations (30 μg/L). The average uranium concentration of water samples from Syr Darya for the period from 2009 to 2014 was determined to be 20.1 (±5.2) μg/L. The uranium contamination of the Syr Darya was determined from the western border to the eastern border and the results are shown in this paper. Copyright © 2017 Elsevier Ltd. All rights reserved.

Determination of drugs in surface water and wastewater samples by liquid chromatography-mass spectrometry: Methods and preliminary results including toxicity studies with Vibrio fischeri

USGS Publications Warehouse

Farre, M.; Ferrer, I.; Ginebreda, A.; Figueras, M.; Olivella, L.; Tirapu, L.; Vilanova, M.; Barcelo, D.

2001-01-01

In the present work a combined analytical method involving toxicity and liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) was developed for the determination of pharmaceutical compounds in water samples. The drugs investigated were the analgesics: ibuprofen, ketoprofen, naproxen, and diclofenac, the decomposition product of the acetyl salicylic acid: salicylic acid and one lipid lowering agent, gemfibrozil. The selected compounds are acidic substances, very polar and all of them are analgesic compounds that can be purchased without medical prescription. The developed protocol consisted, first of all, on the use Microtox?? and ToxAlert??100 toxicity tests with Vibrio fischeri for the different pharmaceutical drugs. The 50% effective concentration (EC50) values and the toxicity units (TU) were determined for every compound using both systems. Sample enrichment of water samples was achieved by solid-phase extraction procedure (SPE), using the Merck LiChrolut?? EN cartridges followed by LC-ESI-MS. Average recoveries loading 1 l of samples with pH=2 varied from 69 to 91% and the detection limits in the range of 15-56 ng/l. The developed method was applied to real samples from wastewater and surface-river waters of Catalonia (north-east of Spain). One batch of samples was analyzed in parallel also by High Resolution Gas Chromatography coupled with Mass Spectrometry (HRGC-MS) and the results have been compared with the LC-ESI-MS method developed in this work. ?? 2001 Elsevier Science B.V. All rights reserved.

Comparison of different methods to quantify fat classes in bakery products.

PubMed

Shin, Jae-Min; Hwang, Young-Ok; Tu, Ock-Ju; Jo, Han-Bin; Kim, Jung-Hun; Chae, Young-Zoo; Rhu, Kyung-Hun; Park, Seung-Kook

2013-01-15

The definition of fat differs in different countries; thus whether fat is listed on food labels depends on the country. Some countries list crude fat content in the 'Fat' section on the food label, whereas other countries list total fat. In this study, three methods were used for determining fat classes and content in bakery products: the Folch method, the automated Soxhlet method, and the AOAC 996.06 method. The results using these methods were compared. Fat (crude) extracted by the Folch and Soxhlet methods was gravimetrically determined and assessed by fat class using capillary gas chromatography (GC). In most samples, fat (total) content determined by the AOAC 996.06 method was lower than the fat (crude) content determined by the Folch or automated Soxhlet methods. Furthermore, monounsaturated fat or saturated fat content determined by the AOAC 996.06 method was lowest. Almost no difference was observed between fat (crude) content determined by the Folch method and that determined by the automated Soxhlet method for nearly all samples. In three samples (wheat biscuits, butter cookies-1, and chocolate chip cookies), monounsaturated fat, saturated fat, and trans fat content obtained by the automated Soxhlet method was higher than that obtained by the Folch method. The polyunsaturated fat content obtained by the automated Soxhlet method was not higher than that obtained by the Folch method in any sample. Copyright © 2012 Elsevier Ltd. All rights reserved.

Determination of Vanadium, Tin and Mercury in Atmospheric Particulate Matter and Cement Dust Samples by Direct Current Plasma Atomic Emission Spectrometry.

ERIC Educational Resources Information Center

Hindy, Kamal T.; And Others

1992-01-01

An atmospheric pollution study applies direct current plasma atomic emission spectrometry (DCP-AES) to samples of total suspended particulate matter collected in two industrial areas and one residential area, and cement dust collected near major cement factories. These samples were analyzed for vanadium, tin, and mercury. The results indicate the…

Estimating the probability that the sample mean is within a desired fraction of the standard deviation of the true mean.

PubMed

Schillaci, Michael A; Schillaci, Mario E

2009-02-01

The use of small sample sizes in human and primate evolutionary research is commonplace. Estimating how well small samples represent the underlying population, however, is not commonplace. Because the accuracy of determinations of taxonomy, phylogeny, and evolutionary process are dependant upon how well the study sample represents the population of interest, characterizing the uncertainty, or potential error, associated with analyses of small sample sizes is essential. We present a method for estimating the probability that the sample mean is within a desired fraction of the standard deviation of the true mean using small (n<10) or very small (n < or = 5) sample sizes. This method can be used by researchers to determine post hoc the probability that their sample is a meaningful approximation of the population parameter. We tested the method using a large craniometric data set commonly used by researchers in the field. Given our results, we suggest that sample estimates of the population mean can be reasonable and meaningful even when based on small, and perhaps even very small, sample sizes.

Factors of soil diversity in the Batumi delta (Georgia)

NASA Astrophysics Data System (ADS)

Turgut, Bülent; Ateş, Merve

2017-01-01

The aim of this study was to determine certain basic properties of soils in the Batumi delta (southwestern Georgia) to determine the relationships of studied properties and to identify differences with regards to these properties between different sampling sites in the delta that were selected based on the delta morphology. In this context, a total of 125 soil samples were collected from five different sampling sites, and the clay, silt and sand content of the samples were determined along with their mean weight diameter (MWD) values, aggregate stability (AS) values, amount of water retained under -33 (FC) and -1500 kPa (WP) pressure and organic matter (OM) content. Correlation analysis indicated that clay content and OM were positively correlated with MWD, and OM was positively correlated with AS. However, the sand content was found to be negatively correlated with MWD. In addition, clay, silt and OM content were positive correlated with FC and WP. Variance analysis results determined statistically significant differences between the sampling sites with respect to all of the evaluated properties. The active delta section of the study area was characterized by high sand content, while the lower delta plain was characterized by high OM and AS values, and the upper delta plain was characterized by high MWD values, high FC and WP moisture content levels and high clay and silt content. In conclusion, it was demonstrated that the examined properties were significantly affected by the different morphological positions and usages of these different areas. These results may help with the management of agricultural lands in the Batumi delta, which has never been studied before.

Spectrofluorimetric determination of cefixime using terbium-danofloxacin probe

PubMed Central

Manzoori, Jamshid L.; Amjadi, Mohammad; Soltani, Naser; Jouyban, Abolghasem

2014-01-01

Objective(s): Cefixime (Cfx), is a semi-synthetic third-generation oral cephalosporin antibiotic that is prescribed for the treatment of susceptible infections. There are some procedures for the determination of Cfx in pharmaceutical formulations and biological samples. Herein a spectrofluorimetric method was proposed for Cfx determination based on the fluorescence quenching of terbium-danofloxacin (Tb3+-Dano) in the presence of Cfx. Materials and Methods: Cfx was detected based on fluorescence quenching of terbium-danofloxacin (Tb3+-Dano) in the presence of Cfx with maximum excitation and emission wavelengths at 347 nm and 545 nm, respectively. The quenched fluorescence intensity of Tb3+- Dano system is proportional to the concentration of Cfx. The optimum conditions for the determination of Cfx were studied. Results: The maximum response was achieved under optimum conditions of [Tris buffer]= 0.008 mol/l (pH 6.5), [Tb3+]=1×10-4 mol/l and [Dano]=1×10-4 mol/l. The developed method was evaluated in terms of accuracy, precision and limit of detection. The linear concentration ranges for quantification of Cfx were 8.8×10-8-8.8×10-7 mol/l and 1.1×10-7-8.8×10-7 mol/l in standard and human serum samples with the detection limits (S/N=3) of 2.8×10-8 mol/l and 3.9×10-8 mol/l, respectively. The Cfx was determined in pharmaceutical tablets and spiked serum samples and the results were satisfactory. Conclusion: This method is simple, practical and relatively interference-free for determination of Cfx in pharmaceutical tablets and serum samples. PMID:24904718

FILTRATION OF GROUND WATER SAMPLES FOR METALS ANALYSIS

EPA Science Inventory

The filtration of a ground water samples with 0.45 um filters for determination of 'dissolved' metals is not only inaccurate for distinguishing between dissolved and particulate phases, but if used for estimates of mobile contaminant loading in a given aquifer, may result in sign...

Airborne concentrations of methylene diphenyl diisocyanate (MDI) in North American wood mills during the manufacturing of oriented strand board (OSB).

PubMed

Karoly, William J; Flatley, John J; Stevenson, Ralph D; Bowers, John D

2004-12-01

Air monitoring data were collected from industrial hygiene surveys over an 8-year period in oriented strand board (OSB) mills. Personal samples were taken to evaluate potential employee exposures to MDI. Area samples were taken to determine the effectiveness of control measures used in the mills to prevent fugitive emissions of wood dust, MDI, and MDI-coated wood dust from the OSB manufacturing process. Personal sampling results (578 samples covering 11 different job categories) ranged from 0.0002-0.524 mg/m3, with a GM = 0.001 and GSD = 3.71. Area sampling results (1657 samples covering 14 stationary locations in the mills) ranged from 0.0002-2.5 mg/m3, with a GM = 0.004 and GSD = 5.52. The statistical range of the data suggests high variability. While exposures to MDI above the established limits (0.051 mg/m3, 8-hour time-weighted average, 0.2 mg/m3, ceiling) can and do occur when engineering controls are not maintained and/or proper work practices and personal protective equipment are not followed/used for certain high exposure potential tasks, the data indicate that over 97% of the personal and 92% of the area sampling results are less than 0.051 mg/m3. Wipe testing was performed to determine the presence of removable, unreacted diisocyanates (NCO functional groups)from various surfaces. Positive results were found in about 13% of the wipe tests on surfaces confined to the blender, forming line, and hopper deck process areas.

Sampling for Air Chemical Emissions from the Life Sciences Laboratory II

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

Ballinger, Marcel Y.; Lindberg, Michael J.

Sampling for air chemical emissions from the Life Science Laboratory II (LSL-II) ventilation stack was performed in an effort to determine potential exposure of maintenance staff to laboratory exhaust on the building roof. The concern about worker exposure was raised in December 2015 and several activities were performed to assist in estimating exposure concentrations. Data quality objectives were developed to determine the need for and scope and parameters of a sampling campaign to measure chemical emissions from research and development activities to the outside air. The activities provided data on temporal variation of air chemical concentrations and a basis formore » evaluating calculated emissions. Sampling for air chemical emissions was performed in the LSL-II ventilation stack over the 6-week period from July 26 to September 1, 2016. A total of 12 sampling events were carried out using 16 sample media. Resulting analysis provided concentration data on 49 analytes. All results were below occupational exposure limits and most results were below detection limits. When compared to calculated emissions, only 5 of the 49 chemicals had measured concentrations greater than predicted. This sampling effort will inform other study components to develop a more complete picture of a worker’s potential exposure from LSL-II rooftop activities. Mixing studies were conducted to inform spatial variation in concentrations at other rooftop locations and can be used in conjunction with these results to provide temporal variations in concentrations for estimating the potential exposure to workers working in and around the LSL-II stack.« less

Contaminant concentration in environmental samples using LIBS and CF-LIBS

NASA Astrophysics Data System (ADS)

Pandhija, S.; Rai, N. K.; Rai, A. K.; Thakur, S. N.

2010-01-01

The present paper deals with the detection and quantification of toxic heavy metals like Cd, Co, Pb, Zn, Cr, etc. in environmental samples by using the technique of laser-induced breakdown spectroscopy (LIBS) and calibration-free LIBS (CF-LIBS). A MATLABTM program has been developed based on the CF-LIBS algorithm given by earlier workers and concentrations of pollutants present in industrial area soil have been determined. LIBS spectra of a number of certified reference soil samples with varying concentrations of toxic elements (Cd, Zn) have been recorded to obtain calibration curves. The concentrations of Cd and Zn in soil samples from the Jajmau area, Kanpur (India) have been determined by using these calibration curves and also by the CF-LIBS approach. Our results clearly demonstrate that the combination of LIBS and CF-LIBS is very useful for the study of pollutants in the environment. Some of the results have also been found to be in good agreement with those of ICP-OES.

Ion mobility spectrometry as a detector for molecular imprinted polymer separation and metronidazole determination in pharmaceutical and human serum samples.

PubMed

Jafari, M T; Rezaei, B; Zaker, B

2009-05-01

Application of ion mobility spectrometry (IMS) as the detection technique for a separation method based on molecular imprinted polymer (MIP) was investigated and evaluated for the first time. On the basis of the results obtained in this work, the MIP-IMS system can be used as a powerful technique for separation, preconcentration, and detection of the metronidazole drug in pharmaceutical and human serum samples. The method is exhaustively validated in terms of sensitivity, selectivity, recovery, reproducibility, and column capacity. The linear dynamic range of 0.05-70.00 microg/mL was obtained for the determination of metronidazole with IMS. The recovery of analyzed drug was calculated to be above 89%, and the relative standard deviation (RSD) was lower than 6% for all experiments. Various real samples were analyzed with the coupled techniques, and the results obtained revealed the efficient cleanup of the samples using MIP separation before the analysis by IMS as a detection technique.

Concentrations of tritium and strontium-90 in water from selected wells at the Idaho National Engineering Laboratory after purging one, two, and three borehole volumes

USGS Publications Warehouse

Bartholomay, R.C.

1993-01-01

Water from 11 wells completed in the Snake River Plain aquifer at the Idaho National Engineering Laboratory was sampled as part of the U.S. Geological Survey's quality assurance program to determine the effect of purging different borehole volumes on tritium and strontium-90 concentrations. Wells were selected for sampling on the basis of the length of time it took to purge a borehole volume of water. Samples were collected after purging one, two, and three borehole volumes. The U.S. Department of Energy's Radiological and Environmental Sciences Laboratory provided analytical services. Statistics were used to determine the reproducibility of analytical results. The comparison between tritium and strontium-90 concentrations after purging one and three borehole volumes and two and three borehole volumes showed that all but two sample pairs with defined numbers were in statistical agreement. Results indicate that concentrations of tritium and strontium-90 are not affected measurably by the number of borehole volumes purged.

Patulin and its dietary intake by fruit juice consumption in Iran.

PubMed

Rahimi, Ebrahim; Rezapoor Jeiran, Masoome

2015-01-01

A survey was conducted to determine levels and dietary intake of patulin (PAT) from fruit juices consumed in Iran. PAT content was determined using high performance liquid chromatography-diode array detection in 161 samples of fruit juices including apple, pineapple, pear, peach, pomegranate and white and red grape juices. Results revealed the presence of PAT in 16.1% of the samples examined, ranging from 5 to 190.7 µg/kg. Average and median PAT content in positive samples was 34.5 and 18.5 µg/kg, respectively. PAT concentration in 2.5% of the samples was higher than the maximum limit as set by European regulations for PAT in fruit products (50 µg/kg). Estimated daily intake of PAT by fruit juice was 16.4, 45.9 and 74.6 ng/kg bw/day for Iranian adults, children and babies, respectively. The results of this study showed that PAT does not seem to be a problem in fruit-based drinks commercialised in Iran, except for apple juice.

Quantitative enzyme-linked immunosorbent assay for determination of polychlorinated biphenyls in environmental soil and sediment samples.

PubMed

Johnson, J C; Van Emon, J M

1996-01-01

An enzyme-linked immunosorbent assay (ELISA) for the quantitative determination of Aroclors 1242, 1248, 1254, and 1260 in soil and sediments was developed and its performance compared with that of gas chromatography (GC). The detection limits for Aroclors 1242 and 1248 in soil are 10.5 and 9 ng/g, respectively. The assay linear dynamic range is 50-1333 ng/g. Cross-reactivity of the assay with 37 structurally related potential cocontaminants in environmental soil samples was examined; none of the chlorinated anisoles, benzenes, or phenols exhibited >3% cross-reactivity, with <0.1% cross-reactivity being the norm. Soil spike recoveries of 107% and 104% were obtained for Aroclors 1242 and 1248, respectively, for a spike level of 5 mg/kg, with corresponding relative standard deviations of 14% and 17%. One hundred forty-eight environmental soil, sediment, and paper pulp samples, obtained from two EPA listed Superfund sites, were analyzed by ELISA and standard GC methods. Samples were extracted for ELISA analysis by shaking with methanol. Additional extractions of the same samples were performed either with supercritical carbon dioxide or by Soxhlet extraction with methanol. ELISA results for both the supercritical fluid and the Soxhlet extracts were in close agreement with the GC results, while the ELISA results for the methanol shake extracts were not. The data for the environmental samples demonstrated the capability of the ELISA to provide accurate results and reinforced the dependence of any detection method, including ELISA, on appropriate extraction procedures.

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.

Trace metal assay of U(3)O(8) powder by electrothermal AAS.

PubMed

Page, A G; Godbole, S V; Kulkarni, M J; Porwal, N K; Shelar, S S; Joshi, B D

1983-10-01

Methods have been developed for the direct determination of Ag, Ca, K., Li, Mg, Na, Pb, Sn and Zn in U(3)O(8) powder samples by electrothermal AAS. Nanogram and lower amounts of these elements have been determined with a relative standard deviation of 6-16% in mg amounts of sample (either alone or mixed with an equal weight of graphite). The results for NBL reference samples were in reasonable agreement with the certified values. X-Ray diffraction studies on the residues left from the graphite mixtures after the atomization cycle, confirmed the formation of uranium carbide (UC(2)).

Methods for collection and analysis of water samples

USGS Publications Warehouse

Rainwater, Frank Hays; Thatcher, Leland Lincoln

1960-01-01

This manual contains methods used by the U.S. Geological Survey to collect, preserve, and analyze water samples. Throughout, the emphasis is on obtaining analytical results that accurately describe the chemical composition of the water in situ. Among the topics discussed are selection of sampling sites, frequency of sampling, field equipment, preservatives and fixatives, analytical techniques of water analysis, and instruments. Seventy-seven laboratory and field procedures are given for determining fifty-three water properties.

Analysis of Sample Size, Counting Time, and Plot Size from an Avian Point Count Survey on Hoosier National Forest, Indiana

Treesearch

Frank R. Thompson; Monica J. Schwalbach

1995-01-01

We report results of a point count survey of breeding birds on Hoosier National Forest in Indiana. We determined sample size requirements to detect differences in means and the effects of count duration and plot size on individual detection rates. Sample size requirements ranged from 100 to >1000 points with Type I and II error rates of <0.1 and 0.2. Sample...

Application of factor analysis of infrared spectra for quantitative determination of beta-tricalcium phosphate in calcium hydroxylapatite.

PubMed

Arsenyev, P A; Trezvov, V V; Saratovskaya, N V

1997-01-01

This work represents a method, which allows to determine phase composition of calcium hydroxylapatite basing on its infrared spectrum. The method uses factor analysis of the spectral data of calibration set of samples to determine minimal number of factors required to reproduce the spectra within experimental error. Multiple linear regression is applied to establish correlation between factor scores of calibration standards and their properties. The regression equations can be used to predict the property value of unknown sample. The regression model was built for determination of beta-tricalcium phosphate content in hydroxylapatite. Statistical estimation of quality of the model was carried out. Application of the factor analysis on spectral data allows to increase accuracy of beta-tricalcium phosphate determination and expand the range of determination towards its less concentration. Reproducibility of results is retained.

Methods for determination of inorganic substances in water and fluvial sediments

USGS Publications Warehouse

Fishman, Marvin J.; Friedman, Linda C.

1989-01-01

Chapter Al of the laboratory manual contains methods used by the U.S. Geological Survey to analyze samples of water, suspended sediments, and bottom material for their content of inorganic constituents. Included are methods for determining the concentration of dissolved constituents in water, the total recoverable and total of constituents in water-suspended sediment samples, and the recoverable and total concentrations of constituents in samples of bottom material. The introduction to the manual includes essential definitions and a brief discussion of the use of significant figures in calculating and reporting analytical results. Quality control in the water-analysis laboratory is discussed, including the accuracy and precision of analyses, the use of standard-reference water samples, and the operation of an effective quality-assurance program. Methods for sample preparation and pretreatment are given also. A brief discussion of the principles of the analytical techniques involved and their particular application to water and sediment analysis is presented. The analytical methods of these techniques are arranged alphabetically by constituent. For each method, the general topics covered are the application, the principle of the method, the interferences, the apparatus and reagents required, a detailed description of the analytical procedure, reporting results, units and significant figures, and analytical precision data, when available. More than 126 methods are given for the determination of 70 inorganic constituents and physical properties of water, suspended sediment, and bottom material.

Methods for determination of inorganic substances in water and fluvial sediments

USGS Publications Warehouse

Fishman, Marvin J.; Friedman, Linda C.

1985-01-01

Chapter Al of the laboratory manual contains methods used by the Geological Survey to analyze samples of water, suspended sediments, and bottom material for their content of inorganic constituents. Included are methods for determining the concentration of dissolved constituents in water, total recoverable and total of constituents in water-suspended sediment samples, and recoverable and total concentrations of constituents in samples of bottom material. Essential definitions are included in the introduction to the manual, along with a brief discussion of the use of significant figures in calculating and reporting analytical results. Quality control in the water-analysis laboratory is discussed, including accuracy and precision of analyses, the use of standard reference water samples, and the operation of an effective quality assurance program. Methods for sample preparation and pretreatment are given also.A brief discussion of the principles of the analytical techniques involved and their particular application to water and sediment analysis is presented. The analytical methods involving these techniques are arranged alphabetically according to constituent. For each method given, the general topics covered are application, principle of the method, interferences, apparatus and reagents required, a detailed description of the analytical procedure, reporting results, units and significant figures, and analytical precision data, when available. More than 125 methods are given for the determination of 70 different inorganic constituents and physical properties of water, suspended sediment, and bottom material.

An anthropometric analysis of Korean male helicopter pilots for helicopter cockpit design.

PubMed

Lee, Wonsup; Jung, Kihyo; Jeong, Jeongrim; Park, Jangwoon; Cho, Jayoung; Kim, Heeeun; Park, Seikwon; You, Heecheon

2013-01-01

This study measured 21 anthropometric dimensions (ADs) of 94 Korean male helicopter pilots in their 20s to 40s and compared them with corresponding measurements of Korean male civilians and the US Army male personnel. The ADs and the sample size of the anthropometric survey were determined by a four-step process: (1) selection of ADs related to helicopter cockpit design, (2) evaluation of the importance of each AD, (3) calculation of required sample sizes for selected precision levels and (4) determination of an appropriate sample size by considering both the AD importance evaluation results and the sample size requirements. The anthropometric comparison reveals that the Korean helicopter pilots are larger (ratio of means = 1.01-1.08) and less dispersed (ratio of standard deviations = 0.71-0.93) than the Korean male civilians and that they are shorter in stature (0.99), have shorter upper limbs (0.89-0.96) and lower limbs (0.93-0.97), but are taller on sitting height, sitting eye height and acromial height (1.01-1.03), and less dispersed (0.68-0.97) than the US Army personnel. The anthropometric characteristics of Korean male helicopter pilots were compared with those of Korean male civilians and US Army male personnel. The sample size determination process and the anthropometric comparison results presented in this study are useful to design an anthropometric survey and a helicopter cockpit layout, respectively.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; comparison of a nitric acid in-bottle digestion procedure to other whole-water digestion procedures

USGS Publications Warehouse

Garbarino, John R.; Hoffman, Gerald L.

1999-01-01

A hydrochloric acid in-bottle digestion procedure is used to partially digest wholewater samples prior to determining recoverable elements by various analytical methods. The use of hydrochloric acid is problematic for some methods of analysis because of spectral interference. The inbottle digestion procedure has been modified to eliminate such interference by using nitric acid instead of hydrochloric acid in the digestion. Implications of this modification are evaluated by comparing results for a series of synthetic whole-water samples. Results are also compared with those obtained by using U.S. Environmental Protection Agency (1994) (USEPA) Method 200.2 total-recoverable digestion procedure. Percentage yields that use the nitric acid inbottle digestion procedure are within 10 percent of the hydrochloric acid in-bottle yields for 25 of the 26 elements determined in two of the three synthetic whole-water samples tested. Differences in percentage yields for the third synthetic whole-water sample were greater than 10 percent for 16 of the 26 elements determined. The USEPA method was the most rigorous for solubilizing elements from particulate matter in all three synthetic whole-water samples. Nevertheless, the variability in the percentage yield by using the USEPA digestion procedure was generally greater than the in-bottle digestion procedure, presumably because of the difficulty in controlling the digestion conditions accurately.

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.

Construction ages of the Upton Stone Chamber: Preliminary findings and suggestions for future luminescence research

USGS Publications Warehouse

Mahan, Shannon; Martin, Frederick; Taylor, Cathy

2015-01-01

The Upton Chamber in Massachusetts, an earth-covered stone structure 3.4 meters (m) in diameter, with a corbelled stone dome, and a 4.3 m long entrance passageway, is studied with the aim of determining whether optically stimulated luminescence (OSL) dating methods can be used to establish the approximate construction date of the entranceway. Three samples, taken from soil behind the lowest stones in the wall of the entrance passageway, returned OSL ages between 385 and 660 years ago (or from 1625 A.D. to 1350 A.D.; using the year 2011 as the 0 year). One sample, taken below the bottom of the artifact layers in an archeological test pit in front of the chamber entrance, returned OSL ages between 650 and 880 years ago. A modern sample collected from a nearby fluvial channel returned an age between 55 and 175 years. The Upton Chamber OSL sampling results are challenging to interpret because there are mixtures in the samples of both younger and older grains that likely result from human modification, root or soil processes, animal bioturbation (i.e. ants and worms), and/or partial bleaching. The ages were determined using the lowest component of the finite mixture model as applied to a distribution of quartz grains. Further research may enable us to determine whether older components are of anthropomorphic or geological origin.

Development of an analytical method for crystalline content determination in amorphous solid dispersions produced by hot-melt extrusion using transmission Raman spectroscopy: A feasibility study.

PubMed

Netchacovitch, L; Dumont, E; Cailletaud, J; Thiry, J; De Bleye, C; Sacré, P-Y; Boiret, M; Evrard, B; Hubert, Ph; Ziemons, E

2017-09-15

The development of a quantitative method determining the crystalline percentage in an amorphous solid dispersion is of great interest in the pharmaceutical field. Indeed, the crystalline Active Pharmaceutical Ingredient transformation into its amorphous state is increasingly used as it enhances the solubility and bioavailability of Biopharmaceutical Classification System class II drugs. One way to produce amorphous solid dispersions is the Hot-Melt Extrusion (HME) process. This study reported the development and the comparison of the analytical performances of two techniques, based on backscattering and transmission Raman spectroscopy, determining the crystalline remaining content in amorphous solid dispersions produced by HME. Principal Component Analysis (PCA) and Partial Least Squares (PLS) regression were performed on preprocessed data and tended towards the same conclusions: for the backscattering Raman results, the use of the DuoScan™ mode improved the PCA and PLS results, due to a larger analyzed sampling volume. For the transmission Raman results, the determination of low crystalline percentages was possible and the best regression model was obtained using this technique. Indeed, the latter acquired spectra through the whole sample volume, in contrast with the previous surface analyses performed using the backscattering mode. This study consequently highlighted the importance of the analyzed sampling volume. Copyright © 2017 Elsevier B.V. All rights reserved.

Summary of the U.S. Geological Survey National Field Quality Assurance Program from 1979 through 1997

USGS Publications Warehouse

Stanley, D.L.; Boozer, T.M.; Schroder, L.J.

1998-01-01

Since the inception of the U.S. Geological Survey National Field Quality Assurance Program, over 85,000 proficiency samples have been analyzed by water-quality analysts. This includes more than 10,000 alkalinity samples, more than 15,000 pH samples, and more than 16,000 specific conductance samples, which were analyzed from 1990 through 1997, and a total of more than 43,000 proficiency samples analyzed from 1979 through 1989. The analyte values were evaluated to determine the fourth-spread, a measure of the width of the middle half of the data, and the F-pseudosigma, a robust replacement for the standard deviation, for each of the different measurement ranges. The result of the statistical evaluation showed that the vast majority of reference sample measurements made by water-quality analysts were within acceptable ranges. From 1990 to 1997, the measurement of pH had the highest level of acceptable results, 98.4 percent, followed by specific conductance with 95.2 percent acceptable results, and alkalinity with 88.6 percent acceptable results. The statistical summary of pH indicates the calculated fourth-spread values for the entire tested range is +0.06 pH units. For specific conductance, the magnitude of the fourth-spread increases as the magnitude of the specific conductance ranges increases. The average relative fourth-spread percent for all reported specific conductance values is +1.8 percent. From 1990 through 1997, the evaluation of the results for alkalinity measurement for the average fourth-spread was determined to be + 3.3 milligrams per liter as calcium carbonate.

[GSTP1, APC and RASSF1 gene methylation in prostate cancer samples: comparative analysis of MS-HRM method and Infinium HumanMethylation450 BeadChip beadchiparray diagnostic value].

PubMed

Skorodumova, L O; Babalyan, K A; Sultanov, R; Vasiliev, A O; Govorov, A V; Pushkar, D Y; Prilepskaya, E A; Danilenko, S A; Generozov, E V; Larin, A K; Kostryukova, E S; Sharova, E I

2016-11-01

There is a clear need in molecular markers for prostate cancer (PC) risk stratification. Alteration of DNA methylation is one of processes that occur during ÐÑ progression. Methylation-sensitive PCR with high resolution melting curve analysis (MS-HRM) can be used for gene methylation analysis in routine laboratory practice. This method requires very small amounts of DNA for analysis. Numerous results have been accumulated on DNA methylation in PC samples analyzed by the Infinium HumanMethylation450 BeadChip (HM450). However, the consistency of MS-HRM results with chip hybridization results has not been examined yet. The aim of this study was to assess the consistency of results of GSTP1, APC and RASSF1 gene methylation analysis in ÐÑ biopsy samples obtained by MS-HRM and chip hybridization. The methylation levels of each gene determined by MS-HRM were statistically different in the group of PC tissue samples and the samples without signs of tumor growth. Chip hybridization data analysis confirmed the results obtained with the MS-HRM. Differences in methylation levels between tumor tissue and histologically intact tissue of each sample determined by MS-HRM and chip hybridization, were consistent with each other. Thus, we showed that the assessment of GSTP1, APC and RASSF1 gene methylation analysis using MS-HRM is suitable for the design of laboratory assays that will differentiate the PC tissue from the tissue without signs of tumor growth.

Neutron activation analysis for antimetabolites. [in food samples

NASA Technical Reports Server (NTRS)

1973-01-01

Determination of metal ion contaminants in food samples is studied. A weighed quantity of each sample was digested in a concentrated mixture of nitric, hydrochloric and perchloric acids to affect complete solution of the food products. The samples were diluted with water and the pH adjusted according to the specific analysis performed. The samples were analyzed by neutron activation analysis, polarography, and atomic absorption spectrophotometry. The solid food samples were also analyzed by neutron activation analysis for increased sensitivity and lower levels of detectability. The results are presented in tabular form.

Technical note: Alternatives to reduce adipose tissue sampling bias.

PubMed

Cruz, G D; Wang, Y; Fadel, J G

2014-10-01

Understanding the mechanisms by which nutritional and pharmaceutical factors can manipulate adipose tissue growth and development in production animals has direct and indirect effects in the profitability of an enterprise. Adipocyte cellularity (number and size) is a key biological response that is commonly measured in animal science research. The variability and sampling of adipocyte cellularity within a muscle has been addressed in previous studies, but no attempt to critically investigate these issues has been proposed in the literature. The present study evaluated 2 sampling techniques (random and systematic) in an attempt to minimize sampling bias and to determine the minimum number of samples from 1 to 15 needed to represent the overall adipose tissue in the muscle. Both sampling procedures were applied on adipose tissue samples dissected from 30 longissimus muscles from cattle finished either on grass or grain. Briefly, adipose tissue samples were fixed with osmium tetroxide, and size and number of adipocytes were determined by a Coulter Counter. These results were then fit in a finite mixture model to obtain distribution parameters of each sample. To evaluate the benefits of increasing number of samples and the advantage of the new sampling technique, the concept of acceptance ratio was used; simply stated, the higher the acceptance ratio, the better the representation of the overall population. As expected, a great improvement on the estimation of the overall adipocyte cellularity parameters was observed using both sampling techniques when sample size number increased from 1 to 15 samples, considering both techniques' acceptance ratio increased from approximately 3 to 25%. When comparing sampling techniques, the systematic procedure slightly improved parameters estimation. The results suggest that more detailed research using other sampling techniques may provide better estimates for minimum sampling.

Establishment and characterization of a new and stable collagen-binding assay for the assessment of von Willebrand factor activity

PubMed Central

Ni, Y; Nesrallah, J; Agnew, M; Geske, F J; Favaloro, E J

2013-01-01

Introduction Laboratory diagnosis of von Willebrand disease (VWD) requires determination of both von Willebrand factor (VWF) protein levels and activity. Current VWF activity tests include the ristocetin cofactor assay and the collagen-binding assay (VWF:CB). The goal of this investigation is to characterize a new collagen-binding assay and to determine its effectiveness in identifying VWD. Methods Analytical studies were carried out to characterize the performance of a new VWF:CB ELISA. Additionally, samples from a normal population were tested as were well-characterized type 1 and type 2 VWD samples. Results Repeatability and within-laboratory precision studies resulted in coefficients of variation (CVs) of ≤11%. A linear range of 1–354% (0.01–3.54 IU/mL) was determined, along with a limit of detection and a lower limit of quantitation of 1.6% and 4.0% (0.016 and 0.04 IU/mL), respectively. Samples tested from apparently healthy individuals resulted in a normal range of 54–217% (0.54–2.17 IU/mL). Known VWD type 1 and type 2 samples were also analyzed by the ELISA, with 99% of samples having VWF:CB below the normal reference range and an estimated 96% sensitivity and 87% specificity using a VWF collagen-binding/antigen cutoff ratio of 0.50. Conclusion This new VWF:CB ELISA provides an accurate measure of collagen-binding activity that aids in the diagnosis and differentiation of type 1 from type 2 VWD. PMID:23107512

Diverse Protocols for Correlative Super-Resolution Fluorescence Imaging and Electron Microscopy of Cells and Tissue

DTIC Science & Technology

2016-05-25

tissue is critical to biology. Many factors determine optimal experimental design, including attainable localization precision, ultrastructural...both imaging modalities. Examples include: weak tissue preservation protocols resulting in poor ultrastructure, e.g. mitochondrial cristae membranes...tension effects during sample drying that may result in artifacts44. Samples dried in the presence of polyvinyl alcohol do not have the haziness

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.

Sampling Strategies and Processing of Biobank Tissue Samples from Porcine Biomedical Models.

PubMed

Blutke, Andreas; Wanke, Rüdiger

2018-03-06

In translational medical research, porcine models have steadily become more popular. Considering the high value of individual animals, particularly of genetically modified pig models, and the often-limited number of available animals of these models, establishment of (biobank) collections of adequately processed tissue samples suited for a broad spectrum of subsequent analyses methods, including analyses not specified at the time point of sampling, represent meaningful approaches to take full advantage of the translational value of the model. With respect to the peculiarities of porcine anatomy, comprehensive guidelines have recently been established for standardized generation of representative, high-quality samples from different porcine organs and tissues. These guidelines are essential prerequisites for the reproducibility of results and their comparability between different studies and investigators. The recording of basic data, such as organ weights and volumes, the determination of the sampling locations and of the numbers of tissue samples to be generated, as well as their orientation, size, processing and trimming directions, are relevant factors determining the generalizability and usability of the specimen for molecular, qualitative, and quantitative morphological analyses. Here, an illustrative, practical, step-by-step demonstration of the most important techniques for generation of representative, multi-purpose biobank specimen from porcine tissues is presented. The methods described here include determination of organ/tissue volumes and densities, the application of a volume-weighted systematic random sampling procedure for parenchymal organs by point-counting, determination of the extent of tissue shrinkage related to histological embedding of samples, and generation of randomly oriented samples for quantitative stereological analyses, such as isotropic uniform random (IUR) sections generated by the "Orientator" and "Isector" methods, and vertical uniform random (VUR) sections.

Survivability of porcine epidemic diarrhea virus (PEDV) in bovine plasma submitted to spray drying processing and held at different time by temperature storage conditions.

PubMed

Pujols, Joan; Segalés, Joaquim

2014-12-05

Bovine plasma was inoculated with porcine epidemic diarrhea virus (PEDV) at an average final titer of 4.2 log10 TCID50/mL to determine the effect of spray drying on viral inactivation. Using a laboratory scale drier, inoculated plasma was spray dried at 200 °C inlet temperature and either 70 or 80 °C throughout substance. Both liquid and dried samples were subjected to three passages on VERO cell monolayers to determine PEDV infectivity. Results indicated liquid samples contained infective virus, but none of the spray dried samples were infectious. Also, survivability of PEDV inoculated on spray dried bovine plasma (SDBP) and stored at 4, 12 or 22 °C was determined for 7, 14 and 21 days. Commercial SDBP powder was inoculated with PEDV to an average final titer of 2.8 log10 TCID50/g. Five samples per time and temperature conditions were subjected to three passages on VERO cell monolayers to determine PEDV infectivity. The virus was non-infectious for all samples stored at 22 °C at 7, 14 and 21 days. PEDV was infective in 1 out of 5 samples stored at 12 °C at 7 days, but none of the samples stored for 14 and 21 days were infectious in cell culture. For samples stored at 4 °C, 4 out of 5 samples were infectious at 7 days, 1 out of 5 samples were infectious at 14 days, but none were infectious at 21 days. In summary, PEDV was not infectious on cell culture within 7 days when stored at room temperature and within 21 days when stored at refrigerated temperature. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of the liquidus temperature of tin using the heat pulse-based melting and comparison with traditional methods

NASA Astrophysics Data System (ADS)

Joung, Wukchul; Park, Jihye; Pearce, Jonathan V.

2018-06-01

In this work, the liquidus temperature of tin was determined by melting the sample using the pressure-controlled loop heat pipe. Square wave-type pressure steps generated periodic 0.7 °C temperature steps in the isothermal region in the vicinity of the tin sample, and the tin was melted with controllable heat pulses from the generated temperature changes. The melting temperatures at specific melted fractions were measured, and they were extrapolated to the melted fraction of unity to determine the liquidus temperature of tin. To investigate the influence of the impurity distribution on the melting behavior, a molten tin sample was solidified by an outward slow freezing or by quenching to segregate the impurities inside the sample with concentrations increasing outwards or to spread the impurities uniformly, respectively. The measured melting temperatures followed the local solidus temperature variations well in the case of the segregated sample and stayed near the solidus temperature in the quenched sample due to the microscopic melting behavior. The extrapolated melting temperatures of the segregated and quenched samples were 0.95 mK and 0.49 mK higher than the outside-nucleated freezing temperature of tin (with uncertainties of 0.15 mK and 0.16 mK, at approximately 95% level of confidence), respectively. The extrapolated melting temperature of the segregated sample was supposed to be a closer approximation to the liquidus temperature of tin, whereas the quenched sample yielded the possibility of a misleading extrapolation to the solidus temperature. Therefore, the determination of the liquidus temperature could result in different extrapolated melting temperatures depending on the way the impurities were distributed within the sample, which has implications for the contemporary methodology for realizing temperature fixed points of the International Temperature Scale of 1990 (ITS-90).

Occurrence and structural characterization of gas hydrates associated with a cold vent field, offshore Vancouver Island

NASA Astrophysics Data System (ADS)

Lu, Hailong; Moudrakovski, Igor; Riedel, Michael; Spence, George; Dutrisac, Regent; Ripmeester, John; Wright, Fred; Dallimore, Scott

2005-10-01

Gas hydrate samples recovered from a cold vent field offshore Vancouver Island were studied in detail both by macroscopic observations and instrumental methods (powder X-ray diffraction method (PXRD), nuclear magnetic resonance (NMR), and Raman spectroscopy). It was found that gas hydrates were massive from 2.64 to 2.94 m below seafloor (mbsf), elongated, nodular and tabular from 4.60 to 4.81 mbsf, and vein-like from 5.48 to 5.68 mbsf, showing a trend of decreasing hydrate content with increasing depth. All samples were determined to be structure I hydrate from PXRD, NMR, and Raman spectroscopies. The hydration numbers were estimated to be 6.1 ± 0.2 on average as determined from the methane distribution over the cage sites from NMR and Raman analytical results. Estimates of conversion levels indicated that ˜78% of the water in the massive samples was hydrate, down to a low value of ˜0.4% for the pore hydrate samples. The results are compared with measurements on synthetic hydrates and samples recovered from below the permafrost on the Mallik site. Differences in methane content and lattice parameters for synthetic and natural samples are relatively minor. Additional work is needed to address the presence of minor gas components and the heterogeneity of natural hydrate samples.

Comparing near-infrared conventional diffuse reflectance spectroscopy and hyperspectral imaging for determination of the bulk properties of solid samples by multivariate regression: determination of Mooney viscosity and plasticity indices of natural rubber.

PubMed

Juliano da Silva, Carlos; Pasquini, Celio

2015-01-21

Conventional reflectance spectroscopy (NIRS) and hyperspectral imaging (HI) in the near-infrared region (1000-2500 nm) are evaluated and compared, using, as the case study, the determination of relevant properties related to the quality of natural rubber. Mooney viscosity (MV) and plasticity indices (PI) (PI0 - original plasticity, PI30 - plasticity after accelerated aging, and PRI - the plasticity retention index after accelerated aging) of rubber were determined using multivariate regression models. Two hundred and eighty six samples of rubber were measured using conventional and hyperspectral near-infrared imaging reflectance instruments in the range of 1000-2500 nm. The sample set was split into regression (n = 191) and external validation (n = 95) sub-sets. Three instruments were employed for data acquisition: a line scanning hyperspectral camera and two conventional FT-NIR spectrometers. Sample heterogeneity was evaluated using hyperspectral images obtained with a resolution of 150 × 150 μm and principal component analysis. The probed sample area (5 cm(2); 24,000 pixels) to achieve representativeness was found to be equivalent to the average of 6 spectra for a 1 cm diameter probing circular window of one FT-NIR instrument. The other spectrophotometer can probe the whole sample in only one measurement. The results show that the rubber properties can be determined with very similar accuracy and precision by Partial Least Square (PLS) regression models regardless of whether HI-NIR or conventional FT-NIR produce the spectral datasets. The best Root Mean Square Errors of Prediction (RMSEPs) of external validation for MV, PI0, PI30, and PRI were 4.3, 1.8, 3.4, and 5.3%, respectively. Though the quantitative results provided by the three instruments can be considered equivalent, the hyperspectral imaging instrument presents a number of advantages, being about 6 times faster than conventional bulk spectrometers, producing robust spectral data by ensuring sample representativeness, and minimizing the effect of the presence of contaminants.

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

Egorov, Oleg; O'Hara, Matthew J.; Grate, Jay W.

An automated fluidic instrument is described that rapidly determines the total 99Tc content of aged nuclear waste samples, where the matrix is chemically and radiologically complex and the existing speciation of the 99Tc is variable. The monitor links microwave-assisted sample preparation with an automated anion exchange column separation and detection using a flow-through solid scintillator detector. The sample preparation steps acidify the sample, decompose organics, and convert all Tc species to the pertechnetate anion. The column-based anion exchange procedure separates the pertechnetate from the complex sample matrix, so that radiometric detection can provide accurate measurement of 99Tc. We developed amore » preprogrammed spike addition procedure to automatically determine matrix-matched calibration. The overall measurement efficiency that is determined simultaneously provides a self-diagnostic parameter for the radiochemical separation and overall instrument function. Continuous, automated operation was demonstrated over the course of 54 h, which resulted in the analysis of 215 samples plus 54 hly spike-addition samples, with consistent overall measurement efficiency for the operation of the monitor. A sample can be processed and measured automatically in just 12.5 min with a detection limit of 23.5 Bq/mL of 99Tc in low activity waste (0.495 mL sample volume), with better than 10% RSD precision at concentrations above the quantification limit. This rapid automated analysis method was developed to support nuclear waste processing operations planned for the Hanford nuclear site.« less

Simultaneous determination of potassium and total fluoride in toothpastes using a SIA system with two potentiometric detectors.

PubMed

Pérez-Olmos, R; Soto, J C; Zárate, N; Díez, I

2008-05-12

A sequential injection analysis (SIA) system has been developed for the first time to quantify potassium and total fluoride in toothpastes and gels used to prevent both dentinal hypersensitivity and dental caries. To enable this simultaneous determination, potentiometric detection, using a conventional fluoride electrode and a tubular potassium selective electrode, formed by a PVC membrane containing valinomycin as ionophore, was carried out. A manifold that uses a three-way solenoid valve was designed. The former under binary sampling conditions, provides reproducible mixing ratios of two solutions. This fact facilitates that the system automatically generates, on-line, the calibration curves required by the analytical procedure. The calibration ranged from 1.0 x 10(-4) to 1.0 x 10(-3) mol L(-1) for both potassium and total fluoride determinations. The R.S.D. (11 readings) resulted to be less than 1.5% for both determinations. Off-line studies related to the dissolution of the solid samples, the transformation of monofluorophosphate in fluoride, the elimination of organic matrix interference onto the plastic membrane of the potassium electrode, and the selection of the most adequate TISAB solution for fluoride determination, were also considered. A sampling rate of 18 samples h(-1) for both determinations was attained, their precisions and accuracies being statistically indistinguishable from those achieved by atomic emission spectroscopy (for potassium determination) and by a conventional batch potentiometry (for total fluoride determination) adopted as reference techniques.

Optical method for the determination of grain orientation in films

DOEpatents

Maris, Humphrey J.

2001-01-01

A method for the determination of grain orientation in a film sample is provided comprising the steps of measuring a first transient optical response of the film and determining the contribution to the transient optical response arising from a change in the energy distribution of the electrons in the sample, determining the contribution to the transient optical response arising from a propagating strain pulse within the sample, and determining the contribution to the transient optical response arising from a change in sample temperature of the sample. The grain orientation of the sample may be determined using the contributions to the transient optical response arising from the change in the energy distribution of the electrons, the propagating strain pulse, and the change in sample temperature. Additionally, a method for determination of the thickness of a film sample is provided. The grain orientation of the sample is first determined. The grain orientation, together with the velocity of sound and a propagation time of a strain pulse through the sample are then used to determine the thickness of the film sample.

Optical method for the determination of grain orientation in films

DOEpatents

Maris, Humphrey J.

2003-05-13

A method for the determination of grain orientation in a film sample is provided comprising the steps of measuring a first transient optical response of the film and determining the contribution to the transient optical response arising from a change in the energy distribution of the electrons in the sample, determining the contribution to the transient optical response arising from a propagating strain pulse within the sample, and determining the contribution to the transient optical response arising from a change in sample temperature of the sample. The grain orientation of the sample may be determined using the contributions to the transient optical response arising from the change in the energy distribution of the electrons, the propagating strain pulse, and the change in sample temperature. Additionally, a method for determination of the thickness of a film sample is provided. The grain orientation of the sample is first determined. The grain orientation, together with the velocity of sound and a propagation time of a strain pulse through the sample are then used to determine the thickness of the film sample.

Simultaneous determination of Cd and Fe in beans and soil of different regions of Brazil using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling.

PubMed

dos Santos, Lisia M G; Welz, Bernhard; Araujo, Rennan G O; Jacob, Silvana do C; Vale, Maria Goreti R; Martens, Andreas; Gonzaga Martens, Irland B; Becker-Ross, Helmut

2009-11-11

A fast routine screening method for the simultaneous determination of cadmium and iron in bean and soil samples is proposed, using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling. The primary absorption line at 228.802 nm has been used for the determination of cadmium, and an adjacent secondary line, at 228.726 nm, for iron. Fourteen bean samples and 10 soil samples from nine states all over Brazil have been analyzed. The limits of detection (3 sigma, n = 10) were 2.0 microg kg(-1) for Cd and 4.5 mg kg(-1) for Fe. The relative standard deviation ranged from 4 to 7% for Cd and from 5 to 28% for Fe, which is usually acceptable for a screening method. The accuracy of the method has been confirmed by the analysis of two certified reference materials; the results were in agreement with the certified values at a 95% confidence interval.

Determination of Cu, Cd, Pb and Cr in yogurt by slurry sampling electrothermal atomic absorption spectrometry: A case study for Brazilian yogurt.

PubMed

de Andrade, Camila Kulek; de Brito, Patrícia Micaella Klack; Dos Anjos, Vanessa Egéa; Quináia, Sueli Pércio

2018-02-01

A slurry sampling electrothermal atomic absorption spectrometric method is proposed for the determination of trace elements such as Cu, Cr, Cd and Pb in yogurt. The main factors affecting the slurry preparation were optimized: nature and concentration of acid solution and sonication time. The analytical method was validated in-house by calibration, linearity, limits of detection and quantification, precision and accuracy test obtaining satisfactory results in all cases. The proposed method was applied for the determination of Cd, Cr, Cu and Pb in some Brazilian yogurt samples. For these samples, the concentrations ranged from 2.5±0.2 to 12.4±0.2ngg -1 ; 34±3 to 899±7ngg -1 ; <8.3 to 12±1ngg -1 ; and <35.4 to 210±16ngg -1 for Cd, Cu, Cr and Pb, respectively. The daily intake of Cd, Cu, Cr and Pb via consumption of these samples was estimated. Copyright © 2017 Elsevier Ltd. All rights reserved.

Determination of polychlorinated biphenyls, selected persistent organochlorine pesticides, and polybrominated flame retardants in fillets of fishes from the 2006 Missouri Department of Conservation Monitoring Programs

USGS Publications Warehouse

Gale, Robert W.; May, Thomas W.; Orazio, Carl E.; McKee, Michael J.

2008-01-01

This report presents the results of a study to determine polychlorinated biphenyl, organochlorine pesticide, and polybrominated diphenyl ether flame retardant concentrations in selected fishes from lakes and streams across Missouri. Fillets were collected from each fish sample, and after homogenization, compositing, and preparation, analyte concentrations were determined with dual column capillary gas chromatography-electron-capture detection. Total concentrations of polychlorinated biphenyls in samples ranged from background levels of about 20 to 1,200 nanograms per gram. Chlordanes and DDT-related chemicals constituted the primary classes of pesticides present at elevated concentrations in most samples, and ranged from 5 to 340 nanograms per gram. Total concentrations of polybrominated diphenyl ethers in samples ranged from background levels of about 5 to about 410 nanograms per gram. Concentrations of total technical chlordane ranged from less than 5 to 260 nanograms per gram. Concentrations of polychlorinated biphenyls, chlordanes, DDT-related compounds, and polybrominated diphenyl ethers were all greatest in samples of blue catfish from Cape Girardeau and Weldon Spring.

An improved method for the rapid determination of 90Sr in cow's milk.

PubMed

Guérin, Nicolas; Riopel, Remi; Rao, Ray; Kramer-Tremblay, Sheila; Dai, Xiongxin

2017-09-01

An improved method was developed to rapidly determine strontium-90 ( 90 Sr) in cow's milk samples in the event of a nuclear emergency. To perform this method, no heating or ashing steps were needed and all of the material used was disposable. Stable Sr tracer was added to each 40 mL milk sample. Hydrochloric acid (HCl) and trichloroacetic acid (TCA) were added to the sample to flocculate the suspended fat and proteins in the milk. The sample was centrifuged and the strontium in the supernatant was precipitated with carbonate. The resulting precipitate was dissolved in 8 M HNO 3 and the solution was passed through a Sr resin to remove potential interferents. Strontium was eluted from the resin using a small volume of water. Strontium-90 was measured by liquid-scintillation counting (LSC) and the tracer by inductively coupled plasma mass spectrometry (ICP-MS). The figures of merit of the method were determined and the method was validated using spiked samples. Crown Copyright © 2017. Published by Elsevier Ltd. All rights reserved.

Speleothem dating using Sulfur to Calcium ratio

NASA Astrophysics Data System (ADS)

Sabri, Raghid

2017-04-01

A speleothem sample from underground water tunnel in Nablus, Palestine, showed contamination from wastewater. The young sample has low concentration of Uranium and could not be dated with uranium thorium dating method. An alternative method was used to determine the age of the sample: lamina counting coupled with Sulfur to calcium ratio peaks counting. Sulfur and Calcium concentrations were measured using SEM-EDS to have a better resolution than the CNS analyzer. Assuming seasonal growth of laminations, it was possible to determine the primarily ages. The sinter was still growing during sampling in 2011. The counting reveals 271 laminae, for seasonal growth it means 135 years. In the 1959, it was observed that there is an unexpected peak of Sulfur to calcium ratio and this peak was repeated seasonally. The sulfur peak increased as a result of diesel use in the heating system during the winter season. For the youngest 117 laminae, 59 S/Ca peaks are observed. Each two lamination layers correspond to one peak. So, it was possible to determine the age of the sample using Sulfur to Calcium ratio.

Evaluation of the application of some gas chromatographic methods for the determination of properties of synthetic fuels

NASA Technical Reports Server (NTRS)

Antoine, A. C.

1979-01-01

The purpose of the investigation was to evaluate the applicability, to some synthetic fuels, of some gas chromatographic methods now under development for use with petroleum based fuels. Thirty-two jet and diesel fuel samples which were prepared from oil shale and coal syncrudes were examined. The boiling range distribution of each was determined by gas chromatography, and from that data distillation properties were calculated. The calculated results gave sufficient agreement with the measured values that the equations could be useable in their present form. Bulk fuel properties were calculated for the sixteen JP-5 and Diesel No. 2 type fuels. The results show that the equations would not give useable results. Capillary column gas chromatography was used to determine the n-alkane content of the eight JP-5 type samples and the results related to the observed freezing points. The results show that the concentrations of the long straight chain molecules in the fuels exert influence on the freezing point but are not the complete controlling factor.

Evaluation of the application of some gas chromatographic methods for the determination of properties of synthetic fuels

NASA Technical Reports Server (NTRS)

Antoine, A. C.

1978-01-01

The purpose of the investigation was to evaluate the applicability, to some synthetic fuels, of some gas chromatographic methods now under development for use with petroleum based fuels. Thirty-two jet and diesel fuel samples which were prepared from oil shale and coal syncrudes were examined. The boiling range distribution of each was determined by gas chromatography, and from that data distillation properties were calculated. The calculated results gave sufficient agreement with the measured values that the equations could be useable in their present form. Bulk fuel properties were calculated for the 16 JP-5 and Diesel No. 2 type fuels. The results show that the equations would not give useable results. Capillary column gas chromatography was used to determine the n-alkane content of the eight JP-5 type samples and the results related to the observed freezing points. The results show that the concentrations of the long straight chain molecules in the fuels exert influence on the freezing point but are not the complete controlling factor.

Exploring the Utilization of Low-Pressure, Piston-Cylinder Experiments to Determine the Bulk Compositions of Finite, Precious Materials

NASA Astrophysics Data System (ADS)

Vander Kaaden, K. E.; McCubbin, F. M.; Harrington, A.

2017-12-01

Determining the bulk composition of precious materials with a finite mass (e.g., meteorite samples) is extremely important in the fields of Earth and Planetary Science. From meteorite studies we are able to place constraints on large scale planetary processes like global differentiation and subsequent volcanism, as well as smaller scale processes like crystallization in a magma chamber or sedimentary compaction at the surface. However, with meteorite samples in particular, far too often we are limited by how precious the sample is as well as its limited mass. In this study, we have utilized aliquots of samples previously studied for toxicological hazards [1] including both the fresh samples (lunar mare basalt NWA 4734, lunar regolith breccia NWA 7611, martian basalt Tissint, martian regolith breccia NWA 7034, a vestian basalt Berthoud, a vestian regolith breccia NWA 2060, and a terrestrial mid-ocean ridge basalt (MORB)), and those that underwent iron leaching (Tissint, NWA 7034, NWA 4734, MORB). With these small masses of material, we performed low pressure ( 0.75 GPa), high temperature (>1600°C) melting experiments. Each sample was analyzed using a JEOL 8530F electron microprobe to determine the bulk composition of the materials that were previously examined in [1]. When available, the results of our microprobe data were compared with bulk rock compositions in the literature. The results of this study show that with this technique, only 50 mg of sample is required to accurately determine the bulk composition of the materials of interest. [1] Harrington, A.D., McCubbin, F.M., Kaur, J., Smirnov, A., Galdanes, K., Schoonen, M.A.A., Chen, L.C., Tsirka, S.E., and Gordon, T. (2017) Pulmonary inflammatory responses to acute meteroite dust exposures - Implications for human space exploration. 48th Lunar and Planetary Science Conference, The Woodlands, TX, #2922.

Comparison of active and passive sampling strategies for the monitoring of pesticide contamination in streams

NASA Astrophysics Data System (ADS)

Assoumani, Azziz; Margoum, Christelle; Guillemain, Céline; Coquery, Marina

2014-05-01

The monitoring of water bodies regarding organic contaminants, and the determination of reliable estimates of concentrations are challenging issues, in particular for the implementation of the Water Framework Directive. Several strategies can be applied to collect water samples for the determination of their contamination level. Grab sampling is fast, easy, and requires little logistical and analytical needs in case of low frequency sampling campaigns. However, this technique lacks of representativeness for streams with high variations of contaminant concentrations, such as pesticides in rivers located in small agricultural watersheds. Increasing the representativeness of this sampling strategy implies greater logistical needs and higher analytical costs. Average automated sampling is therefore a solution as it allows, in a single analysis, the determination of more accurate and more relevant estimates of concentrations. Two types of automatic samplings can be performed: time-related sampling allows the assessment of average concentrations, whereas flow-dependent sampling leads to average flux concentrations. However, the purchase and the maintenance of automatic samplers are quite expensive. Passive sampling has recently been developed as an alternative to grab or average automated sampling, to obtain at lower cost, more realistic estimates of the average concentrations of contaminants in streams. These devices allow the passive accumulation of contaminants from large volumes of water, resulting in ultratrace level detection and smoothed integrative sampling over periods ranging from days to weeks. They allow the determination of time-weighted average (TWA) concentrations of the dissolved fraction of target contaminants, but they need to be calibrated in controlled conditions prior to field applications. In other words, the kinetics of the uptake of the target contaminants into the sampler must be studied in order to determine the corresponding sampling rate constants (Rs). Each constant links the mass of the a target contaminant accumulated in the sampler to its concentration in water. At the end of the field application, the Rs are used to calculate the TWA concentration of each target contaminant with the final mass of the contaminants accumulated in the sampler. Stir Bar Sorptive Extraction (SBSE) is a solvent free sample preparation technique dedicated to the analysis of moderately hydrophobic to hydrophobic compounds in liquid and gas samples. It is composed of a magnet enclosed in a glass tube coated with a thick film of polydimethysiloxane (PDMS). We recently developed the in situ application of SBSE as a passive sampling technique (herein named "Passive SBSE") for the monitoring of agricultural pesticides. The aim of this study is to perform the calibration of the passive SBSE in the laboratory, and to apply and compare this technique to active sampling strategies for the monitoring of 16 relatively hydrophobic to hydrophobic pesticides in streams, during 2 1-month sampling campaigns. Time-weighted averaged concentrations of the target pesticides obtained from passive SBSE were compared to the target pesticide concentrations of grab samples, and time-related and flow-dependent samples of the streams. Results showed passive SBSE as an efficient alternative to conventional active sampling strategies.

A survey sampling approach for pesticide monitoring of community water systems using groundwater as a drinking water source.

PubMed

Whitmore, Roy W; Chen, Wenlin

2013-12-04

The ability to infer human exposure to substances from drinking water using monitoring data helps determine and/or refine potential risks associated with drinking water consumption. We describe a survey sampling approach and its application to an atrazine groundwater monitoring study to adequately characterize upper exposure centiles and associated confidence intervals with predetermined precision. Study design and data analysis included sampling frame definition, sample stratification, sample size determination, allocation to strata, analysis weights, and weighted population estimates. Sampling frame encompassed 15 840 groundwater community water systems (CWS) in 21 states throughout the U. S. Median, and 95th percentile atrazine concentrations were 0.0022 and 0.024 ppb, respectively, for all CWS. Statistical estimates agreed with historical monitoring results, suggesting that the study design was adequate and robust. This methodology makes no assumptions regarding the occurrence distribution (e.g., lognormality); thus analyses based on the design-induced distribution provide the most robust basis for making inferences from the sample to target population.

Neutron activation analysis of certified samples by the absolute method

NASA Astrophysics Data System (ADS)

Kadem, F.; Belouadah, N.; Idiri, Z.

2015-07-01

The nuclear reactions analysis technique is mainly based on the relative method or the use of activation cross sections. In order to validate nuclear data for the calculated cross section evaluated from systematic studies, we used the neutron activation analysis technique (NAA) to determine the various constituent concentrations of certified samples for animal blood, milk and hay. In this analysis, the absolute method is used. The neutron activation technique involves irradiating the sample and subsequently performing a measurement of the activity of the sample. The fundamental equation of the activation connects several physical parameters including the cross section that is essential for the quantitative determination of the different elements composing the sample without resorting to the use of standard sample. Called the absolute method, it allows a measurement as accurate as the relative method. The results obtained by the absolute method showed that the values are as precise as the relative method requiring the use of standard sample for each element to be quantified.

Beyond the "science of sophomores": does the rational choice explanation of crime generalize from university students to an actual offender sample?

PubMed

Bouffard, Jeff; Bry, Jeff; Smith, Shamayne; Bry, Rhonda

2008-12-01

Much of the criminological literature testing rational choice theory has utilized hypothetical scenarios presented to university students. Although this research generally supports rational choice theory, a common criticism is that conclusions from these studies may not generalize to samples of actual offenders. This study proceeds to examine this issue in two steps. First, a traditional sample of university students is examined to determine how various costs and benefits relate to their hypothetical likelihood of offending. Then the same data collection procedures are employed with a somewhat different sample of younger, adjudicated, and institutionalized offenders to determine whether the conclusions drawn from the student sample generalize to this offender sample. Results generally suggest that the content and process of hypothetical criminal decision making differ in the sample of known offenders relative to the university students. Limitations of the current study, as well as suggestions for future research, are discussed.

Modified Sample Preparation Approach for the Determination of the Phenolic and Humic-Like Substances in Natural Organic Materials By the Folin Ciocalteu Method.

PubMed

Pontoni, Ludovico; Panico, Antonio; Matanò, Alessia; van Hullebusch, Eric D; Fabbricino, Massimiliano; Esposito, Giovanni; Pirozzi, Francesco

2017-12-06

A novel modification of the sample preparation procedure for the Folin-Ciocalteu colorimetric assay for the determination of total phenolic compounds in natural solid and semisolid organic materials (e.g., foods, organic solid waste, soils, plant tissues, agricultural residues, manure) is proposed. In this method, the sample is prepared by adding sodium sulfate as a solid diluting agent before homogenization. The method allows for the determination of total phenols (TP) in samples with high solids contents, and it provides good accuracy and reproducibility. Additionally, this method permits analyses of significant amounts of sample, which reduces problems related to heterogeneity. We applied this method to phenols-rich lignocellulosic and humic-like solids and semisolid samples, including rice straw (RS), peat-rich soil (PS), and food waste (FW). The TP concentrations measured with the solid dilution (SD) preparation were substantially higher (increases of 41.4%, 15.5%, and 59.4% in RS, PS and FW, respectively) than those obtained with the traditional method (solids suspended in water). These results showed that the traditional method underestimates the phenolic contents in the studied solids.

Determination of polychlorinated biphenyls, selected persistent organochlorine pesticides, and polybrominated flame retardants in fillets of fishes from the 2007 Missouri Department of Conservation Monitoring Program

USGS Publications Warehouse

Gale, Robert W.; Orazio, Carl E.; McKee, Michael J.

2009-01-01

This report presents the results of a study to determine polychlorinated biphenyl, organochlorine pesticide, and polybrominated diphenylether flame retardant concentrations in selected fishes from lakes and streams across Missouri. Fillets were collected from each fish sample and after homogenization, compositing, and preparation, analyte concentrations were determined with dual column capillary gas chromatography-electron-capture detection. Total concentrations of polychlorinated biphenyls in samples ranged from background levels of about 50 to 300 nanograms per gram. In samples with elevated contaminant concentrations, chlordanes, DDT-related chemicals, and dieldrin constituted the primary classes of pesticides present, and ranged from 5 to 75 nanograms per gram. Total concentrations of polybrominated diphenyl ethers in samples ranged from background levels of 5 to 86 nanograms per gram. Channel catfish from the upper and lower Blue River and lake sturgeon from the Mississippi River at Saverton exhibited different polybrominated diphenyl ethers ratios. Concentrations of polychlorinated biphenyls, chlordanes, DDT-related compounds, and polybrominated diphenyl ethers all were greatest in samples of channel catfish from the upper and lower Blue River, and in samples of lake sturgeon from the Mississippi River at Saverton.

Organic petrology of selected oil shale samples from lower Carboniferous Albert Formation, New Brunswick, Canada

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

Kalkreuth, W.; Macauley, G.

1984-04-01

Incident light microscopy was used to describe maturation and composition of organic material in oil shale samples from the Lower Carboniferous Albert Formation of New Brunswick. The maturation level was determined in normal (white) light by measuring vitrinite reflectance and in fluorescent light by measuring fluorescence spectral of alginite B. Results indicate low to intermediate maturation for all of the samples. Composition was determined by maceral analysis. Alginite B is the major organic component in all samples having significant oil potential. Oil yields obtained from the Fischer Assay process, and oil and gas potentials from Rock-Eval analyses correlate to themore » amounts of alginite B and bituminite determined in the samples. In some of the samples characterized by similar high concentrations of alginite B, decrease in Fischer Assay yields and oil and gas potentials is related to an increase in maturation, as expected by increase in the fluorescence parameter lambda/sub max/ and red/green quotient of alginite B. Incident light microscopy, particularly with fluorescent light, offers a valuable tool for the identification of the organic matter in oil shales and for the evaluation of their oil and gas potentials.« less

Precise method for the measurement of catalase activity in honey.

PubMed

Huidobro, José F; Sánchez, M Pilar; Muniategui, Soledad; Sancho, M Teresa

2005-01-01

An improved method is reported for the determination of catalase activity in honey. We tested different dialysis membranes, dialysis fluid compositions and amounts, dialysis temperatures, sample amounts, and dialysis times. The best results were obtained by dialysis of 7.50 g sample in a cellulose dialysis sack, using two 3 L portions of 0.015 M sodium phosphate buffer (pH 7.0) as the dialysis fluid at 4 degrees C for 22 h. As in previous methods, catalase activity was determined on the basis of the rate of disappearance of the substrate, H202, with the H202 determined spectrophotometrically at 400 nm in an assay system containing o-dianisidine and peroxidase. Trials indicated that the best solvent for the o-dianisidine was 0.2 M sodium phosphate buffer, pH 6.1; the best starting H202 concentration was 3 mM; the best HCl concentration for stopping the reaction was 6 N; and the best sample volume for catalase measurement was 7.0 mL. Precision values (relative standard deviations for analyses of 10 subsamples of each of 3 samples) were high, ranging from 0.48% for samples with high catalase activity to 1.98% for samples with low catalase activity.

Effects of sterilization treatments on the analysis of TOC in water samples.

PubMed

Shi, Yiming; Xu, Lingfeng; Gong, Dongqin; Lu, Jun

2010-01-01

Decomposition experiments conducted with and without microbial processes are commonly used to study the effects of environmental microorganisms on the degradation of organic pollutants. However, the effects of biological pretreatment (sterilization) on organic matter often have a negative impact on such experiments. Based on the principle of water total organic carbon (TOC) analysis, the effects of physical sterilization treatments on determination of TOC and other water quality parameters were investigated. The results revealed that two conventional physical sterilization treatments, autoclaving and 60Co gamma-radiation sterilization, led to the direct decomposition of some organic pollutants, resulting in remarkable errors in the analysis of TOC in water samples. Furthermore, the extent of the errors varied with the intensity and the duration of sterilization treatments. Accordingly, a novel sterilization method for water samples, 0.45 microm micro-filtration coupled with ultraviolet radiation (MCUR), was developed in the present study. The results indicated that the MCUR method was capable of exerting a high bactericidal effect on the water sample while significantly decreasing the negative impact on the analysis of TOC and other water quality parameters. Before and after sterilization treatments, the relative errors of TOC determination could be controlled to lower than 3% for water samples with different categories and concentrations of organic pollutants by using MCUR.

[Principal component analysis and cluster analysis of inorganic elements in sea cucumber Apostichopus japonicus].

PubMed

Liu, Xiao-Fang; Xue, Chang-Hu; Wang, Yu-Ming; Li, Zhao-Jie; Xue, Yong; Xu, Jie

2011-11-01

The present study is to investigate the feasibility of multi-elements analysis in determination of the geographical origin of sea cucumber Apostichopus japonicus, and to make choice of the effective tracers in sea cucumber Apostichopus japonicus geographical origin assessment. The content of the elements such as Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Mo, Cd, Hg and Pb in sea cucumber Apostichopus japonicus samples from seven places of geographical origin were determined by means of ICP-MS. The results were used for the development of elements database. Cluster analysis(CA) and principal component analysis (PCA) were applied to differentiate the sea cucumber Apostichopus japonicus geographical origin. Three principal components which accounted for over 89% of the total variance were extracted from the standardized data. The results of Q-type cluster analysis showed that the 26 samples could be clustered reasonably into five groups, the classification results were significantly associated with the marine distribution of the sea cucumber Apostichopus japonicus samples. The CA and PCA were the effective methods for elements analysis of sea cucumber Apostichopus japonicus samples. The content of the mineral elements in sea cucumber Apostichopus japonicus samples was good chemical descriptors for differentiating their geographical origins.

Computer program uses Monte Carlo techniques for statistical system performance analysis

NASA Technical Reports Server (NTRS)

Wohl, D. P.

1967-01-01

Computer program with Monte Carlo sampling techniques determines the effect of a component part of a unit upon the overall system performance. It utilizes the full statistics of the disturbances and misalignments of each component to provide unbiased results through simulated random sampling.

Energy-dispersive X-ray fluorescence systems as analytical tool for assessment of contaminated soils.

PubMed

Vanhoof, Chris; Corthouts, Valère; Tirez, Kristof

2004-04-01

To determine the heavy metal content in soil samples at contaminated locations, a static and time consuming procedure is used in most cases. Soil samples are collected and analyzed in the laboratory at high quality and high analytical costs. The demand by government and consultants for a more dynamic approach and by customers requiring performances in which analyses are performed in the field with immediate feedback of the analytical results, is growing. Especially during the follow-up of remediation projects or during the determination of the sampling strategy, field analyses are advisable. For this purpose four types of ED-XRF systems, ranging from portable up to high performance laboratory systems, have been evaluated. The evaluation criteria are based on the performance characteristics for all the ED-XRF systems such as limit of detection, accuracy and the measurement uncertainty on one hand, and also the influence of the sample pretreatment on the obtained results on the other hand. The study proved that the field portable system and the bench top system, placed in a mobile van, can be applied as field techniques, resulting in semi-quantitative analytical results. A limited homogenization of the analyzed sample significantly increases the representativeness of the soil sample. The ED-XRF systems can be differentiated by their limits of detection which are a factor of 10 to 20 higher for the portable system. The accuracy of the results and the measurement uncertainty also improved using the bench top system. Therefore, the selection criteria for applicability of both field systems are based on the required detection level and also the required accuracy of the results.

Solar Flare Track Exposure Ages in Regolith Particles: A Calibration for Transmission Electron Microscope Measurements

NASA Technical Reports Server (NTRS)

Berger, Eve L.; Keller, Lindsay P.

2015-01-01

Mineral grains in lunar and asteroidal regolith samples provide a unique record of their interaction with the space environment. Space weathering effects result from multiple processes including: exposure to the solar wind, which results in ion damage and implantation effects that are preserved in the rims of grains (typically the outermost 100 nm); cosmic ray and solar flare activity, which result in track formation; and impact processes that result in the accumulation of vapor-deposited elements, impact melts and adhering grains on particle surfaces. Determining the rate at which these effects accumulate in the grains during their space exposure is critical to studies of the surface evolution of airless bodies. Solar flare energetic particles (mainly Fe-group nuclei) have a penetration depth of a few millimeters and leave a trail of ionization damage in insulating materials that is readily observable by transmission electron microscope (TEM) imaging. The density of solar flare particle tracks is used to infer the length of time an object was at or near the regolith surface (i.e., its exposure age). Track measurements by TEM methods are routine, yet track production rate calibrations have only been determined using chemical etching techniques [e.g., 1, and references therein]. We used focused ion beam-scanning electron microscope (FIB-SEM) sample preparation techniques combined with TEM imaging to determine the track density/exposure age relations for lunar rock 64455. The 64455 sample was used earlier by [2] to determine a track production rate by chemical etching of tracks in anorthite. Here, we show that combined FIB/TEM techniques provide a more accurate determination of a track production rate and also allow us to extend the calibration to solar flare tracks in olivine.

Determination of Depleted Uranium in Environmental Bio-monitor Samples and Soil from Target sites in Western Balkan Region

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

Sahoo, Sarata K.; Enomoto, Hiroko; Tokonami, Shinji

2008-08-07

Lichen and Moss are widely used to assess the atmospheric pollution by heavy metals and radionuclides. In this paper, we report results of uranium and its isotope ratios using mass spectrometric measurements (followed by chemical separation procedure) for mosses, lichens and soil samples from a depleted uranium (DU) target site in western Balkan region. Samples were collected in 2003 from Han Pijesak (Republika Srpska in Bosnia and Hercegovina). Inductively coupled plasma mass spectrometry (ICP-MS) measurements show the presence of high concentration of uranium in some samples. Concentration of uranium in moss samples ranged from 5.2-755.43 Bq/Kg. We have determined {supmore » 235}U/{sup 238}U isotope ratio using thermal ionization mass spectrometry (TIMS) from the samples with high uranium content and the ratios are in the range of 0.002097-0.002380. TIMS measurement confirms presence of DU in some samples. However, we have not noticed any traces of DU in samples containing lesser amount of uranium or from any samples from the living environment of same area.« less

Measurements of cesium in Arctic beluga and caribou before and after the Fukushima accident of 2011.

PubMed

Stocki, T J; Gamberg, M; Loseto, L; Pellerin, E; Bergman, L; Mercier, J-F; Genovesi, L; Cooke, M; Todd, B; Sandles, D; Whyte, J; Wang, X

2016-10-01

Concern from northern communities following the Fukushima Daiichi nuclear accident of March 2011 has prompted a reassessment of the safety of their traditional foods with respect to radioactivity levels. To this end, a study was conducted to measure the levels of radionuclides in Arctic caribou (Rangifer tarandus) and beluga (Delphinapterus leucas). The main radionuclide of concern is cesium-137, which is easily transferred through the lichen-caribou food chain. Previous studies have been conducted on the cesium-137 levels in Canadian caribou herds from 1958 to 2000, allowing researchers to determine the amount of cesium-137 in caribou specifically attributable to atmospheric weapons testing and the Chernobyl nuclear accident in 1986. In this study, samples of lichens, mushrooms, caribou, beluga and beluga prey collected before and after the Fukushima accident were analyzed for radioactivity levels. Samples were processed and measured using gamma ray spectroscopy to identify the radionuclides present and determine the radioactivity concentration. Both calibration standards and Monte Carlo simulations were used to determine the efficiency of the detectors for the samples, taking into account differences in individual sample sizes as well as matrices. In particular, a careful analysis of the atomic composition of lichens and mushrooms was performed to ensure the efficiencies for these sample types were correct. A comparison of the concentrations from before and after the accident indicated that there was no increase in radioactivity as a result of the atmospheric plume from the Fukushima accident. Some cesium-137, likely attributable to fallout from atmospheric weapons testing of the 1950s and 1960s (since there was no cesium-134 measured in the samples), was measured in the post Fukushima caribou and beluga whale samples; however, this amount was determined to be insignificant for any radiological concern (9.1 ± 1.8 and 0.63 ± 0.23 Bq kg -1  ww respectively). The activity concentrations of cesium-137 was about 200 times smaller than that of natural radioactive potassium in the beluga samples. Both the caribou and beluga results showed that these foods continue to be a healthy food choice for northern Canadians with respect to radioactivity, and this result has been communicated to the nearby northern communities and stakeholders. Copyright © 2016. Published by Elsevier Ltd.

Determination of Caffeine in Beverages by High Performance Liquid Chromatography.

ERIC Educational Resources Information Center

DiNunzio, James E.

1985-01-01

Describes the equipment, procedures, and results for the determination of caffeine in beverages by high performance liquid chromatography. The method is simple, fast, accurate, and, because sample preparation is minimal, it is well suited for use in a teaching laboratory. (JN)

Sequential injection titration method using second-order signals: determination of acidity in plant oils and biodiesel samples.

PubMed

del Río, Vanessa; Larrechi, M Soledad; Callao, M Pilar

2010-06-15

A new concept of flow titration is proposed and demonstrated for the determination of total acidity in plant oils and biodiesel. We use sequential injection analysis (SIA) with a diode array spectrophotometric detector linked to chemometric tools such as multivariate curve resolution-alternating least squares (MCR-ALS). This system is based on the evolution of the basic specie of an acid-base indicator, alizarine, when it comes into contact with a sample that contains free fatty acids. The gradual pH change in the reactor coil due to diffusion and reaction phenomenona allows the sequential appearance of both species of the indicator in the detector coil, recording a data matrix for each sample. The SIA-MCR-ALS method helps to reduce the amounts of sample, the reagents and the time consumed. Each determination consumes 0.413ml of sample, 0.250ml of indicator and 3ml of carrier (ethanol) and generates 3.333ml of waste. The frequency of the analysis is high (12 samples h(-1) including all steps, i.e., cleaning, preparing and analysing). The utilized reagents are of common use in the laboratory and it is not necessary to use the reagents of perfect known concentration. The method was applied to determine acidity in plant oil and biodiesel samples. Results obtained by the proposed method compare well with those obtained by the official European Community method that is time consuming and uses large amounts of organic solvents.

Aerial sampling of emissions from biomass pile burns in ...

EPA Pesticide Factsheets

Emissions from burning piles of post-harvest timber slash in Grande Ronde, Oregon were sampled using an instrument platform lofted into the plume using a tether-controlled aerostat or balloon. Emissions of carbon monoxide, carbon dioxide, methane, particulate matter (PM2.5 µm), black carbon, ultraviolet absorbing PM, elemental/organic carbon, semi-volatile organics (polycyclic aromatic hydrocarbons and polychlorinated dibenzodioxins/dibenzofurans), filter-based metals, and volatile organics were sampled for determination of emission factors. The effect on emissions from covering or not covering piles with polyethylene sheets to prevent fuel wetting was determined. Results showed that the uncovered (“wet”) piles burned with lower combustion efficiency and higher emissions of volatile organic compounds. Results for other pollutants will also be discussed. This work determined the emissions from open burning of forest slash wood, with and without plastic sheeting. The foresters advocate the use of plastic to keep the slash wood dry and aid in the controlled combustion of the slash to reduce fuel loading. Concerns about the emissions from the burning plastic prompted this work which conducted an extensive characterization of dry, wet, and dry with plastic slash pile emissions.

Simultaneous determination of selected biogenic amines in alcoholic beverage samples by isotachophoretic and chromatographic methods.

PubMed

Jastrzębska, Aneta; Piasta, Anna; Szłyk, Edward

2014-01-01

A simple and useful method for the determination of biogenic amines in beverage samples based on isotachophoretic separation is described. The proposed procedure permitted simultaneous analysis of histamine, tyramine, cadaverine, putrescine, tryptamine, 2-phenylethylamine, spermine and spermidine. The data presented demonstrate the utility, simplicity, flexibility, sensitivity and environmentally friendly character of the proposed method. The precision of the method expressed as coefficient of variations varied from 0.1% to 5.9% for beverage samples, whereas recoveries varied from 91% to 101%. The results for the determination of biogenic amines were compared with an HPLC procedure based on a pre-column derivatisation reaction of biogenic amines with dansyl chloride. Furthermore, the derivatisation procedure was optimised by verification of concentration and pH of the buffer, the addition of organic solvents, reaction time and temperature.

Elastic anisotropy effects on the electrical responses of a thin sample of nematic liquid crystal.

PubMed

Gomes, O A; Yednak, C A R; Ribeiro de Almeida, R R; Teixeira-Souza, R T; Evangelista, L R

2017-03-01

The electrical responses of a nematic liquid crystal cell are investigated by means of the elastic continuum theory. The nematic medium is considered as a parallel circuit of a resistance and a capacitance and the electric current profile across the sample is determined as a function of the elastic constants. In the reorientation process of the nematic director, the resistance and capacitance of the sample are determined by taking into account the elastic anisotropy. A nonmonotonic profile for the current is observed in which a minimum value of the current may be used to estimate the elastic constants values. This scenario suggests a theoretical method to determine the values of the bulk elastic constants in a single planar aligned cell just by changing the direction of applied electrical field and measuring the resulting electrical current.

Sampling colloids and colloid-associated contaminants in ground water

USGS Publications Warehouse

Backhus, Debera A.; Ryan, Joseph N.; Groher, Daniel M.; MacFarlane, John K.; Gschwend, Philip M.

1993-01-01

It has recently been recognized that mobile colloids may affect the transport of contaminants in ground water. To determine the significance of this process, knowledge of both the total mobile load (dissolved + colloid-associated) and the dissolved concentration of a ground-water contaminant must be obtained. Additional information regarding mobile colloid characteristics and concentrations are required to predict accurately the fate and effects of contaminants at sites where significant quantities of colloids are found. To obtain this information, a sampling scheme has been designed and refined to collect mobile colloids while avoiding the inclusion of normally immobile subsurface and well-derived solids. The effectiveness of this sampling protocol was evaluated at a number of contaminated and pristine sites.The sampling results indicated that slow, prolonged pumping of ground water is much more effective at obtaining ground-water samples that represent in situ colloid populations than bailing. Bailed samples from a coal tar-contaminated site contained 10–100 times greater colloid concentrations and up to 750 times greater polycyclic aromatic hydrocarbon concentrations as were detected in slowly pumped samples. The sampling results also indicated that ground-water colloid concentrations should be monitored in the field to determine the adequacy of purging if colloid and colloid-associated contaminants are of interest. To avoid changes in the natural ground-water colloid population through precipitation or coagulation, in situ ground-water chemistry conditions must be preserved during sampling and storage. Samples collected for determination of the total mobile load of colloids and low-solubility contaminants must not be filtered because some mobile colloids are removed by this process. Finally, suggestions that mobile colloids are present in ground water at any particular site should be corroborated with auxiliary data, such as colloid levels in “background” wells, colloid-size distributions, ground-water geochemistry, and colloid surface characteristics.

A laboratory-scale pretreatment and hydrolysis assay for determination of reactivity in cellulosic biomass feedstocks.

PubMed

Wolfrum, Edward J; Ness, Ryan M; Nagle, Nicholas J; Peterson, Darren J; Scarlata, Christopher J

2013-11-14

The rapid determination of the release of structural sugars from biomass feedstocks is an important enabling technology for the development of cellulosic biofuels. An assay that is used to determine sugar release for large numbers of samples must be robust, rapid, and easy to perform, and must use modest amounts of the samples to be tested.In this work we present a laboratory-scale combined pretreatment and saccharification assay that can be used as a biomass feedstock screening tool. The assay uses a commercially available automated solvent extraction system for pretreatment followed by a small-scale enzymatic hydrolysis step. The assay allows multiple samples to be screened simultaneously, and uses only ~3 g of biomass per sample. If the composition of the biomass sample is known, the results of the assay can be expressed as reactivity (fraction of structural carbohydrate present in the biomass sample released as monomeric sugars). We first present pretreatment and enzymatic hydrolysis experiments on a set of representative biomass feedstock samples (corn stover, poplar, sorghum, switchgrass) in order to put the assay in context, and then show the results of the assay applied to approximately 150 different feedstock samples covering 5 different materials. From the compositional analysis data we identify a positive correlation between lignin and structural carbohydrates, and from the reactivity data we identify a negative correlation between both carbohydrate and lignin content and total reactivity. The negative correlation between lignin content and total reactivity suggests that lignin may interfere with sugar release, or that more mature samples (with higher structural sugars) may have more recalcitrant lignin. The assay presented in this work provides a robust and straightforward method to measure the sugar release after pretreatment and saccharification that can be used as a biomass feedstock screening tool. We demonstrated the utility of the assay by identifying correlations between feedstock composition and reactivity in a population of 150 samples.

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.

Total and inorganic arsenic in fish samples from Norwegian waters.

PubMed

Julshamn, Kaare; Nilsen, Bente M; Frantzen, Sylvia; Valdersnes, Stig; Maage, Amund; Nedreaas, Kjell; Sloth, Jens J

2012-01-01

The contents of total arsenic and inorganic arsenic were determined in fillet samples of Northeast Artic cod, herring, mackerel, Greenland halibut, tusk, saithe and Atlantic halibut. In total, 923 individual fish samples were analysed. The fish were mostly caught in the open sea off the coast of Norway, from 40 positions. The determination of total arsenic was carried out by inductively coupled plasma mass spectrometry following microwave-assisted wet digestion. The determination of inorganic arsenic was carried out by high-performance liquid chromatography-ICP-MS following microwave-assisted dissolution of the samples. The concentrations found for total arsenic varied greatly between fish species, and ranged from 0.3 to 110 mg kg(-1) wet weight. For inorganic arsenic, the concentrations found were very low (<0.006 mg kg(-1)) in all cases. The obtained results question the assumptions made by the European Food Safety Authority (EFSA) on the inorganic arsenic level in fish used in the recent EFSA opinion on arsenic in food.

Determination of epichlorohydrin and 1,3-dichloro-2-propanol in synthesis of cationic etherifying reagent by headspace gas chromatography.

PubMed

Tao, Zheng-Yi; Chai, Xin-Sheng; Wu, Shu-Bin

2011-09-16

This study demonstrates a headspace gas chromatographic(HS-GC) technique for the determination of residual epichlorohydrin (ECH) and generated 1,3-dichloro-2-propanol (DCP) in synthesis process of 3-chloro-2-hydroxypropyltrimethylammonium chloride (CHTAC). By a weight-based sampling method, coupled with significant dilution in 15.8% sodium sulfate and 0.1% silver nitrate mixed solution rapidly, the sample for HS-GC analysis is prepared. Based on the reaction stoichiometry, the conversion (R) of CHTAC during the synthesis process can be calculated from sampling weight and GC peak area. The results showed that the method has a good measurement precision (RSD<2.5%) and accuracy (recovery=101-104%) for the quantification of both ECH and DCP in the process samples. The present method is simple and accurate, which can be used for the efficient determination of the CHTAC conversion in the synthesis research. Copyright © 2011 Elsevier B.V. All rights reserved.

Use of High-Resolution Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS) for Sequential Multi-Element Determination of Metals in Seawater and Wastewater Samples

NASA Astrophysics Data System (ADS)

Peña-Vázquez, E.; Barciela-Alonso, M. C.; Pita-Calvo, C.; Domínguez-González, R.; Bermejo-Barrera, P.

2015-09-01

The objective of this work is to develop a method for the determination of metals in saline matrices using high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Module SFS 6 for sample injection was used in the manual mode, and flame operating conditions were selected. The main absorption lines were used for all the elements, and the number of selected analytical pixels were 5 (CP±2) for Cd, Cu, Fe, Ni, Pb and Zn, and 3 pixels for Mn (CP±1). Samples were acidified (0.5% (v/v) nitric acid), and the standard addition method was used for the sequential determination of the analytes in diluted samples (1:2). The method showed good precision (RSD(%) < 4%, except for Pb (6.5%)) and good recoveries. Accuracy was checked after the analysis of an SPS-WW2 wastewater reference material diluted with synthetic seawater (dilution 1:2), showing a good agreement between certified and experimental results.

A rapid method for simultaneously determining ethanol and methanol content in wines by full evaporation headspace gas chromatography.

PubMed

Zhang, Chun-Yun; Lin, Neng-Biao; Chai, Xin-Sheng; Zhong-Li; Barnes, Donald G

2015-09-15

This work reports on a full evaporation headspace gas chromatographic (FE HS-GC) method for simultaneously determining the ethanol (EtOH) and methanol (MeOH) content in wines. A small sample (10μL) was placed in a headspace sample vial, and a near-complete mass transfer of ethanol and methanol from the liquid sample to the vapor phase was obtained within three minutes at a temperature of 105°C, which allowed the measurement of the EtOH and MeOH content in the sample by GC. The results showed excellent precision and accuracy, as shown by the reproducibilities of 1.02% and 2.11% for EtOH and MeOH, respectively, and recoveries that ranged from 96.1% to 104% for both alcohols. The method is efficient, accurate and suitable for the determination of EtOH and MeOH in wine production and quality control. Copyright © 2015 Elsevier Ltd. All rights reserved.

The Third SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-3)

NASA Technical Reports Server (NTRS)

Hooker, Stanford B.; VanHeukelem, Laurei; Thomas, Crystal S.; Claustre, Herve; Ras, Josephine; Schluter, Louise; Clementson, Lesley; vanderLinde, Dirk; Eker-Develi, Elif; Berthon, Jean-Francois;

The differential path phase comparison method for determining pressure derivatives of elastic constants of solids

NASA Astrophysics Data System (ADS)

Peselnick, L.

1982-08-01

An ultrasonic method is presented which combines features of the differential path and the phase comparison methods. The proposed differential path phase comparison method, referred to as the `hybrid' method for brevity, eliminates errors resulting from phase changes in the bond between the sample and buffer rod. Define r(P) [and R(P)] as the square of the normalized frequency for cancellation of sample waves for shear [and for compressional] waves. Define N as the number of wavelengths in twice the sample length. The pressure derivatives r'(P) and R' (P) for samples of Alcoa 2024-T4 aluminum were obtained by using the phase comparison and the hybrid methods. The values of the pressure derivatives obtained by using the phase comparison method show variations by as much as 40% for small values of N (N < 50). The pressure derivatives as determined from the hybrid method are reproducible to within ±2% independent of N. The values of the pressure derivatives determined by the phase comparison method for large N are the same as those determined by the hybrid method. Advantages of the hybrid method are (1) no pressure dependent phase shift at the buffer-sample interface, (2) elimination of deviatoric stress in the sample portion of the sample assembly with application of hydrostatic pressure, and (3) operation at lower ultrasonic frequencies (for comparable sample lengths), which eliminates detrimental high frequency ultrasonic problems. A reduction of the uncertainties of the pressure derivatives of single crystals and of low porosity polycrystals permits extrapolation of such experimental data to deeper mantle depths.

Rapid Determination of the Chemical Oxygen Demand of Water Using a Thermal Biosensor

PubMed Central

Yao, Na; Wang, Jinqi; Zhou, Yikai

2014-01-01

In this paper we describe a thermal biosensor with a flow injection analysis system for the determination of the chemical oxygen demand (COD) of water samples. Glucose solutions of different concentrations and actual water samples were tested, and their COD values were determined by measuring the heat generated when the samples passed through a column containing periodic acid. The biosensor exhibited a large linear range (5 to 3000 mg/L) and a low detection limit (1.84 mg/L). It could tolerate the presence of chloride ions in concentrations of 0.015 M without requiring a masking agent. The sensor was successfully used for detecting the COD values of actual samples. The COD values of water samples from various sources were correlated with those obtained by the standard dichromate method; the linear regression coefficient was found to be 0.996. The sensor is environmentally friendly, economical, and highly stable, and exhibits good reproducibility and accuracy. In addition, its response time is short, and there is no danger of hazardous emissions or external contamination. Finally, the samples to be tested do not have to be pretreated. These results suggest that the biosensor is suitable for the continuous monitoring of the COD values of actual wastewater samples. PMID:24915178

Solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for gold determination in geological samples after preconcentration onto carbon nanotubes

NASA Astrophysics Data System (ADS)

Dobrowolski, Ryszard; Mróz, Agnieszka; Dąbrowska, Marzena; Olszański, Piotr

2017-06-01

A novelty method for the determination of gold in geological samples by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GF AAS) after solid-phase extraction onto modified carbon nanotubes (CNT) was described. The methodology developed is based on solid phase extraction of Au(III) ions from digested samples to eliminate strong interference caused by iron compounds and problems related to inhomogeneities of the samples. The use of aqueous or solid standard for calibration was studied and the slope of calibration curve was the same for both of these modes. This statement indicates the possibility to perform the calibration of the method using aqueous standard solutions. Under optimum conditions the absolute detection limit for gold was equal to 2.24 · 10- 6 μg g- 1 while the adsorption capacity of modified carbon nanotubes was 264 mg g- 1. The proposed procedure was validated by the application of certified reference materials (CRMs) with different content of gold and different matrix, the results were in good agreement with certified values. The method was successfully applied for separation and determination of gold ions in complex geological samples, with precision generally better than 8%.

A rapid and high-precision method for sulfur isotope δ(34)S determination with a multiple-collector inductively coupled plasma mass spectrometer: matrix effect correction and applications for water samples without chemical purification.

PubMed

Lin, An-Jun; Yang, Tao; Jiang, Shao-Yong

2014-04-15

Previous studies have indicated that prior chemical purification of samples, although complex and time-consuming, is essential in obtaining precise and accurate results for sulfur isotope ratios using multiple-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). In this study, we introduce a new, rapid and precise MC-ICP-MS method for sulfur isotope determination from water samples without chemical purification. The analytical work was performed on an MC-ICP-MS instrument with medium mass resolution (m/Δm ~ 3000). Standard-sample bracketing (SSB) was used to correct samples throughout the analytical sessions. Reference materials included an Alfa-S (ammonium sulfate) standard solution, ammonium sulfate provided by the lab of the authors and fresh seawater from the South China Sea. A range of matrix-matched Alfa-S standard solutions and ammonium sulfate solutions was used to investigate the matrix (salinity) effect (matrix was added in the form of NaCl). A seawater sample was used to confirm the reliability of the method. Using matrix-matched (salinity-matched) Alfa-S as the working standard, the measured δ(34)S value of AS (-6.73 ± 0.09‰) was consistent with the reference value (-6.78 ± 0.07‰) within the uncertainty, suggesting that this method could be recommended for the measurement of water samples without prior chemical purification. The δ(34)S value determination for the unpurified seawater also yielded excellent results (21.03 ± 0.18‰) that are consistent with the reference value (20.99‰), thus confirming the feasibility of the technique. The data and the results indicate that it is feasible to use MC-ICP-MS and matrix-matched working standards to measure the sulfur isotopic compositions of water samples directly without chemical purification. In comparison with the existing MC-ICP-MS techniques, the new method is better for directly measuring δ(34)S values in water samples with complex matrices; therefore, it can significantly accelerate analytical turnover. Copyright © 2014 John Wiley & Sons, Ltd.

Color quality of pigments in cochineals (Dactylopius coccus Costa). Geographical origin characterization using multivariate statistical analysis.

PubMed

Méndez, Jesús; González, Mónica; Lobo, M Gloria; Carnero, Aurelio

2004-03-10

The commercial value of a cochineal (Dactylopius coccus Costa) sample is associated with its color quality. Because the cochineal is a legal food colorant, its color quality is generally understood as its pigment content. Simply put, the higher this content, the more valuable the sample is to the market. In an effort to devise a way to measure the color quality of a cochineal, the present study evaluates different parameters of color measurement such as chromatic attributes (L*, and a*), percentage of carminic acid, tint determination, and chromatographic profile of pigments. Tint determination did not achieve this objective because this parameter does not correlate with carminic acid content. On the other hand, carminic acid showed a highly significant correlation (r = - 0.922, p = 0.000) with L* values determined from powdered cochineal samples. The combination of the information from the spectrophotometric determination of carminic acid with that of the pigment profile acquired by liquid chromatography (LC) and the composition of the red and yellow pigment groups, also acquired by LC, enables greater accuracy in judging the quality of the final sample. As a result of this study, it was possible to achieve the separation of cochineal samples according to geographical origin using two statistical techniques: cluster analysis and principal component analysis.

Evaluation of a gas chromatography method for azelaic acid determination in selected biological samples.

PubMed

Garelnabi, Mahdi; Litvinov, Dmitry; Parthasarathy, Sampath

2010-09-01

Azelaic acid (AzA) is the best known dicarboxilic acid to have pharmaceutical benefits and clinical applications and also to be associated with some diseases pathophysiology. We extracted and methylesterified AzA and determined its concentration in human plasma obtained from healthy individuals and also in mice fed AzA containing diet for three months. AzA was detected in Gas Chromatography (GC) and confirmed by Liquid chromatography mass spectrometry (LCMS), and gas chromatography mass spectrometry (GCMC). Our results have shown that AzA can be determined efficiently in selected biological samples by GC method with 1nM limit of detection (LoD) and the limit of quantification (LoQ); was established at 50nM. Analytical Sensitivity as assayed by hexane demonstrated an analytical sensitivity at 0.050nM. The method has demonstrated 8-10% CV batch repeatability across the sample types and 13-18.9% CV for the Within-Lab Precision analysis. The method has shown that AzA can efficiently be recovered from various sample preparation including liver tissue homogenate (95%) and human plasma (97%). Because of its simplicity and lower limit of quantification, the present method provides a useful tool for determining AzA in various biological sample preparations.

Fabrication and Characterization of Surrogate Glasses Aimed to Validate Nuclear Forensic Techniques

DTIC Science & Technology

2017-12-01

sample is processed while submerged and produces fine sized particles the exposure levels and risk of contamination from the samples is also greatly...induced the partial collapses of the xerogel network strengthened the network while the sample sizes were reduced [22], [26]. As a result the wt...inhomogeneous, making it difficult to clearly determine which features were present in the sample before LDHP and which were caused by it. In this study

Comparability among four invertebrate sampling methods and two multimetric indexes, Fountain Creek Basin, Colorado, 2010–2012

USGS Publications Warehouse

Bruce, James F.; Roberts, James J.; Zuellig, Robert E.

2018-05-24

The U.S. Geological Survey (USGS), in cooperation with Colorado Springs City Engineering and Colorado Springs Utilities, analyzed previously collected invertebrate data to determine the comparability among four sampling methods and two versions (2010 and 2017) of the Colorado Benthic Macroinvertebrate Multimetric Index (MMI). For this study, annual macroinvertebrate samples were collected concurrently (in space and time) at 15 USGS surface-water gaging stations in the Fountain Creek Basin from 2010 to 2012 using four sampling methods. The USGS monitoring project in the basin uses two of the methods and the Colorado Department of Public Health and Environment recommends the other two. These methods belong to two distinct sample types, one that targets single habitats and one that targets multiple habitats. The study results indicate that there are significant differences in MMI values obtained from the single-habitat and multihabitat sample types but methods from each program within each sample type produced comparable values. This study also determined that MMI values calculated by different versions of the Colorado Benthic Macroinvertebrate MMI are indistinguishable. This indicates that the Colorado Department of Public Health and Environment methods are comparable with the USGS monitoring project methods for single-habitat and multihabitat sample types. This report discusses the direct application of the study results to inform the revision of the existing USGS monitoring project in the Fountain Creek Basin.

Cross Validation of Two Partitioning-Based Sampling Approaches in Mesocosms Containing PCB Contaminated Field Sediment, Biota, and Activated Carbon Amendment.

PubMed

Schmidt, Stine N; Wang, Alice P; Gidley, Philip T; Wooley, Allyson H; Lotufo, Guilherme R; Burgess, Robert M; Ghosh, Upal; Fernandez, Loretta A; Mayer, Philipp

2017-09-05

The Gold Standard for determining freely dissolved concentrations (C free ) of hydrophobic organic compounds in sediment interstitial water would be in situ deployment combined with equilibrium sampling, which is generally difficult to achieve. In the present study, ex situ equilibrium sampling with multiple thicknesses of silicone and in situ pre-equilibrium sampling with low density polyethylene (LDPE) loaded with performance reference compounds were applied independently to measure polychlorinated biphenyls (PCBs) in mesocosms with (1) New Bedford Harbor sediment (MA, U.S.A.), (2) sediment and biota, and (3) activated carbon amended sediment and biota. The aim was to cross validate the two different sampling approaches. Around 100 PCB congeners were quantified in the two sampling polymers, and the results confirmed the good precision of both methods and were in overall good agreement with recently published LDPE to silicone partition ratios. Further, the methods yielded C free in good agreement for all three experiments. The average ratio between C free determined by the two methods was factor 1.4 ± 0.3 (range: 0.6-2.0), and the results thus cross-validated the two sampling approaches. For future investigations, specific aims and requirements in terms of application, data treatment, and data quality requirements should dictate the selection of the most appropriate partitioning-based sampling approach.

RAPID DETERMINATION OF RA-226 IN ENVIRONMENTAL SAMPLES

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

Maxwell, S.

2012-01-03

A new rapid method for the determination of {sup 226}Ra in environmental samples has been developed at the Savannah River Site Environmental Lab (Aiken, SC, USA) that can be used for emergency response or routine sample analyses. The need for rapid analyses in the event of a Radiological Dispersive Device or Improvised Nuclear Device event is well-known. In addition, the recent accident at Fukushima Nuclear Power Plant in March, 2011 reinforces the need to have rapid analyses for radionuclides in environmental samples in the event of a nuclear accident. {sup 226}Ra (T1/2 = 1,620 years) is one of the mostmore » toxic of the long-lived alpha-emitters present in the environment due to its long life and its tendency to concentrate in bones, which increases the internal radiation dose of individuals. The new method to determine {sup 226}Ra in environmental samples utilizes a rapid sodium hydroxide fusion method for solid samples, calcium carbonate precipitation to preconcentrate Ra, and rapid column separation steps to remove interferences. The column separation process uses cation exchange resin to remove large amounts of calcium, Sr Resin to remove barium and Ln Resin as a final purification step to remove {sup 225}Ac and potential interferences. The purified {sup 226}Ra sample test sources are prepared using barium sulfate microprecipitation in the presence of isopropanol for counting by alpha spectrometry. The method showed good chemical recoveries and effective removal of interferences. The determination of {sup 226}Ra in environmental samples can be performed in less than 16 h for vegetation, concrete, brick, soil, and air filter samples with excellent quality for emergency or routine analyses. The sample preparation work takes less than 6 h. {sup 225}Ra (T1/2 = 14.9 day) tracer is used and the {sup 225}Ra progeny {sup 217}At is used to determine chemical yield via alpha spectrometry. The rapid fusion technique is a rugged sample digestion method that ensures that any refractory radium particles are effectively digested. The preconcentration and column separation steps can also be applied to aqueous samples with good results.« less

A method of discriminating transuranic radionuclides from radon progeny using low-resolution alpha spectroscopy and curve-fitting techniques.

PubMed

Konzen, Kevin; Brey, Richard

2012-05-01

²²²Rn (radon) and ²²⁰Rn (thoron) progeny are known to interfere with determining the presence of long-lived transuranic radionuclides, such as plutonium and americium, and require from several hours up to several days for conclusive results. Methods are proposed that should expedite the analysis of air samples for determining the amount of transuranic radionuclides present using low-resolution alpha spectroscopy systems available from typical alpha continuous air monitors (CAMs) with multi-channel analyzer (MCA) capabilities. An alpha spectra simulation program was developed in Microsoft Excel visual basic that employed the use of Monte Carlo numerical methods and serial-decay differential equations that resembled actual spectra. Transuranic radionuclides were able to be quantified with statistical certainty by applying peak fitting equations using the method of least squares. Initial favorable results were achieved when samples containing radon progeny were decayed 15 to 30 min, and samples containing both radon and thoron progeny were decayed at least 60 min. The effort indicates that timely decisions can be made when determining transuranic activity using available alpha CAMs with alpha spectroscopy capabilities for counting retrospective air samples if accompanied by analyses that consider the characteristics of serial decay.

Quality assessment of pharmaceutical tablet samples using Fourier transform near infrared spectroscopy and multivariate analysis

NASA Astrophysics Data System (ADS)

Kandpal, Lalit Mohan; Tewari, Jagdish; Gopinathan, Nishanth; Stolee, Jessica; Strong, Rick; Boulas, Pierre; Cho, Byoung-Kwan

2017-09-01

Determination of the content uniformity, assessed by the amount of an active pharmaceutical ingredient (API), and hardness of pharmaceutical materials is important for achieving a high-quality formulation and to ensure the intended therapeutic effects of the end-product. In this work, Fourier transform near infrared (FT-NIR) spectroscopy was used to determine the content uniformity and hardness of a pharmaceutical mini-tablet and standard tablet samples. Tablet samples were scanned using an FT-NIR instrument and tablet spectra were collected at wavelengths of 1000-2500 nm. Furthermore, multivariate analysis was applied to extract the relationship between the FT-NIR spectra and the measured parameters. The results of FT-NIR spectroscopy for API and hardness prediction were as precise as the reference high-performance liquid chromatography and mechanical hardness tests. For the prediction of mini-tablet API content, the highest coefficient of determination for the prediction (R2p) was found to be 0.99 with a standard error of prediction (SEP) of 0.72 mg. Moreover, the standard tablet hardness measurement had a R2p value of 0.91 with an SEP of 0.25 kg. These results suggest that FT-NIR spectroscopy is an alternative and accurate nondestructive measurement tool for the detection of the chemical and physical properties of pharmaceutical samples.

Determination and evaluation of cadmium, copper, nickel, and zinc in agricultural soils of western Macedonia, Greece.

PubMed

Papadopoulos, A; Prochaska, C; Papadopoulos, F; Gantidis, N; Metaxa, E

2007-10-01

The objective of this study was to determine the levels of major phytotoxic metals--including cadmium (Cd), copper (Cu), nickel (Ni), and zinc (Zn)--in agricultural soils of Western Macedonia, Greece. We also wanted to determine the possible relationships among elements and between soil properties and elemental concentrations. Surface soil samples, n = 570, were collected and analyzed. The results of the elemental analysis showed that the mean metal concentrations were consistent with reported typical concentrations found in Greek agricultural soils in the cases of Zn and Cu. Cd exhibited lower and Ni higher mean concentrations than the typical levels reported in the literature. Metal concentrations in the majority of the examined samples (>69%) were found to be higher than the respective critical plant-deficiency levels. However, only 0.4% and 0.2% of the analyzed soil samples, respectively, exhibited Cd and Ni concentrations higher than the levels that cause plant toxicity, as referenced by other investigators. These results suggest that the soils studied can be considered as unpolluted with respect to the examined food-chain metal contaminants. However, the levels of the metal concentrations in some of the soil samples, and the low correlation of the metals with soil properties, suggest an anthropogenic rather that lithogenic origin.

Determination of air-loop volume and radon partition coefficient for measuring radon in water sample.

PubMed

Lee, Kil Yong; Burnett, William C

A simple method for the direct determination of the air-loop volume in a RAD7 system as well as the radon partition coefficient was developed allowing for an accurate measurement of the radon activity in any type of water. The air-loop volume may be measured directly using an external radon source and an empty bottle with a precisely measured volume. The partition coefficient and activity of radon in the water sample may then be determined via the RAD7 using the determined air-loop volume. Activity ratios instead of absolute activities were used to measure the air-loop volume and the radon partition coefficient. In order to verify this approach, we measured the radon partition coefficient in deionized water in the temperature range of 10-30 °C and compared the values to those calculated from the well-known Weigel equation. The results were within 5 % variance throughout the temperature range. We also applied the approach for measurement of the radon partition coefficient in synthetic saline water (0-75 ppt salinity) as well as tap water. The radon activity of the tap water sample was determined by this method as well as the standard RAD-H 2 O and BigBottle RAD-H 2 O. The results have shown good agreement between this method and the standard methods.

Determination of trace metals in spirits by total reflection X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Siviero, G.; Cinosi, A.; Monticelli, D.; Seralessandri, L.

2018-06-01

Eight spirituous samples were analyzed for trace metal content with Horizon Total Reflection X-Ray Fluorescence (TXRF) Spectrometer. The expected single metal amount is at the ng/g level in a mixed aqueous/organic matrix, thus requiring a sample preparation method capable of achieving suitable limits of detection. On-site enrichment and Atmospheric Pressure-Vapor Phase Decomposition allowed to detect Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Sr and Pb with detection limits ranging from 0.1 ng/g to 4.6 ng/g. These results highlight how the synergy between instrument and sample preparation strategy may foster the use of TXRF as a fast and reliable technique for the determination of trace elements in spirituous samples, either for quality control or risk assessment purposes.

Theory and practice in the electrometric determination of pH in precipitation

NASA Astrophysics Data System (ADS)

Brennan, Carla Jo; Peden, Mark E.

Basic theory and laboratory investigations have been applied to the electrometric determination of pH in precipitation samples in an effort to improve the reliability of the results obtained from these low ionic strength samples. The theoretical problems inherent in the measurement of pH in rain have been examined using natural precipitation samples with varying ionic strengths and pH values. The importance of electrode design and construction has been stressed. The proper choice of electrode can minimize or eliminate problems arising from residual liquid junction potentials, streaming potentials and temperature differences. Reliable pH measurements can be made in precipitation samples using commercially available calibration buffers providing low ionic strength quality control solutions are routinely used to verify electrode and meter performance.

Annual radiological environmental operating report, Browns Ferry Nuclear Plant, 1991

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

Not Available

1992-04-01

This report describes the environmental radiological monitoring program conducted by TVA in the vicinity of Browns Ferry Nuclear Plant in 1991. The program includes the collection of samples from the environment and the determination of the concentrations of radioactive materials in the samples. Samples are taken from stations in the general area of the plant and from areas not influenced by plant operations. Station locations are selected after careful consideration of the weather patterns and projected radiation doses to the various areas around the plant. Material sampled includes air, water, milk, foods, vegetation, soil, fish, sediment, and direct radiation levels.more » Results from stations near the plant are compared with concentrations from control stations and with preoperational measurements to determine potential impacts of plant operations.« less

Simultaneous determination of gross alpha, gross beta and ²²⁶Ra in natural water by liquid scintillation counting.

PubMed

Fons, J; Zapata-García, D; Tent, J; Llauradó, M

2013-11-01

The determination of gross alpha, gross beta and (226)Ra activity in natural waters is useful in a wide range of environmental studies. Furthermore, gross alpha and gross beta parameters are included in international legislation on the quality of drinking water [Council Directive 98/83/EC]. In this work, a low-background liquid scintillation counter (Wallac, Quantulus 1220) was used to simultaneously determine gross alpha, gross beta and (226)Ra activity in natural water samples. Sample preparation involved evaporation to remove (222)Rn and its short-lived decay daughters. The evaporation process concentrated the sample ten-fold. Afterwards, a sample aliquot of 8 mL was mixed with 12 mL of Ultima Gold AB scintillation cocktail in low-diffusion vials. In this study, a theoretical mathematical model based on secular equilibrium conditions between (226)Ra and its short-lived decay daughters is presented. The proposed model makes it possible to determine (226)Ra activity from two measurements. These measurements also allow determining gross alpha and gross beta simultaneously. To validate the proposed model, spiked samples with different activity levels for each parameter were analysed. Additionally, to evaluate the model's applicability in natural water, eight natural water samples from different parts of Spain were analysed. The eight natural water samples were also characterised by alpha spectrometry for the naturally occurring isotopes of uranium ((234)U, (235)U and (238)U), radium ((224)Ra and (226)Ra), (210)Po and (232)Th. The results for gross alpha and (226)Ra activity were compared with alpha spectrometry characterization, and an acceptable concordance was obtained. Copyright © 2013 Elsevier Ltd. All rights reserved.

In vitro production of GHB in blood and serum samples under various storage conditions.

PubMed

Zörntlein, S W; Kopp, A; Becker, J; Kaufmann, T J; Röhrich, J; Urban, R

2012-01-10

The in vitro production of GHB was observed in freshly collected, untreated whole blood samples using glass BD-Vacutainers and polypropylene S-monovettes. GHB concentrations were determined daily over a period of one week and after 3, 6 and 9 weeks again. Furthermore, the GHB concentration in 40 untreated random whole blood samples stored at 4°C for a longer period of time (10 samples 12 month, 10 samples 24 month and 20 samples 36 month) was also determined. For comparison, the in vitro production of GHB in freshly collected and prepared serum samples was observed. GHB serum concentrations were determined three times over a period of one week and once again after six weeks. Sample preparation was performed by means of methanolic extraction following the precipitation of whole blood and serum samples. A methanolic standard calibration was done in a low range of 0.005-0.1 μg/mL (LOD: 0.004, LLOQ: 0.013). For quantification a spiked blood bank serum with a determined GHB concentration of 0.09 μg/mL was used. Corrected calibrations in the range of 0.09-5.09 μg/mL were used (LOD: 0.08 μg/mL, LLOQ: 0.30 μg/mL), recovery: 91.3% (high level: 4.09 μg/mL) 50.5% (low level: 0.19 μg/mL). Relevant elevation of GHB was observed in all whole blood samples stored in liquid form (4°C or room temperature). In two of the 40 whole blood samples stored over a longer period of time at 4°C, GHB concentrations in the range of 13 μg/mL were even determined. These findings constitute grounds for caution. Even a GHB cut-off level of 5 μg/mL cannot be considered as "absolutely positive" proof of a case of exogenous administration, at least in untreated liquid blood samples in long time storage. However, no significant elevations of GHB were otherwise observed in any of the serum samples independently of storage temperature nor in the whole blood samples that were frozen for storage. The results suggest that the cut-off for exogenous GHB of 5 μg/mL could be lowered significantly, with the consequence of winning valuable time for the potential victim, but only if serum is collected for GHB determination or if the whole blood sample is frozen immediately after collection and the procedure well documented. Copyright © 2011 Elsevier Ireland Ltd. All rights reserved.

Chemical Characterization of an Envelope B/D Sample from Hanford Tank 241-AZ-102

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

Hay, M.S.

2000-08-23

A sample from Hanford waste tank 241-AZ-102 was received at the Savannah River Technology Center (SRTC) and chemically characterized. The sample containing supernate and a small amount of sludge solids was analyzed as-received. The filtered supernatant liquid, the total dried solids of the sample, and the washed insoluble solids obtained from filtration of the sample were analyzed. A mass balance calculation of the three fractions of the sample analyzed indicate the analytical results appear relatively self-consistent for major components of the sample. However, some inconsistency was observed between results were more than one method of determination was employed and formore » species present in low concentrations. The actinides isotopes, plutonium, americium, and curium, present analytical challenges due to the low concentration of these species and the potential for introduction of small amounts of contamination during sampling handling resulting in large uncertainties. A direct comparison to previous analyses of material from tank 241-AZ-102 showed good agreement with the filtered supernatant liquid. However, the comparison of solids data showed poor agreement. The poor agreement shown between the current results for the solids samples and previous analyses most likely results from the uncertainties associated with obtaining small solids samples from a large non-homogenized waste tank.« less

Development of an automated method for determining oil in water by direct aqueous supercritical fluid extraction coupled on-line with infrared spectroscopy.

PubMed

Minty, B; Ramsey, E D; Davies, I

2000-12-01

A direct aqueous supercritical fluid extraction (SFE) system was developed which can be directly interfaced to an infrared spectrometer for the determination of oil in water. The technique is designed to provide an environmentally clean, automated alternative to established IR methods for oil in water analysis which require the use of restricted organic solvents. The SFE-FTIR method involves minimum sample handling stages, with on-line analysis of a 500 ml water sample being complete within 15 min. Method accuracy for determining water samples spiked with gasoline, white spirit, kerosene, diesel or engine oil was 81-100% with precision (RSD) ranging from 3 to 17%. An independent evaluation determined a 2 ppm limit of quantification for diesel in industrial effluents. The results of a comparative study involving an established IR method and the SFE-FTIR method indicate that oil levels calculated using an accepted equation which includes coefficients derived from reference hydrocarbon standards may result in significant errors. A new approach permitted the derivation of quantification coefficients for the SFE-FTIR analyses which provided improved results. In situations where the identity of the oil to be analysed is known, a rapid off-line SFE-FTIR system calibration procedure was developed and successfully applied to various oils. An optional in-line silica gel clean-up procedure incorporated within the SFE-FTIR system enables the same water sample to be analysed for total oil content including vegetable oils and selectively for petroleum oil content within a total of 20 min. At the end of an analysis the SFE system is cleaned using an in situ 3 min clean cycle.

Quality-assurance data for routine water analysis in the National Water-Quality Laboratory of the US Geological Survey for water year 1988

USGS Publications Warehouse

Lucey, K.J.

1989-01-01

The US Geological Survey maintains a quality assurance program based on the analysis of reference samples for its National Water Quality Laboratory located in Denver, Colorado. Reference samples containing selected inorganic, nutrient, and precipitation (low-level concentration) constituents are prepared at the Survey 's Water Quality Services Unit in Ocala, Florida, disguised as routine samples, and sent daily or weekly, as appropriate, to the laboratory through other Survey offices. The results are stored permanently in the National Water Data Storage and Retrieval System (WATSTORE), the Survey 's database for all water data. These data are analyzed statistically for precision and bias. An overall evaluation of the inorganic major ion and trace metal constituent data for water year 1988 indicated a lack of precision in the National Water Quality Laboratory for the determination of 8 out of 58 constituents: calcium (inductively coupled plasma emission spectrometry), fluoride, iron (atomic absorption spectrometry), iron (total recoverable), magnesium (atomic absorption spectrometry), manganese (total recoverable), potassium, and sodium (inductively coupled plasma emission spectrometry). The results for 31 constituents had positive or negative bias during water year 1988. A lack of precision was indicated in the determination of three of the six nutrient constituents: nitrate plus nitrite nitrogen as nitrogen, nitrite nitrogen as nitrogen, and orthophosphate as phosphorus. A biased condition was indicated in the determination of ammonia nitrogen as nitrogen, ammonia plus organic nitrogen as nitrogen, and nitrate plus nitrite nitrogen as nitrogen. There was acceptable precision in the determination of all 10 constituents contained in precipitation samples. Results for ammonia nitrogen as nitrogen, sodium, and fluoride indicated a biased condition. (Author 's abstract)

77 FR 26292 - Risk Evaluation and Mitigation Strategy Assessments: Social Science Methodologies to Assess Goals...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-05-03

... determine endpoints; questionnaire design and analyses; and presentation of survey results. To date, FDA has..., the workshop will invest considerable time in identifying best methodological practices for conducting... sample, sample size, question design, process, and endpoints. Panel 2 will focus on alternatives to...

Outgassing tests on iras solar panel samples

NASA Technical Reports Server (NTRS)

Premat, G.; Zwaal, A.; Pennings, N. H.

1980-01-01

Several outgassing tests were carried out on representative solar panel samples in order to determine the extent of contamination that could be expected from this source. The materials for the construction of the solar panels were selected as a result of contamination obtained in micro volatile condensable materials tests.

Quality assurance in the determination of metals in clinical chemistry and toxicology: the METOS project. Metalli Tossici.

PubMed

Patriarca, M; Menditto, A; Morisi, G

1995-01-01

National external quality assessment schemes (EQAS) for the determination of trace elements in blood (Al, Cd, Cu, Pb, Zn) have been promoted in Italy since 1983. They were organized by a working group of the Istituto Superiore di Sanità and known as "METOS (Metalli Tossici, toxic metals) project". The organization of the schemes included the preparation of suitable control materials by the promoting centre and the elaboration of valuable strategies of sample distribution, treatment of data and evaluation of results, that could be applied even to a small number of participants. The procedures used and the results obtained in ten years of activity of the METOS project are reported. Within the framework of the programme some information has been obtained, confirming the validity of the procedures used for sample preparation, sample distribution and evaluation of laboratories performance.

Studies on the Evaluation Methods for the Food Quality with a Non-contact type Capacitance Sensor.

NASA Astrophysics Data System (ADS)

Narumiya, Tadaoki; Hagura, Yoshio

Changes of capacitance and temperature of ethyl alcohol, hamburger and dough with cheese filling were measured with specially-made measuring devices during the freezing and thawing. The results of measurement of capacitance and temperature suggest a linear correlation for ethyl alcohol as a single constituent substance. The adequate correlation is too estimated from the results of food samples, though the capacitance of food sample varies greatly at the start and end of freezing and thawing process. It has been demonstrated that the quality or physical condition of food sample can be determined easily by the measurement of capacitance using the specially-made devices. Also the quality or physical condition of food can be determined easily by the non-contact and non-destructive measurements of capacitance. A variety application of the present technique is conceivable for the process control of the freezing and thawing foods.

Identification of heavy metals on vegetables at the banks of Kaligarang river using neutron analysis activation method

NASA Astrophysics Data System (ADS)

Yulianti, D.; Marwoto, P.; Fianti

2018-03-01

This research aims to determine the type, concentration, and distribution of heavy metals in vegetables on the banks river Kaligarang using Neutron Analysis Activation (NAA) Method. The result is then compared to its predefined threshold. Vegetable samples included papaya leaf, cassava leaf, spinach, and water spinach. This research was conducted by taking a snippet of sediment and vegetation from 4 locations of Kaligarang river. These snippets are then prepared for further irradiated in the reactor for radioactive samples emiting γ-ray. The level of γ-ray energy determines the contained elements of sample that would be matched to Neutron Activation Table. The results showed that vegetablesat Kaligarang are containing Cr-50, Co-59, Zn-64, Fe-58, and Mn-25, and well distributed at all research locations. Furthermore, the level of the detected metal elements is less than the predefined threshold.

[Determination of acidity and vitamin C in apples using portable NIR analyzer].

PubMed

Yang, Fan; Li, Ya-Ting; Gu, Xuan; Ma, Jiang; Fan, Xing; Wang, Xiao-Xuan; Zhang, Zhuo-Yong

2011-09-01

Near infrared (NIR) spectroscopy technology based on a portable NIR analyzer, combined with kernel Isomap algorithm and generalized regression neural network (GRNN) has been applied to establishing quantitative models for prediction of acidity and vitamin C in six kinds of apple samples. The obtained results demonstrated that the fitting and the predictive accuracy of the models with kernel Isomap algorithm were satisfactory. The correlation between actual and predicted values of calibration samples (R(c)) obtained by the acidity model was 0.999 4, and for prediction samples (R(p)) was 0.979 9. The root mean square error of prediction set (RMSEP) was 0.055 8. For the vitamin C model, R(c) was 0.989 1, R(p) was 0.927 2, and RMSEP was 4.043 1. Results proved that the portable NIR analyzer can be a feasible tool for the determination of acidity and vitamin C in apples.

Lessons learned from surface wipe sampling for lead in three workplaces.

PubMed

Beaucham, Catherine; Ceballos, Diana; King, Bradley

2017-08-01

Surface wipe sampling in the occupational environment is a technique widely used by industrial hygienists. Although several organizations have promulgated standards for sampling lead and other metals, uncertainty still exists when trying to determine an appropriate wipe sampling strategy and how to interpret sampling results. Investigators from the National Institute for Occupational Safety and Health (NIOSH) Health Hazard Evaluation Program have used surface wipe sampling as part of their exposure assessment sampling strategies in a wide range of workplaces. This article discusses wipe sampling for measuring lead on surfaces in three facilities: (1) a battery recycling facility; (2) a firing range and gun store; and (3) an electronic scrap recycling facility. We summarize our findings from the facilities and what we learned by integrating wipe sampling into our sampling plan. Wiping sampling demonstrated lead in non-production surfaces in all three workplaces and that the potential that employees were taking lead home to their families existed. We also found that the presence of metals such as tin can interfere with the colorimetric results. We also discuss the advantages and disadvantages of colorimetric analysis of surface wipe samples and the challenges we faced when interpreting wipe sampling results.

Fast batch injection analysis system for on-site determination of ethanol in gasohol and fuel ethanol.

PubMed

Pereira, Polyana F; Marra, Mariana C; Munoz, Rodrigo A A; Richter, Eduardo M

2012-02-15

A simple, accurate and fast (180 injections h(-1)) batch injection analysis (BIA) system with multiple-pulse amperometric detection has been developed for selective determination of ethanol in gasohol and fuel ethanol. A sample aliquot (100 μL) was directly injected onto a gold electrode immersed in 0.5 mol L(-1) NaOH solution (unique reagent). The proposed BIA method requires minimal sample manipulation and can be easily used for on-site analysis. The results obtained with the BIA method were compared to those obtained by gas-chromatography and similar results were obtained (at 95% of confidence level). Published by Elsevier B.V.

Rapid determination of Faraday rotation in optical glasses by means of secondary Faraday modulator.

PubMed

Sofronie, M; Elisa, M; Sava, B A; Boroica, L; Valeanu, M; Kuncser, V

2015-05-01

A rapid high sensitive method for determining the Faraday rotation of optical glasses is proposed. Starting from an experimental setup based on a Faraday rod coupled to a lock-in amplifier in the detection chain, two methodologies were developed for providing reliable results on samples presenting low and large Faraday rotations. The proposed methodologies were critically discussed and compared, via results obtained in transmission geometry, on a new series of aluminophosphate glasses with or without rare-earth doping ions. An example on how the method can be used for a rapid examination of the optical homogeneity of the sample with respect to magneto-optical effects is also provided.

Determining Consumer Preference for Furniture Product Characteristics

ERIC Educational Resources Information Center

Turner, Carolyn S.; Edwards, Kay P.

1974-01-01

The paper describes instruments for determining preferences of consumers for selected product characteristics associated with furniture choices--specifically style, color, color scheme, texture, and materials--and the procedures for administration of those instruments. Results are based on a random sampling of public housing residents. (Author/MW)

Legionella in water samples: how can you interpret the results obtained by quantitative PCR?

PubMed

Ditommaso, Savina; Ricciardi, Elisa; Giacomuzzi, Monica; Arauco Rivera, Susan R; Zotti, Carla M

2015-02-01

Evaluation of the potential risk associated with Legionella has traditionally been determined from culture-based methods. Quantitative polymerase chain reaction (qPCR) is an alternative tool that offers rapid, sensitive and specific detection of Legionella in environmental water samples. In this study we compare the results obtained by conventional qPCR (iQ-Check™ Quanti Legionella spp.; Bio-Rad) and by culture method on artificial samples prepared in Page's saline by addiction of Legionella pneumophila serogroup 1 (ATCC 33152) and we analyse the selective quantification of viable Legionella cells by the qPCR-PMA method. The amount of Legionella DNA (GU) determined by qPCR was 28-fold higher than the load detected by culture (CFU). Applying the qPCR combined with PMA treatment we obtained a reduction of 98.5% of the qPCR signal from dead cells. We observed a dissimilarity in the ability of PMA to suppress the PCR signal in samples with different amounts of bacteria: the effective elimination of detection signals by PMA depended on the concentration of GU and increasing amounts of cells resulted in higher values of reduction. Using the results from this study we created an algorithm to facilitate the interpretation of viable cell level estimation with qPCR-PMA. Copyright © 2014 Elsevier Ltd. All rights reserved.

Validation of feasibility and quality of chicken breast meat cooked under various water-cooking conditions.

PubMed

Chumngoen, Wanwisa; Chen, Hsin-Yi; Tan, Fa-Jui

2016-12-01

Under laboratory conditions, the qualities of boneless chicken breasts are commonly determined by placing them in a bag and cooking them in a water bath. The results are often applied as references for comparing the influences of cooking techniques. However, whether a sample cooked under this "laboratory" condition actually represents the meat cooked under the "real-life" condition in which meat is frequently cooked directly in water without packaging remains unclear. Whether the two cooking conditions lead to comparable results in meat quality should be determined. This study evaluated the influence of cooking conditions, including "placed-in-bag and cooked in a water bath (BC)" and "cooked directly in hot water (WC)" conditions, on the quality of chicken meat. The results reveal that BC samples had a longer cooking time. Deboned-and-skinless BC samples had a higher cooking loss and lower protein solubility (P < 0.01). BC samples with bone and skin had a higher lightness in both skin and muscle. No significant differences were observed in attributes, including shear force, collagen solubility, microstructures, redness, yellowness and descriptive sensory characteristics between treatments. Based on the results, considering the quality attributes that might be influenced, is critical when conducting relevant research. © 2016 Japanese Society of Animal Science.

An on-line potentiometric sequential injection titration process analyser for the determination of acetic acid.

PubMed

van Staden, J F; Mashamba, Mulalo G; Stefan, Raluca I

2002-09-01

An on-line potentiometric sequential injection titration process analyser for the determination of acetic acid is proposed. A solution of 0.1 mol L(-1) sodium chloride is used as carrier. Titration is achieved by aspirating acetic acid samples between two strong base-zone volumes into a holding coil and by channelling the stack of well-defined zones with flow reversal through a reaction coil to a potentiometric sensor where the peak widths were measured. A linear relationship between peak width and logarithm of the acid concentration was obtained in the range 1-9 g/100 mL. Vinegar samples were analysed without any sample pre-treatment. The method has a relative standard deviation of 0.4% with a sample frequency of 28 samples per hour. The results revealed good agreement between the proposed sequential injection and an automated batch titration method.

Surface-water-quality assessment of the upper Illinois River Basin in Illinois, Indiana, and Wisconsin; data on agricultural organic compounds, nutrients, and sediment in water, 1988-90

USGS Publications Warehouse

Sullivan, D.J.; Terrio, P.J.

1994-01-01

This report describes the sampling design and methods and presents data collected to determine the distribution of agricultural organic compounds, nutrients, and sediment in selected areas of the upper Illinois River Basin as part of the National Water-Quality Assessment program. Four stations in small watersheds (two urban, two agricultural) were sampled in 1988 and 1989. Seventeen stations in an agricultural subbasin were sampled in 1990. Samples were collected before, during, and after runoff events from late spring to midsummer to determine concentrations of agricultural organic compounds in surface waters resulting from storm runoff, as well as background concentrations. Over 200 water samples were analyzed for agricultural organic compound, nutrient, and suspended-sediment concentrations. The agricultural organic compounds included triazine and chlorophenoxy-acid herbicides, and organo-phosphorus insecticides.

Optoelectronic system of online measurements of unburned carbon in coal fly ash

NASA Astrophysics Data System (ADS)

Golas, Janusz; Jankowski, Henryk; Niewczas, Bogdan; Piechna, Janusz; Skiba, Antoni; Szkutnik, Wojciech; Szkutnik, Zdzislaw P.; Wartak, Ryszarda; Worek, Cezary

2001-08-01

Carbon-in-ash level is an important consideration for combustion efficiency as well as ash marketing. The optoelectronic analyzing system for on-line determination and monitoring of the u burned carbon content of ash samples is presented. The apparatus operates on the principle that carbon content is proportional to the reflectance of IR light. Ash samples are collected iso kinetically from the flue gas duct and placed in a sample tube with a flat glass bottom. The same is then exposed to a light. The reflectance intensity is used by the system's computer to determine residual carbon content from correlation curves. The sample is then air purged back to the duct or to the attached sample canister to enable laboratory check analysis. The total cycle time takes between 5 and 10 minutes. Real time result of carbon content with accuracy 0.3-0.7 percent are reported and can be used for boiler controlling.

A novel method for the determination of chemical purity and assay of menaquinone-7. Comparison with the methods from the official USP monograph.

PubMed

Jedynak, Łukasz; Jedynak, Maria; Kossykowska, Magdalena; Zagrodzka, Joanna

2017-02-20

An HPLC method with UV detection and separation with the use of a C30 reversed phase analytical column for the determination of chemical purity and assay of menaquinone-7 (MK7) in one chromatographic run was developed. The method is superior to the methods published in the USP Monograph in terms of selectivity, sensitivity and accuracy, as well as time, solvent and sample consumption. The developed methodology was applied to MK7 samples of active pharmaceutical ingredient (API) purity, MK7 samples of lower quality and crude MK7 samples before purification. The comparison of the results revealed that the use of USP methodology could lead to serious overestimation (up to a few percent) of both purity and MK7 assay in menaquinone-7 samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Cocaine abuse determination by ion mobility spectrometry using molecular imprinting.

PubMed

Sorribes-Soriano, A; Esteve-Turrillas, F A; Armenta, S; de la Guardia, M; Herrero-Martínez, J M

2017-01-20

A cocaine-based molecular imprinted polymer (MIP) has been produced by bulk polymerization and employed as selective solid-phase extraction support for the determination of cocaine in saliva samples by ion mobility spectrometry (IMS). The most appropriate conditions for washing and elution of cocaine from MIPs were studied and MIPs were characterized in terms of analyte binding capacity, reusability in water and saliva analysis, imprinting factor and selectivity were established and compared with non-imprinted polymers. The proposed MIP-IMS method provided a LOD of 18μgL -1 and quantitative recoveries for blank saliva samples spiked from 75 to 500μgL -1 cocaine. Oral fluid samples were collected from cocaine consumers and analysed by the proposed MIP-IMS methodology. Results, ranging from below the LOD to 51±2mgL -1 , were statistically comparable to those obtained by a confirmatory gas chromatography-mass spectrometry method. Moreover, results were compared to a qualitative lateral flow immunoassay procedure providing similar classification of the samples. Thus, MIP-IMS can be considered an useful alternative that provided fast, selective and sensitive results with a cost affordable instrumentation that does not require skilled operators. Copyright © 2016 Elsevier B.V. All rights reserved.

An Environmental Friendly Procedure for Photometric Determination of Hypochlorite in Tap Water Employing a Miniaturized Multicommuted Flow Analysis Setup

PubMed Central

Borges, Sivanildo S.; Reis, Boaventura F.

2011-01-01

A photometric procedure for the determination of ClO− in tap water employing a miniaturized multicommuted flow analysis setup and an LED-based photometer is described. The analytical procedure was implemented using leucocrystal violet (LCV; 4,4′,4′′-methylidynetris (N,N-dimethylaniline), C25H31N3) as a chromogenic reagent. Solenoid micropumps employed for solutions propelling were assembled together with the photometer in order to compose a compact unit of small dimensions. After control variables optimization, the system was applied for the determination of ClO− in samples of tap water, and aiming accuracy assessment samples were also analyzed using an independent method. Applying the paired t-test between results obtained using both methods, no significant difference at the 95% confidence level was observed. Other useful features include low reagent consumption, 2.4 μg of LCV per determination, a linear response ranging from 0.02 up to 2.0 mg L−1  ClO−, a relative standard deviation of 1.0% (n = 11) for samples containing 0.2 mg L−1  ClO−, a detection limit of 6.0 μg L−1  ClO−, a sampling throughput of 84 determinations per hour, and a waste generation of 432 μL per determination. PMID:21747732

Determination of microbiological and chemical properties of probiotic boza and its consumer acceptability.

PubMed

Arslan, Sultan; Durak, Atike N; Erbas, Mustafa; Tanriverdi, Emel; Gulcan, Ummugulsum

2015-01-01

The aim of research was producing boza as a probiotic product with certificated probiotic starter cultures (Lactobacillus acidophilus LA-5 and Bifidobacterium bifidum BB-12 and Saccharomyces boulardii). Analysis were done in boza samples taken in fermentation and storage. Probiotic and non-probiotic bacteria were enumerated with pour plate technique and yeast enumerated spread plate technique. Sugar, organic acid and Water soluble vitamin content were determined by using of HPLC. Sensory analyses were done by two different types of panels, once comprised of trained panelists and the other of consumers. Shelf life was determined according the results of sensory analysis. It was determinated that S. boulardii and L acidophilius counts increased nearly 0.5 log unit during of boza fermentation. Lactic, acetic, citric, butyric and succinic acid as organic acids and thiamin, niacin, B6 and pantothenic acid as water soluble vitamin evaluated in boza samples. Shelf life of the probiotic boza determined as 12 days at +4°C fridge storage temperature. The boza samples had a probiotic effect because it had viable microorganisms more than 10(6) cfu/ml which was defined enough for functional foods. All boza samples had lower pH value than 4.5, so it is evaluated that boza is a safety food as its low pH preventing pathogen growth.

Gas-diffusion microextraction coupled with spectrophotometry for the determination of formaldehyde in cork agglomerates.

PubMed

Brandão, Pedro F; Ramos, Rui M; Valente, Inês M; Almeida, Paulo J; Carro, Antonia M; Lorenzo, Rosa A; Rodrigues, José A

2017-04-01

In this work, a simple methodology was developed for the extraction and determination of free formaldehyde content in cork agglomerate samples. For the first time, gas-diffusion microextraction was used for the extraction of volatile formaldehyde directly from samples, with simultaneous derivatization with acetylacetone (Hantzsch reaction). The absorbance of the coloured solution was read in a spectrophotometer at 412 nm. Different extraction parameters were studied and optimized (extraction temperature, sample mass, volume of acceptor solution, extraction time and concentration of derivatization reagent) by means of an asymmetric screening. The developed methodology proved to be a reliable tool for the determination of formaldehyde in cork agglomerates with the following suitable method features: low LOD (0.14 mg kg -1 ) and LOQ (0.47 mg kg -1 ), r 2  = 0.9994, and intraday and interday precision of 3.5 and 4.9%, respectively. The developed methodology was applied to the determination of formaldehyde in different cork agglomerate samples, and contents between 1.9 and 9.4 mg kg -1 were found. Furthermore, formaldehyde was also determined by the standard method EN 717-3 for comparison purposes; no significant differences between the results of both methods were observed. Graphical abstract Representation of the GDME system and its main components.

Genetic analysis of 7 medieval skeletons from Aragonese Pyrenees

PubMed Central

Núńez, Carolina; Sosa, Cecilia; Baeta, Miriam; Geppert, Maria; Turnbough, Meredith; Phillips, Nicole; Casalod, Yolanda; Bolea, Miguel; Roby, Rhonda; Budowle, Bruce; Martínez-Jarreta, Begońa

2011-01-01

Aim To perform a genetic characterization of 7 skeletons from medieval age found in a burial site in the Aragonese Pyrenees. Methods Allele frequencies of autosomal short tandem repeats (STR) loci were determined by 3 different STR systems. Mitochondrial DNA (mtDNA) and Y-chromosome haplogroups were determined by sequencing of the hypervariable segment 1 of mtDNA and typing of phylogenetic Y chromosome single nucleotide polymorphisms (Y-SNP) markers, respectively. Possible familial relationships were also investigated. Results Complete or partial STR profiles were obtained in 3 of the 7 samples. Mitochondrial DNA haplogroup was determined in 6 samples, with 5 of them corresponding to the haplogroup H and 1 to the haplogroup U5a. Y-chromosome haplogroup was determined in 2 samples, corresponding to the haplogroup R. In one of them, the sub-branch R1b1b2 was determined. mtDNA sequences indicated that some of the individuals could be maternally related, while STR profiles indicated no direct family relationships. Conclusions Despite the antiquity of the samples and great difficulty that genetic analyses entail, the combined use of autosomal STR markers, Y-chromosome informative SNPs, and mtDNA sequences allowed us to genotype a group of skeletons from the medieval age. PMID:21674829

Performance evaluation of laser induced breakdown spectroscopy in the measurement of liquid and solid samples

NASA Astrophysics Data System (ADS)

Bilge, Gonca; Sezer, Banu; Boyaci, Ismail Hakki; Eseller, Kemal Efe; Berberoglu, Halil

2018-07-01

Liquid analysis by using LIBS is a complicated process due to difficulties encountered during the collection of light and formation of plasma in liquid. To avoid these, some applications are performed such as aerosol formation and transforming liquid into solid state. However, performance of LIBS in liquid samples still remains a challenging issue. In this study, performance evaluation of LIBS and parameter optimizations in liquid and solid phase samples were performed. For this purpose, milk was chosen as model sample; milk powder was used as solid sample, and milk was used as liquid sample in the experiments. Different experimental setups have been constructed for each sampling technique, and optimizations were performed to determine suitable parameters such as delay time, laser energy, repetition rate and speed of rotary table for solid sampling technique, and flow rate of carrier gas for liquid sampling technique. Target element was determined as Ca, which is a critically important element in milk for determining its nutritional value and Ca addition. In optimum parameters, limit of detection (LOD), limit of quantification (LOQ) and relative standard deviation (RSD) values were calculated as 0.11%, 0.36% and 8.29% respectively for milk powders samples; while LOD, LOQ and RSD values were calculated as 0.24%, 0.81%, and 10.93% respectively for milk samples. It can be said that LIBS is an applicable method in both liquid and solid samples with suitable systems and parameters. However, liquid analysis requires much more developed systems for more accurate results.

Capillary electrophoresis coupled with electrochemiluminescence for determination of atomoxetine hydrochloride and the study on its interactions with three proteins.

PubMed

Zeng, Hua-jin; Yang, Ran; Zhang, Ying; Li, Jian-jun; Qu, Ling-bo

2015-03-01

A simple, rapid and sensitive method for the determination of atomoxetine hydrochloride (AH) by capillary electrophoresis with electrochemiluminescence detection (CE-ECL) using tris(2,2'-bipyridyl) ruthenium (II) was developed. Under optimized conditions, the determinations of AH in capsules and rat plasmas and the study on its interactions with three plasma proteins, including bovine serum albumin, cytochrome c and myoglobin were performed successfully. Relative to some previous studies, in this paper the methodologies for the determination of AH in aqueous solution and spiked plasma systems were established, respectively. By comparing the difference between the two work curves of two systems, the matrix effect in plasma samples on the determination of AH by the CE-ECL method was discussed in detail. The results indicated that the effect of the matrix in plasma samples should not be ignored even if no obvious interference was found in the electropherograms and the establishment of method validation in complex samples by the CE-ECL method was necessary. Copyright © 2014 John Wiley & Sons, Ltd.

Residual stresses in continuous graphite fiber Al metal matrix composites

NASA Technical Reports Server (NTRS)

Park, Hun Sub; Zong, Gui Sheng; Marcus, Harris L.

1988-01-01

The residual stresses in graphite fiber reinforced aluminum (Gr/Al) composites with various thermal histories are measured using X-ray diffraction (XRD) methods. The XRD stress analysis is based on the determination of lattice strains by precise measurements of the interplanar spacings in different directions of the sample. The sample is a plate consisting of two-ply P 100 Gr/Al 6061 precursor wires and Al 6061 overlayers. Prior to XRD measurement, the 6061 overlayers are electrochemically removed. In order to calibrate the relationship between stress magnitude and lattice spacing shift, samples of Al 6061 are loaded at varying stress levels in a three-point bend fixture, while the stresses are simultaneously determined by XRD and surface-attached strain gages. The stresses determined by XRD closely match those determined by the strain gages. Using these calibrations, the longitudinal residual stresses of P 100 Gr/Al 6061 composites are measured for various heat treatments, and the results are presented.

Measurements of Shock Effects Recorded by Hayabusa Samples

NASA Technical Reports Server (NTRS)

Zolensky, Michael; Mikouchi, Takashi; Hagiya, Kenji; Ohsumi, Kazumasa; Martinez, James; Komatsu, Mutsumi; Chan, Queenie H-.S.

2015-01-01

We requested and have been approved for 5 Hayabusa samples in order definitively establish the degree of shock experienced by the regolith of asteroid Itokawa, and to devise a bridge between shock determinations by standard light optical petrography, crystal structures as determined by synchrotron X-ray diffraction (SXRD), and degree of crystallinity as determined by electron back-scattered diffraction (EBSD) [1,2]. As of the writing of this abstract we are awaiting the approved samples. We propose measurements of astromaterial crystal structures and regolith processes. The proposed research work will improve our understanding of how small, primitive solar system bodies formed and evolved, and improve understanding of the processes that determine the history and future of habitability of environments on other solar system bodies. The results of the proposed research will directly enrich the ongoing asteroid and comet exploration missions by NASA, JAXA and ESA, and broaden our understanding of the origin and evolution of small bodies in the early solar system, and elucidate the nature of asteroid and comet regolith.

Measurements of Shock Effects Recorded by Itokawa Samples

NASA Technical Reports Server (NTRS)

Zolensky, Michael; Mikouchi, Takashi; Hagiya, Kenji; Ohsumi, Kazumasa; Martinez, James; Komatsu, Mutsumi; Chan, Queenie H-.S.

2016-01-01

We requested and have been approved for 5 Hayabusa samples in order definitively establish the degree of shock experienced by the regolith of asteroid Itokawa, and to devise a bridge between shock determinations by standard light optical petrography, crystal structures as determined by synchrotron X-ray diffraction (SXRD), and degree of crystallinity as determined by electron back-scattered diffraction (EBSD). As of the writing of this abstract we are awaiting the approved samples. We propose measurements of astromaterial crystal structures and regolith processes. The proposed research work will improve our understanding of how small, primitive solar system bodies formed and evolved, and improve understanding of the processes that determine the history and future of habitability of environments on other solar system bodies. The results of the proposed research will directly enrich the ongoing asteroid and comet exploration missions by NASA, JAXA and ESA, and broaden our understanding of the origin and evolution of small bodies in the early solar system, and elucidate the nature of asteroid and comet regolith.

Development and validation of a magnetic solid-phase extraction with high-performance liquid chromatography method for the simultaneous determination of amphetamine and methadone in urine.

PubMed

Taghvimi, Arezou; Hamishehkar, Hamed; Ebrahimi, Mahmoud

2016-06-01

The simultaneous determination of amphetamine and methadone was carried out by magnetic graphene oxide nanoparticles, a magnetic solid-phase extraction adsorbent, as a new sample treatment technique. The main factors (the amounts of sample volume, amount of adsorbent, type and amount of extraction organic solvent, time of extraction and desorption, pH, the ionic strength of extraction medium, and agitation rate) influencing the extraction efficiency were investigated and optimized. Under the optimized conditions, good linearity was observed in the range of 100-1500 ng/mL for amphetamine and 100-1000 ng/mL for methadone. The method was evaluated for determination of AM and methadone in positive urine samples, satisfactory results were obtained, therefore magnetic solid-phase extraction can be applied as a novel method for the determination of drugs of abuse in forensic laboratories. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous determination of rare earth elements in ore and anti-corrosion coating samples using a portable capillary electrophoresis instrument with contactless conductivity detection.

PubMed

Nguyen, Thi Anh Huong; Nguyen, Van Ri; Le, Duc Dung; Nguyen, Thi Thanh Binh; Cao, Van Hoang; Nguyen, Thi Kim Dung; Sáiz, Jorge; Hauser, Peter C; Mai, Thanh Duc

2016-07-29

The employment of an in-house-made capillary electrophoresis (CE) instrument with capacitively coupled contactless conductivity detection (C(4)D) as a simple and inexpensive solution for simultaneous determination of many rare earth elements (REEs) in ore samples from Vietnam, as well as in anti-corrosion coating samples is reported. 14 REEs (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu) were determined using an electrolyte composed of 20mM arginine and 10mM α-hydroxyisobutyric acid adjusted to pH 4.2 with acetic acid. The best detection limit achieved was 0.24mg/L using the developed CE-C(4)D method. Good agreement between results from CE-C(4)D and the confirmation method (ICP-MS) was achieved, with a coefficient of determination (r(2)) for the two pairs of data of 0.998. Copyright © 2016 Elsevier B.V. All rights reserved.

Analysis of simplified heat transfer models for thermal property determination of nano-film by TDTR method

NASA Astrophysics Data System (ADS)

Wang, Xinwei; Chen, Zhe; Sun, Fangyuan; Zhang, Hang; Jiang, Yuyan; Tang, Dawei

2018-03-01

Heat transfer in nanostructures is of critical importance for a wide range of applications such as functional materials and thermal management of electronics. Time-domain thermoreflectance (TDTR) has been proved to be a reliable measurement technique for the thermal property determinations of nanoscale structures. However, it is difficult to determine more than three thermal properties at the same time. Heat transfer model simplifications can reduce the fitting variables and provide an alternative way for thermal property determination. In this paper, two simplified models are investigated and analyzed by the transform matrix method and simulations. TDTR measurements are performed on Al-SiO2-Si samples with different SiO2 thickness. Both theoretical and experimental results show that the simplified tri-layer model (STM) is reliable and suitable for thin film samples with a wide range of thickness. Furthermore, the STM can also extract the intrinsic thermal conductivity and interfacial thermal resistance from serial samples with different thickness.

Evaluation of an in-practice wet-chemistry analyzer using canine and feline serum samples.

PubMed

Irvine, Katherine L; Burt, Kay; Papasouliotis, Kostas

2016-01-01

A wet-chemistry biochemical analyzer was assessed for in-practice veterinary use. Its small size may mean a cost-effective method for low-throughput in-house biochemical analyses for first-opinion practice. The objectives of our study were to determine imprecision, total observed error, and acceptability of the analyzer for measurement of common canine and feline serum analytes, and to compare clinical sample results to those from a commercial reference analyzer. Imprecision was determined by within- and between-run repeatability for canine and feline pooled samples, and manufacturer-supplied quality control material (QCM). Total observed error (TEobs) was determined for pooled samples and QCM. Performance was assessed for canine and feline pooled samples by sigma metric determination. Agreement and errors between the in-practice and reference analyzers were determined for canine and feline clinical samples by Bland-Altman and Deming regression analyses. Within- and between-run precision was high for most analytes, and TEobs(%) was mostly lower than total allowable error. Performance based on sigma metrics was good (σ > 4) for many analytes and marginal (σ > 3) for most of the remainder. Correlation between the analyzers was very high for most canine analytes and high for most feline analytes. Between-analyzer bias was generally attributed to high constant error. The in-practice analyzer showed good overall performance, with only calcium and phosphate analyses identified as significantly problematic. Agreement for most analytes was insufficient for transposition of reference intervals, and we recommend that in-practice-specific reference intervals be established in the laboratory. © 2015 The Author(s).

Short communication: determination of potential 5-hydroxymethyl-2-furaldehyde and 2-furaldehyde compounds in follow-on milks and infant formulas using the high-performance liquid chromatography method.

PubMed

Er Demirhan, B; Demirhan, B; Sönmez, C; Torul, H; Tamer, U; Yentür, G

2015-02-01

The aim of present study was to determine the levels of potential 5-hydroxymethyl-2-furaldehyde (HMF) and 2-furaldehyde (F) in 109 baby food samples (60 follow-on milks, 49 cereal- and milk-based infant formulas) obtained from different markets in Ankara (Turkey). Potential HMF and F compounds were determined by HPLC. Mean levels (± standard error) of HMF and F of follow-on milk samples were found to be 237.85±18.25 and 9.44±0.39 µg/100mL, respectively. Regarding the infant formulas, mean levels of HMF and F were found to be 905.41±91.94 and 13.22±1.21 µg/100g. As a result, potential HMF was determined in all of the samples; potential F was determined in all the samples except 1. The mean levels of potential HMF and F of infant formulas were higher than mean levels of potential HMF and F of follow-on milks. In addition, HMF and F values of some samples with an imminent expiration date were found to be higher than HMF and F values of the other samples. At present, no limits have been established in the Turkish Food Codex (TFC) for furfural compounds concentrations in infant formula and milks. Establishing limits related to these compounds would be important for protecting the quality of infant foods. Copyright © 2015 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Ecology and thermal inactivation of microbes in and on interplanetary space vehicle components

NASA Technical Reports Server (NTRS)

Reyes, A. L.

1975-01-01

A series of experiments was conducted to determine the dry heat resistance of microorganisms in soil obtained from Denver Colorado, Pasadena California, Kennedy Space Center Florida, and Cincinnati Ohio. The results of the KSC terminal sterilization cycle experiment are given in graphs. The average number of viable organisms per m1 was calculated for 18 replicate soil samples for each sample area and points plotted equivalent to 30 hr exposure at 112 C. The result showed a reduction of 3 logs from the initial population for both KSC and Cincinnati soil samples. Results from other areas are given in graphs.

300 Area process trench sediment analysis report

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

Zimmerman, M.G.; Kossik, C.D.

1987-12-01

This report describes the results of a sampling program for the sediments underlying the Process Trenches serving the 300 Area on the Hanford reservation. These Process Trenches were the subject of a Closure Plan submitted to the Washington State Department of Ecology and to the US Environmental Protection Agency in lieu of a Part B permit application on November 8, 1985. The closure plan described a proposed sampling plan for the underlying sediments and potential remedial actions to be determined by the sample analyses results. The results and proposed remedial action plan are presented and discussed in this report. 50more » refs., 6 figs., 8 tabs.« less

Accuracy of BRT and Delvotest microbial inhibition tests as affected by composition of ewe's milk.

PubMed

Althaus, Rafael; Torres, Antonio; Peris, Cristofol; Beltran, M Carmen; Fernandez, Nemesio; Molina, M Pilar

2003-03-01

The presence of drug residues in ewe's milk samples can be determined by microbial assays. The main limitation of these tests is the large number of false-positive results associated with them. False-positive results can be explained by the interaction of certain substances naturally existing in ewe's milk with the growth of the microorganism used in the test. In this study, milk chemical composition (fat, protein, lactose, total solids), somatic cell counts (SCCs), free fatty acid concentrations, and lactoperoxidase system components were determined in order to investigate their influence on the rate of false-positive results for the BRT and Delvotest microbiological inhibitor tests. Milk samples were obtained after morning milking of Manchega ewes at 15, 30, 45, 60, 75, 90, 105, 120, and 135 days after parturition. The animals did not receive any kind of treatment or medicated feed throughout the experiment. The false-positive rates for BRT and Delvotest were 3.75 and 2.4%, respectively. When the logistic regression model was applied, the percentages of total solids for positive samples were significantly different from those for negative samples (16.90 versus 18.42% for BRT, 16.05 versus 18.45% for Delvotest), while the SCC logarithmic transformation was significantly higher for the positive samples than for the negative samples (5.38 versus 5.11 log units for BRT, 5.32 versus 5.11 log units for Delvotest). Moreover, Delvotest-positive samples exhibited thiocyanate concentrations higher than those of Delvotest-negative samples (8.18 mg/liter versus 6.85 mg/liter). Further analyses are needed to confirm the possible presence of antimicrobial residues in this particular type of milk sample.

Simultaneous determination of thirteen organophosphate esters in settled indoor house dust and a comparison between two sampling techniques.

PubMed

Fan, Xinghua; Kubwabo, Cariton; Rasmussen, Pat E; Wu, Fang

2014-09-01

An analytical method for the simultaneous determination of 13 organophosphate esters (OPEs) in house dust was developed. The method is based on solvent extraction by sonication, sample cleanup by solid phase extraction (SPE), and analysis by gas chromatography-positive chemical ionization-tandem mass spectrometry (GC/PCI-MS/MS). Method detection limits (MDLs) ranged from 0.03 to 0.43 μg/g and recoveries from 60% to 118%. The inter- and intra-day variations ranged from 3% to 23%. The method was applied to dust samples collected using two vacuum sampling techniques from 134 urban Canadian homes: a sample of fresh or "active" dust (FD) collected by technicians and a composite sample taken from the household vacuum cleaner (HD). Results show that the two sampling methods (i.e., FD vs HD) provided comparable results. Tributoxyethyl phosphate (TBEP), triphenyl phosphate (TPhP), tris(chloropropyl) phosphate (TCPP), tri(2-chloroethyl) phosphate (TCEP), tris(dichloro-isopropyl) phosphate (TDCPP), tricresyl phosphate (TCrP), and tri-n-butyl phosphate (TnBP) were detected in the majority of samples. The most predominant OPE was TBEP, with median concentrations of 31.9 μg/g and 22.8 μg/g in FD and HD samples, respectively, 1 to 2 orders of magnitude higher than other OPEs. The method was also applied to the analysis of OPEs in the National Institute of Standards and Technology (NIST) standard reference material (NIST SRM 2585, organic contaminants in house dust). The results from SRM 2585 may contribute to the certification of OPE concentration values in this SRM. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

Sex determination in skeletal remains from the medieval Eastern Adriatic coast – discriminant function analysis of humeri

PubMed Central

Bašić, Željana; Anterić, Ivana; Vilović, Katarina; Petaros, Anja; Bosnar, Alan; Madžar, Tomislav; Polašek, Ozren; Anđelinović, Šimun

2013-01-01

Aim To investigate the usefulness of humerus measurement for sex determination in a sample of medieval skeletons from the Eastern Adriatic Coast. Additional aim was to compare the results with contemporary female population. Methods Five humerus measurements (maximum length, epicondylar width, maximum vertical diameter of the head, maximum and minimum diameter of the humerus at midshaft) for 80 male and 35 female medieval and 19 female contemporary humeri were recorded. Only sufficiently preserved skeletons and those with no obvious pathological or traumatic changes that could affect the measurements were included. For ten samples, analysis of DNA was performed in order to determine sex using amelogenin. Results The initial comparison of men and women indicated significant differences in all five measures (P < 0.001). Discriminant function for sex determination indicated that as much as 85% of cases could be properly categorized, with better results in men (86%) than women (80%). Furthermore, the comparison of the medieval and contemporary women did not show significant difference in any of the measured features. Sex results obtained by anthropological and DNA analysis matched in all 10 cases. Conclusion The results indicate that humerus measurement in Croatian medieval population may be sufficient to determine the sex of the skeleton. Furthermore, it seems that secular changes have not substantially affected contemporary population, suggesting that the results of this study are transferable to contemporary population as well. PMID:23771758

Spectrophotometric determination of triclosan based on diazotization reaction: response surface optimization using Box-Behnken design.

PubMed

Kaur, Inderpreet; Gaba, Sonal; Kaur, Sukhraj; Kumar, Rajeev; Chawla, Jyoti

2018-05-01

A spectrophotometric method based on diazotization of aniline with triclosan has been developed for the determination of triclosan in water samples. The diazotization process involves two steps: (1) reaction of aniline with sodium nitrite in an acidic medium to form diazonium ion and (2) reaction of diazonium ion with triclosan to form a yellowish-orange azo compound in an alkaline medium. The resulting yellowish-orange product has a maximum absorption at 352 nm which allows the determination of triclosan in aqueous solution in the linear concentration range of 0.1-3.0 μM with R 2 = 0.998. The concentration of hydrochloric acid, sodium nitrite, and aniline was optimized for diazotization reaction to achieve good spectrophotometric determination of triclosan. The optimization of experimental conditions for spectrophotometric determination of triclosan in terms of concentration of sodium nitrite, hydrogen chloride and aniline was also carried out by using Box-Behnken design of response surface methodology and results obtained were in agreement with the experimentally optimized values. The proposed method was then successfully applied for analyses of triclosan content in water samples.

A mass spectrometric line for tritium analysis of water and noble gas measurements from different water amounts in the range of microlitres and millilitres.

PubMed

Papp, Laszlo; Palcsu, Laszlo; Major, Zoltan; Rinyu, Laszlo; Tóth, Istvan

2012-01-01

This paper describes the procedure followed for noble gas measurements for litres, millilitres and microlitres of water samples in our laboratory, including sample preparation, mass spectrometric measurement procedure, and the complete calibrations. The preparation line extracts dissolved gases from water samples of volumes of 0.2 μ l to 3 l and it separates them as noble and other chemically active gases. Our compact system handles the following measurements: (i) determination of tritium concentration of environmental water samples by the (3)He ingrowth method; (ii) noble gas measurements from surface water and groundwater; and (iii) noble gas measurements from fluid inclusions of solid geological archives (e.g. speleothems). As a result, the tritium measurements have a detection limit of 0.012 TU, and the expectation value (between 1 and 20 TU) is within 0.2 % of the real concentrations with a standard deviation of 2.4 %. The reproducibility of noble gas measurements for water samples of 20-40 ml allows us to determine solubility temperatures by an uncertainty better than 0.5 °C. Moreover, noble gas measurements for tiny water amounts (in the microlitre range) show that the results of the performed calibration measurements for most noble gas isotopes occur with a deviation of less than 2 %. Theoretically, these precisions for noble gas concentrations obtained from measurements of waters samples of a few microlitres allow us to determine noble gas temperatures by an uncertainty of less than 1 °C. Here, we present the first noble gas measurements of tiny amounts of artificial water samples prepared under laboratory conditions.

Multiresidue method for the determination of 227 pesticides in hot pepper (Capsicum annuum L.) by liquid chromatography with tandem mass spectrometry.

PubMed

Zhu, Yong-Zhe; Zhao, Mei-Ai; Nan Feng, Ya; Han Kim, Jeong

2014-10-01

A high-throughput, rapid, and efficient modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method with a simple cleanup procedure has been developed for simultaneously determining 227 pesticides in pepper samples by liquid chromatography with tandem mass spectrometry (running time: 10 min). Pesticide residues were extracted/partitioned with an acetonitrile/DisQuE QuEChERS pouch, and the resulting samples were cleaned up with different methods: dispersive solid-phase extraction with primary secondary amines or multiwalled carbon nanotubes and graphitized carbon solid mini cartridge column. The results indicated that multiwalled carbon nanotubes dispersive sorbents achieved the best recoveries and had less matrix interference. The numbers of pesticides with a recovery in the range of 70-120% were 199 at a spiked level of 40 μg/kg. The correlation coefficients (r(2)) for 227 pesticides were above 0.99, while the limits of quantitation of pesticides in pepper samples ranged from 0.13 to 13.51 μg/kg (S/N = 10), and the limits of detection ranged from 0.04 to 4.05 μg/kg (S/N = 3). The relative standard deviations of approximately 197 pesticides were below 20% at spiked levels of 40 μg/kg. Based on these results, the proposed method was chosen as the most suitable cleanup procedure for the determination of multiresidue pesticides in pepper samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Statistical sex determination from craniometrics: Comparison of linear discriminant analysis, logistic regression, and support vector machines.

PubMed

Santos, Frédéric; Guyomarc'h, Pierre; Bruzek, Jaroslav

2014-12-01

Accuracy of identification tools in forensic anthropology primarily rely upon the variations inherent in the data upon which they are built. Sex determination methods based on craniometrics are widely used and known to be specific to several factors (e.g. sample distribution, population, age, secular trends, measurement technique, etc.). The goal of this study is to discuss the potential variations linked to the statistical treatment of the data. Traditional craniometrics of four samples extracted from documented osteological collections (from Portugal, France, the U.S.A., and Thailand) were used to test three different classification methods: linear discriminant analysis (LDA), logistic regression (LR), and support vector machines (SVM). The Portuguese sample was set as a training model on which the other samples were applied in order to assess the validity and reliability of the different models. The tests were performed using different parameters: some included the selection of the best predictors; some included a strict decision threshold (sex assessed only if the related posterior probability was high, including the notion of indeterminate result); and some used an unbalanced sex-ratio. Results indicated that LR tends to perform slightly better than the other techniques and offers a better selection of predictors. Also, the use of a decision threshold (i.e. p>0.95) is essential to ensure an acceptable reliability of sex determination methods based on craniometrics. Although the Portuguese, French, and American samples share a similar sexual dimorphism, application of Western models on the Thai sample (that displayed a lower degree of dimorphism) was unsuccessful. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

An overview of the ecological half-life of the 137Cs radioisotope and a determination of radioactivity levels in sediment samples after Chernobyl in the Eastern Black Sea, Turkey

NASA Astrophysics Data System (ADS)

Baltas, Hasan; Sirin, Murat; Dalgic, Goktug; Cevik, Ugur

2018-01-01

A study which determined the activity concentration of 137Cs in sediments contaminated by effluents from the Chernobyl accident which had collected along the coast of the Eastern Black Sea region in Turkey was carried out in 1993. Marine sediment samples were collected in 2015 from the same fifteen sampling points, and the activity concentrations of 226Ra, 232Th, 40K and 137Cs were determined for the sediment samples. The activity concentrations ranged from 10.94-25.95, 12.14-33.05, 265.74-459.89 and 2.08-37.45 Bq kg- 1 for 226Ra, 232Th, 40K and 137Cs respectively. The results showed that there was a steep decline in 137Cs within the sediment at most of the sampling sites from the Eastern Black Sea region during the 22-year period, except for two sites at which the measured levels were much higher. This may be the result of the combined effects of radioactive contaminant entry into this area from rivers, environmental changes and nuclear testing between 1993 and 2015. Furthermore, the ecological half-life (EHL) of the 137Cs radionuclide was estimated for the sediment samples, and radiological hazard parameters such as the absorbed dose rate in air (D), the annual effective dose equivalent (AEDE) and the excess lifetime cancer risk (ELCR) were calculated and compared with the international recommended values. It was shown that these sediments do not present any significant health risk for humans in this area.

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

Scheele, R.D.

In 1995, available subsegment samples of wastes taken from the Hanford Site underground radioactive waste storage tanks 241-C-112 (C-112) and 241-C-109 (C-109) were reanalyzed to determine the nickel concentrations in the samples and to determine whether the use of a nickel crucible in the analytical sample preparation biased the reported nickel concentrations reported by Simpson and coworkers and in the original report that this report supplements. The reanalysis strategy to determine nickel was to use a sodium peroxide flux in a zirconium crucible instead of the previously used potassium hydroxide flux in a nickel crucible. This supplemental report provides themore » results of the reanalyses and updates tables from the original report which reflect the new nickel analyses. Nickel is important with respect to management of the potentially reactive ferrocyanide wastes as it is one of the key defining characteristics of the solids that resulted from scavenging radiocesium using ferrocyanides. In Hanford Site wastes, few other processes introduced nickel into the wastes other than radiocobalt scavenging, which was often coupled with the ferrocyanide-scavenging process. Thus the presence of nickel in a waste provides strong evidence that the original waste was or contained ferrocyanide waste at one time. Given the potential import of nickel as a defining characteristic and marker for ferrocyanide wastes, the Pacific Northwest Laboratory`s (PNL) Analytical Chemistry Laboratory (ACL) reanalyzed available samples from tanks C-112 and C-109 using inductively coupled argon plasma/atomic emission spectrometry (ICP/AES) and an alternative sample preparation method which precluded contamination of the analytical samples with nickel.« less

Miniaturized sample preparation needle: a versatile design for the rapid analysis of smoking-related compounds in hair and air samples.

PubMed

Saito, Yoshihiro; Ueta, Ikuo; Ogawa, Mitsuhiro; Hayashida, Makiko; Jinno, Kiyokatsu

2007-05-09

Miniaturized needle extraction device has been developed as a versatile sample preparation device designed for the rapid and simple analysis of smoking-related compounds in smokers' hair samples and environmental tobacco smoke. Packed with polymeric particle, the resulting particle-packed needle was employed as a miniaturized sample preparation device for the analysis of typical volatile organic compounds in tobacco smoke. Introducing a bundle of polymer-coated filaments as the extraction medium, the needle was further applied as a novel sample preparation device containing simultaneous derivatization/extraction process of volatile aldehydes. Formaldehyde (FA) and acetaldehyde (AA) in smoker's breath during the smoking were successfully derivatized with two derivatization reagents in the polymer-coated fiber-packed needle device followed by the separation and determination in gas chromatography (GC). Smokers' hair samples were also packed into the needle, allowing the direct extraction of nicotine from the hair sample in a conventional GC injector. Optimizing the main experimental parameters for each technique, successful determination of several smoking-related compounds with these needle extraction methods has been demonstrated.

The Statistics and Mathematics of High Dimension Low Sample Size Asymptotics.

PubMed

Shen, Dan; Shen, Haipeng; Zhu, Hongtu; Marron, J S

2016-10-01

The aim of this paper is to establish several deep theoretical properties of principal component analysis for multiple-component spike covariance models. Our new results reveal an asymptotic conical structure in critical sample eigendirections under the spike models with distinguishable (or indistinguishable) eigenvalues, when the sample size and/or the number of variables (or dimension) tend to infinity. The consistency of the sample eigenvectors relative to their population counterparts is determined by the ratio between the dimension and the product of the sample size with the spike size. When this ratio converges to a nonzero constant, the sample eigenvector converges to a cone, with a certain angle to its corresponding population eigenvector. In the High Dimension, Low Sample Size case, the angle between the sample eigenvector and its population counterpart converges to a limiting distribution. Several generalizations of the multi-spike covariance models are also explored, and additional theoretical results are presented.

Method development for the determination of fluorine in water samples via the molecular absorption of strontium monofluoride formed in an electrothermal atomizer

NASA Astrophysics Data System (ADS)

Ozbek, Nil; Akman, Suleyman

The presence of fluorine (F) was detected via the rotational molecular absorption line of diatomic strontium-monofluoride (SrF) generated in the gas phase at 651.187 nm using high-resolution continuum source electrothermal atomic absorption spectrometry. Upon the addition of excess strontium (Sr) as the nitrate, the fluorine in the sample was converted to SrF in the gas phase of a graphite furnace. The effects on the accuracy, precision and sensitivity of variables such as the SrF wavelength, graphite furnace program, amount of Sr, coating of the graphite tube and platform with Zr and Ir and the use of a modifier were investigated and optimized. It was determined that there was no need to use a modifier or to cover the platform/tubes with Zr or Ir. Fluorine concentrations in various water samples (certified waste water, tap water, drinking water and mineral water) were determined using 20 μg of Sr as the molecule-forming reagent and applying a maximum pyrolysis temperature of 800 °C and a molecule-forming temperature of 2200 °C with a heating rate of 2000 °C s- 1. Good linearity was maintained up to 0.1 μg of F. The accuracy and precision of the method were tested by analyzing certified reference wastewater. The results were in good agreement with certified values, and the precision was satisfactory (RSD < 10%). The limit of detection and the characteristic mass for the method were 0.36 ng and 0.55 ng, respectively. Finally, the fluorine concentrations in several drinking water and mineral water samples taken from the market were determined. The results were in good agreement with the values supplied by the producers. No significant differences were found between the results from the linear calibration and standard addition techniques. The method was determined to be simple, fast, accurate and sensitive.

[Investigation on simultaneous determination of dihydroxybenzene isomers in water samples using multi-walled carbon nanotube modified screen-printed electrode].

PubMed

Li, Yuan-Ting; Li, Da-Wei; Song, Wei; Long, Yi-Tao

2011-02-01

A disposable electrode, multi-walled carbon nanotube modified screen printed electrode (MWCNT/SPE), had been fabricated using screen printing technology and drop-coating method to determine dihydroxybenzene isomers (hydroquinone, catechol and resorcinol). The cyclic voltammetry behavior of dihydroxybenzene isomers had been investigated with the MWCNT/SPE. The results reveal that MWCNT/SPE, which shows a strong electrocatalytic activity for the oxidation of dihydroxybenzenes, can entirely separate the oxidation peaks of them. According to differential pulse voltammetry tests, the peak currents of dihydroxybenzene isomers are linear to their concentrations at the range of 8.20 x 10(-6) -1.00 x 10(-3), 8.20 x 10(-6) -1.00 x 10(-3) and 1.64 x 10(-5) -1.16 x 10(-3) mol x L(-1), with the detection limits of 4.34 x 10(-6), 3.42 x 10(-6) and 6.70 x 10(-6) mol x L(-1) for hydroquinone, catechol and resorcinol, respectively. For the determination of dihydroxybenzene isomers in water samples, the value of recovery found by standard addition method was in the range of 96.2%-104.9%. These results indicate MWCNT/SPE can be applied to rapid in-situ determination of dihydroxybenzenes-polluted water samples.

Determination of iodine and molybdenum in milk by quadrupole ICP-MS.

PubMed

Reid, Helen J; Bashammakh, Abdul A; Goodall, Phillip S; Landon, Mark R; O'Connor, Ciaran; Sharp, Barry L

2008-03-15

A reliable method for the determination of iodine and molybdenum in milk samples, using alkaline digestion with tetramethylammonium hydroxide and hydrogen peroxide, followed by quadrupole ICP-MS analysis, has been developed and tested using certified reference materials. The use of He+O2 (1.0 ml min(-1) and 0.6 ml min(-1)) in the collision-reaction cell of the mass spectrometer to remove (129)Xe+-- initially to enable the determination of low levels of 129I--also resulted in the quantitative conversion of Mo(+) to MoO2+ which enabled the molybdenum in the milk to be determined at similar mass to the iodine with the use of Sb as a common internal standard. In order to separate and pre-concentrate iodine at sub microg l(-1) concentrations, a novel method was developed using a cation-exchange column loaded with Pd2+ and Ca2+ ions to selectively retain iodide followed by elution with a small volume of ammonium thiosulfate. This method showed excellent results for aqueous iodide solutions, although the complex milk digest matrix made the method unsuitable for such samples. An investigation of the iodine species formed during oxidation and extraction of milk sample digests was carried out with a view to controlling the iodine chemistry.

Simultaneous LC-MS/MS determination of phenylbutyrate, phenylacetate benzoate and their corresponding metabolites phenylacetylglutamine and hippurate in blood and urine.

PubMed

Laryea, Maurice D; Herebian, Diran; Meissner, Thomas; Mayatepek, Ertan

2010-12-01

Inborn errors of urea metabolism result in hyperammonemia. Treatment of urea cycle disorders can effectively lower plasma ammonium levels and results in survival in the majority of patients. Available medications for treating urea cycle disorders include sodium benzoate (BA), sodium phenylacetate (PAA), and sodium phenylbutyrate (PBA) and are given to provide alternate routes for disposition of waste nitrogen excretion. In this study, we develop and validate a liquid chromatography tandem mass spectrometry (LC-MS/MS) method for simultaneous determination of benzoic acid, phenylacetic acid, phenylbutyric acid, phenylacetylglutamine, and hippuric acid in plasma and urine from children with inborn errors of urea synthesis. Plasma extracts and diluted urine samples were injected on a reverse-phase column and identified and quantified by selected reaction monitoring (SRM) in negative ion mode. Deuterated analogues served as internal standards. Analysis time was 7 min. Assay precision, accuracy, and linearity and sample stability were determined using enriched samples. Quantification limits of the method were 100 ng/ml (0.3-0.8 μmol/L) for all analytes, and recoveries were >90%. Inter- and intraday relative standard deviations were <10%. Our newly developed LC-MS/MS represents a robust, sensitive, and rapid method that allows simultaneous determination of the five compounds in plasma and urine.

Comparison of Adsorbed Mercury Screening Method With Cold-Vapor Atomic Absorption Spectrophotometry for Determination of Mercury in Soil

NASA Technical Reports Server (NTRS)

Easterling, Donald F.; Hovanitz, Edward S.; Street, Kenneth W.

2000-01-01

A field screening method for the determination of elemental mercury in environmental soil samples involves the thermal desorption of the mercury from the sample onto gold and then the thermal desorption from the gold to a gold-film mercury vapor analyzer. This field screening method contains a large number of conditions that could be optimized for the various types of soils encountered. In this study, the conditions were optimized for the determination of mercury in silty clay materials, and the results were comparable to the cold-vapor atomic absorption spectrophotometric method of determination. This paper discusses the benefits and disadvantages of employing the field screening method and provides the sequence of conditions that must be optimized to employ this method of determination on other soil types.

Determining Optimal Waste Volume From an Intravenous Catheter

PubMed Central

Baker, Rachel B.; Summer, Suzanne S.; Lawrence, Michelle; Shova, Amy; McGraw, Catherine A.; Khoury, Jane

2013-01-01

Waste is blood drawn from an intravenous (IV) catheter to remove saline before obtaining a blood sample. This study examines the minimum waste volume resulting in an undiluted sample. A repeated measures design was used. Investigators placed an IV catheter in 60 healthy adults and obtained samples at baseline and following waste volume ranging from 0.5 mL to 3 mL. A random effects mixed model was used to determine the stabilizing point. For sodium and glucose measurements, this stabilizing point was 1 mL of waste. Knowing that only 1 mL of waste is needed will prevent clinicians from obtaining extra waste and discarding blood needlessly. PMID:23455970

Resonance Ionization Mass Spectrometry System for Measurement of Environmental Samples

NASA Astrophysics Data System (ADS)

Pibida, L.; McMahon, C. A.; Nörtershäuser, W.; Bushaw, B. A.

2002-10-01

A resonance ionization mass spectrometry (RIMS) system has been developed at the National Institute of Standards and Technology (NIST) for sensitive and selective determination of radio-cesium in the environment. The overall efficiency was determined to be 4×10-7 with a combined (laser and mass spectrometer) selectivity of 108 for both 135Cs and 137Cs with respect to 133Cs. RIMS isotopic ratio measurements of 135Cs/ 137Cs were performed on a nuclear fuel burn-up sample and compared to measurements on a similar system at Pacific Northwest National Laboratory (PNNL) and to conventional thermal ionization mass spectrometry (TIMS). Results of preliminary RIMS investigations on a freshwater lake sediment sample are also discussed.

Analytical procedures for the determination of selected trace elements in peat and plant samples by inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Krachler, Michael; Mohl, Carola; Emons, Hendrik; Shotyk, William

2002-08-01

A simple, robust and reliable analytical procedure for the determination of 15 elements, namely Ca, V, Cr, Mn, Co, Ni, Cu, Zn, Rb, Ag, Cd, Ba, Tl, Th and U in peat and plant materials by inductively coupled plasma-quadrupole mass spectrometry (ICP-QMS) was developed. Powdered sample aliquots of approximately 220 mg were dissolved with various acid mixtures in a microwave heated high-pressure autoclave capable to digest 40 samples simultaneously. The selection of appropriate amounts of digestion acids (nitric acid, hydrofluoric acid or tetrafluoroboric acid) was crucial to obtain accurate results. The optimized acid mixture for digestion of plant and peat samples consisted of 3 ml HNO 3 and 0.1 ml HBF 4. An ultrasonic nebulizer with an additional membrane desolvation unit was found beneficial for the determination of Co, Ni, Ag, Tl, Th and U, allowing to aspirate a dry sample aerosol into the ICP-QMS. A pneumatic cross flow nebulizer served as sample introduction device for the other elements. Internal standardization was achieved with 103Rh for all elements, except for Th whose ICP-QMS signals were corrected by 103Rh and 185Re. Quality control was ascertained by analysis of the certified plant reference material GBW 07602 Bush Branches and Leaves. In almost all cases HNO 3 alone could not fully liberate the analytes of interest from the peat or plant matrix, probably because of the silicates present. After adding small amounts (0.05-0.1 ml) of either HF or HBF 4 to the digestion mixture, concentrations quantified by ICP-QMS generally increased significantly, in the case of Rb up to 80%. Further increasing the volumes of HF or HBF 4 in turn, resulted in a loss of recoveries of almost all elements, some of which amounted to approximately 60%. The successful analytical procedures were applied to the determination of two bulk peat materials. In general, good agreement between the found concentrations and results from an inter-laboratory trial or from instrumental neutron activation data were obtained, underpinning the suitability of the developed analytical approach.

Temperature dependence on the pesticide sampling rate of polar organic chemical integrative samplers (POCIS).

PubMed

Yabuki, Yoshinori; Nagai, Takashi; Inao, Keiya; Ono, Junko; Aiko, Nobuyuki; Ohtsuka, Nobutoshi; Tanaka, Hitoshi; Tanimori, Shinji

2016-10-01

Laboratory experiments were performed to determine the sampling rates of pesticides for the polar organic chemical integrative samplers (POCIS) used in Japan. The concentrations of pesticides in aquatic environments were estimated from the accumulated amounts of pesticide on POCIS, and the effect of water temperature on the pesticide sampling rates was evaluated. The sampling rates of 48 pesticides at 18, 24, and 30 °C were obtained, and this study confirmed that increasing trend of sampling rates was resulted with increasing water temperature for many pesticides.

Direct metal laser deposition of titanium powder Ti-6Al-4V

NASA Astrophysics Data System (ADS)

Bykovskiy, D. P.; Petrovskiy, V. N.; Sergeev, K. L.; Osintsev, A. V.; Dzhumaev, P. S.; Polskiy, V. I.

2017-12-01

The paper presents the results of mechanical properties study of the material produced by direct metal laser deposition of VT6 titanium powder. The properties were determined by the results of stretching at tensile testing machine, as well as compared with the properties of the same rolled material. These results show that obtained samples have properties on the level or even higher than that ones of the samples obtained from the rolled material in a certain range of technological regimes.

Determination of very low levels of 5-(hydroxymethyl)-2-furaldehyde (HMF) in natural honey: comparison between the HPLC technique and the spectrophotometric white method.

PubMed

Truzzi, Cristina; Annibaldi, Anna; Illuminati, Silvia; Finale, Carolina; Rossetti, Monica; Scarponi, Giuseppe

2012-07-01

In this work we compared 2 official methods for the determination of HMF in honey, the spectrophotometric White method and the HPLC method (International Honey Commission) for the determination of HMF in unifloral honey and honeydew samples with a very low HMF content (<4 mg/kg), which is the most critical determination in terms of accuracy and precision of methods. In honey solutions, the limits of quantification for HPLC and White methods are 0.83 mg/L and 0.67 mg/L, respectively, and the linearity range is confirmed up to 20 mg/L for the HPLC method and up to 5 mg/L for the White method. In honeys with HMF >5 mg/kg, the molar extinction coefficient is 15369, lower than the literature value of 16830, and should be used for HMF determination. For samples with HMF content in the range 1-4 mg/kg the accuracy of the 2 methods is comparable both for unifloral and honeydew samples, whereas as regards precision, the HPLC method gives better results (3.5% compared with 6.4% for the White method). So, in general, the HPLC method seems to be more appropriate for the determination of HMF in honey in the range 1-4 mg/kg thanks to its greater precision, but for samples with a HMF content of less than 1 mg/kg the analyses are inaccurate for both methods. This work can help governmental and private laboratories that perform food analyses to choose the best method for the determination of HMF at very low levels in unifloral honey and honeydew samples. © 2012 Institute of Food Technologists®

Prevalence and causes of abnormal PSA recovery.

PubMed

Lautenbach, Noémie; Müntener, Michael; Zanoni, Paolo; Saleh, Lanja; Saba, Karim; Umbehr, Martin; Velagapudi, Srividya; Hof, Danielle; Sulser, Tullio; Wild, Peter J; von Eckardstein, Arnold; Poyet, Cédric

2018-01-26

Prostate-specific antigen (PSA) test is of paramount importance as a diagnostic tool for the detection and monitoring of patients with prostate cancer. In the presence of interfering factors such as heterophilic antibodies or anti-PSA antibodies the PSA test can yield significantly falsified results. The prevalence of these factors is unknown. We determined the recovery of PSA concentrations diluting patient samples with a standard serum of known PSA concentration. Based on the frequency distribution of recoveries in a pre-study on 268 samples, samples with recoveries <80% or >120% were defined as suspect, re-tested and further characterized to identify the cause of interference. A total of 1158 consecutive serum samples were analyzed. Four samples (0.3%) showed reproducibly disturbed recoveries of 10%, 68%, 166% and 4441%. In three samples heterophilic antibodies were identified as the probable cause, in the fourth anti-PSA-autoantibodies. The very low recovery caused by the latter interference was confirmed in serum, as well as heparin- and EDTA plasma of blood samples obtained 6 months later. Analysis by eight different immunoassays showed recoveries ranging between <10% and 80%. In a follow-up study of 212 random plasma samples we found seven samples with autoantibodies against PSA which however did not show any disturbed PSA recovery. About 0.3% of PSA determinations by the electrochemiluminescence assay (ECLIA) of Roche diagnostics are disturbed by heterophilic or anti-PSA autoantibodies. Although they are rare, these interferences can cause relevant misinterpretations of a PSA test result.

Development and validation of a highly sensitive gas chromatographic-mass spectrometric screening method for the simultaneous determination of nanogram levels of fentanyl, sufentanil and alfentanil in air and surface contamination wipes.

PubMed

Van Nimmen, Nadine F J; Veulemans, Hendrik A F

2004-05-07

A highly sensitive gas chromatographic-mass spectrometric (GC-MS) analytical method for the determination of the opioid narcotics fentanyl, alfentanil, and sufentanil in industrial hygiene personal air samples and surface contamination wipes was developed and comprehensively validated. Sample preparation involved a single step extraction of the samples with methanol, fortified with a fixed amount of the penta-deuterated analogues of the opioid narcotics as internal standard. The GC-MS analytical procedure using selected ion monitoring (SIM) was shown to be highly selective. Linearity was shown for levels of extracted wipe and air samples corresponding to at least 0.1-2 times their surface contamination limit (SCL) and accordingly to 0.1-2 times their time weighted average occupational exposure limit (OEL-TWA) based on a full shift 9601 air sample. Extraction recoveries were determined for spiked air samples and surface wipes and were found to be quantitative for both sampling media in the entire range studied. The air sampling method's limit of detection (LOD) was determined to be 0.4 ng per sample for fentanyl and sufentanil and 1.6 ng per sample for alfentanil, corresponding to less than 1% of their individual OEL for a full shift air sample (9601). The limit of quantification (LOQ) was found to be 1.4, 1.2, and 5.0 ng per filter for fentanyl, sufentanil, and alfentanil, respectively. The wipe sampling method had LODs of 4 ng per wipe for fentanyl and sufentanil and 16 ng per wipe for alfentanil and LOQs of respectively, 14, 12, and 50 ng per wipe. The analytical intra-assay precision of the air sampling and wipe sampling method, defined as the coefficient of variation on the analytical result of six replicate spiked media was below 10 and 5%, respectively, for all opioids at all spike levels. Accuracy expressed as relative error was determined to be below 10%, except for alfentanil at the lowest spike level (-13.1%). The stability of the opioids during simulated air sampling was investigated. For fentanyl and sufentanil a quantitative recovery was observed at all spike levels, while for alfentanil recoveries ranged from 60.3 to 85.4%. When spiked air samples were stored at ambient temperature and at -15 degrees C quantitative recovery was found for fentanyl and sufentanil after 7 and 14 days. For alfentanil a slight loss seemed to occur upon storage during 7 days, being more explicit after 14 days. Ambient storage of spiked wipes seemed to lead to significant losses of all opioids studied, yielding recoveries of 37.7-88.3%. Upon storage of similar wipes at -15 degrees C a significantly higher recovery was found ranging from 77.3 to 88.3%. The developed analytical and sampling procedures have been recently applied in an explorative field study of which the results of surface contamination wipe sampling are presented in this paper. To our knowledge, this is the first study addressing the development and validation of analytical procedures for the assessment of external occupational exposure to potent opioid narcotics.

Motivation to Quit Smoking after Acute Coronary Syndrome.

PubMed

Rocha, Vânia; Guerra, Marina; Lemos, Marina; Maciel, Júlia; Williams, Geoffrey

2017-01-31

Self-Determination Theory explores the process through which a person acquires motivation to initiate new behaviours related to health and to maintain them over time. This study aimed to determine the overall fit of Self-Determination Theory Model for Health Behavior to the data obtained from a sample of smokers hospitalized with acute coronary syndrome, and to identify the predictors of smoking status six months after clinical discharge. The sample included 110 participants, regular smokers, hospitalized due to acute coronary syndrome. Questionnaires were administered to assess autonomous self-regulation, perceived competence, family support, depressive symptoms and meaning in life. Participants were asked if they were currently smokers six months after clinical discharge. The results showed that the process variables specified by Self-Determination Theory fit the data well. Perceived competence predicted abstinence from smoking six months after clinical discharge. Our findings have similar characteristics to other international samples in which Self-Determination Theory models havebeen tested. It is important to facilitate perceived competence, as the patients who continue to smoke have shorter length of life. This study highlights the importance of considering clinical interventions based on Self-Determination Theory to facilitatesmoking cessation.

Evaluation of the furosine and homoarginine methods for determining reactive lysine in rumen-undegraded protein.

PubMed

Boucher, S E; Pedersen, C; Stein, H H; Schwab, C G

2009-08-01

Three samples of soybean meal (SBM), 3 samples of expeller SBM (SoyPlus, West Central Cooperative, Ralston, IA), 5 samples of distillers dried grains with solubles (DDGS), and 5 samples of fish meal were used to evaluate the furosine and homoarginine procedures to estimate reactive Lys in the rumen-undegraded protein fraction (RUP-Lys). One sample each of SBM, expeller SBM, and DDGS were subjected to additional heat treatment in the lab to ensure there was a wide range in reactive RUP-Lys content among the samples. Furosine is a secondary product of the initial stages of the Maillard reaction and can be used to calculate blocked Lys. Homoarginine is formed via the reaction of reactive Lys with O-methylisourea and can be used to calculate the concentration of reactive Lys. In previous experiments, each sample was ruminally incubated in situ for 16 h, and standardized RUP-Lys digestibility of the samples was determined in cecectomized roosters. All rumen-undegraded residue (RUR) samples were analyzed for furosine and Lys; however, only 9 of the 16 samples contained furosine, and only the 4 unheated DDGS samples contained appreciable amounts of furosine. Blocked RUP-Lys was calculated from the furosine and Lys concentrations of the RUR. Both the intact feed and RUR samples were evaluated using the homoarginine method. All samples were incubated with an O-methylisourea/BaOH solution for 72 h and analyzed for Lys and homoarginine concentrations. Reactive Lys concentrations of the intact feeds and RUR were calculated. Results of the experiment indicate that blocked RUP-Lys determined via the furosine method was negatively correlated with standardized RUP-Lys digestibility, and reactive RUP-Lys determined via the guanidination method was positively correlated with standardized RUP-Lys digestibility. Reactive Lys concentrations of the intact samples were also highly correlated with RUP-Lys digestibility. In conclusion, the furosine assay is useful in predicting RUP-Lys digestibility of DDGS samples, and the guanidination procedure can be used to predict RUP-Lys digestibility of SBM, expeller SBM, DDGS, and fish meal samples.

Naturally acquired bovine besnoitiosis: Differential distribution of parasites in the skin of chronically infected cattle.

PubMed

Schares, G; Langenmayer, M C; Majzoub-Altweck, M; Scharr, J C; Gentile, A; Maksimov, A; Schares, S; Conraths, F J; Gollnick, N S

2016-01-30

Bovine besnoitiosis is caused by Besnoitia besnoiti, an apicomplexan parasite closely related to Toxoplasma gondii and Neospora caninum. In the acute stage of besnoitiosis, cattle suffer from pyrexia, swollen lymph nodes, anorexia and subcutaneous edema. In the chronic stage, tissue cysts are formed in a variety of tissues including the skin. Knowledge about the distribution of tissue cysts of different parts of the skin of infected animals is scarce. Four chronically infected cattle were euthanized and skin samples were taken from a total of 77 standardized cutaneous locations per animal. Portions of the dermis were taken, from which DNA was extracted and examined by real-time PCR. Cycle of transition (Ct) values reflecting the amount of parasite DNA in the samples were determined. For statistical analysis, samples were attributed to 11 larger skin regions ('OuterHindlegDistal', 'Rump, ForelegMiddle', 'NoseFrontEars', 'CheekEye', 'SideLowerPart', 'ForelegDistal', 'SideUpperPart', 'LegsInner', 'VentralHeadNeck', 'DorsalNeckWithersBackTail'). While all samples revealed a positive result in three female cattle, only 63.6% (49/77) of the samples of a bull showed positive results. For statistical analysis, a Ct value of 45 was assumed for samples with a negative result. The dams showed median Ct values of 16.1, 17.5 and 19.4, while in skin samples of the bull a median Ct value of 37.6 was observed. To determine the differences in DNA concentrations between different locations of the skin of the animals, a relative Ct (relCt) was determined by subtracting for each animal indv the MedianCtindv from each sample Ct. Analyses of the relCt values showed that the highest relative parasite DNA concentrations were observed in the categories 'OuterHindlegDistal', 'Rump', 'ForelegMiddle' and 'NoseFrontEars'. The relCt values in these categories differed statistically significantly from those determined for the categories 'VentralHeadNeck' and 'DorsalNeckWithersBackTail'. The analysis showed clear differences in the distribution and the detectability of parasite DNA in the skin of cattle infected with B. besnoiti. In all four animals, samples from the 'Rump' region (Regio fermoris) showed high parasite DNA concentrations. Because this region is also easily accessible for veterinarians, this skin location appears to be optimal for taking skin biopsies for detection or isolation of B. besnoiti. Copyright © 2015 Elsevier B.V. All rights reserved.

Extraction efficiency and implications for absolute quantitation of propranolol in mouse brain, liver and kidney thin tissue sections using droplet-based liquid microjunction surface sampling-HPLC ESI-MS/MS

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

Kertesz, Vilmos; Weiskittel, Taylor M.; Vavek, Marissa

Currently, absolute quantitation aspects of droplet-based surface sampling for thin tissue analysis using a fully automated autosampler/HPLC-ESI-MS/MS system are not fully evaluated. Knowledge of extraction efficiency and its reproducibility is required to judge the potential of the method for absolute quantitation of analytes from thin tissue sections. Methods: Adjacent thin tissue sections of propranolol dosed mouse brain (10- μm-thick), kidney (10- μm-thick) and liver (8-, 10-, 16- and 24- μm-thick) were obtained. Absolute concentration of propranolol was determined in tissue punches from serial sections using standard bulk tissue extraction protocols and subsequent HPLC separations and tandem mass spectrometric analysis. Thesemore » values were used to determine propranolol extraction efficiency from the tissues with the droplet-based surface sampling approach. Results: Extraction efficiency of propranolol using 10- μm-thick brain, kidney and liver thin tissues using droplet-based surface sampling varied between ~45-63%. Extraction efficiency decreased from ~65% to ~36% with liver thickness increasing from 8 μm to 24 μm. Randomly selecting half of the samples as standards, precision and accuracy of propranolol concentrations obtained for the other half of samples as quality control metrics were determined. Resulting precision ( ±15%) and accuracy ( ±3%) values, respectively, were within acceptable limits. In conclusion, comparative quantitation of adjacent mouse thin tissue sections of different organs and of various thicknesses by droplet-based surface sampling and by bulk extraction of tissue punches showed that extraction efficiency was incomplete using the former method, and that it depended on the organ and tissue thickness. However, once extraction efficiency was determined and applied, the droplet-based approach provided the required quantitation accuracy and precision for assay validations. Furthermore, this means that once the extraction efficiency was calibrated for a given tissue type and drug, the droplet-based approach provides a non-labor intensive and high-throughput means to acquire spatially resolved quantitative analysis of multiple samples of the same type.« less

Extraction efficiency and implications for absolute quantitation of propranolol in mouse brain, liver and kidney thin tissue sections using droplet-based liquid microjunction surface sampling-HPLC ESI-MS/MS

DOE PAGES

Kertesz, Vilmos; Weiskittel, Taylor M.; Vavek, Marissa; ...

2016-06-22

Currently, absolute quantitation aspects of droplet-based surface sampling for thin tissue analysis using a fully automated autosampler/HPLC-ESI-MS/MS system are not fully evaluated. Knowledge of extraction efficiency and its reproducibility is required to judge the potential of the method for absolute quantitation of analytes from thin tissue sections. Methods: Adjacent thin tissue sections of propranolol dosed mouse brain (10- μm-thick), kidney (10- μm-thick) and liver (8-, 10-, 16- and 24- μm-thick) were obtained. Absolute concentration of propranolol was determined in tissue punches from serial sections using standard bulk tissue extraction protocols and subsequent HPLC separations and tandem mass spectrometric analysis. Thesemore » values were used to determine propranolol extraction efficiency from the tissues with the droplet-based surface sampling approach. Results: Extraction efficiency of propranolol using 10- μm-thick brain, kidney and liver thin tissues using droplet-based surface sampling varied between ~45-63%. Extraction efficiency decreased from ~65% to ~36% with liver thickness increasing from 8 μm to 24 μm. Randomly selecting half of the samples as standards, precision and accuracy of propranolol concentrations obtained for the other half of samples as quality control metrics were determined. Resulting precision ( ±15%) and accuracy ( ±3%) values, respectively, were within acceptable limits. In conclusion, comparative quantitation of adjacent mouse thin tissue sections of different organs and of various thicknesses by droplet-based surface sampling and by bulk extraction of tissue punches showed that extraction efficiency was incomplete using the former method, and that it depended on the organ and tissue thickness. However, once extraction efficiency was determined and applied, the droplet-based approach provided the required quantitation accuracy and precision for assay validations. Furthermore, this means that once the extraction efficiency was calibrated for a given tissue type and drug, the droplet-based approach provides a non-labor intensive and high-throughput means to acquire spatially resolved quantitative analysis of multiple samples of the same type.« less

Potential for false positive HIV test results with the serial rapid HIV testing algorithm.

PubMed

Baveewo, Steven; Kamya, Moses R; Mayanja-Kizza, Harriet; Fatch, Robin; Bangsberg, David R; Coates, Thomas; Hahn, Judith A; Wanyenze, Rhoda K

2012-03-19

Rapid HIV tests provide same-day results and are widely used in HIV testing programs in areas with limited personnel and laboratory infrastructure. The Uganda Ministry of Health currently recommends the serial rapid testing algorithm with Determine, STAT-PAK, and Uni-Gold for diagnosis of HIV infection. Using this algorithm, individuals who test positive on Determine, negative to STAT-PAK and positive to Uni-Gold are reported as HIV positive. We conducted further testing on this subgroup of samples using qualitative DNA PCR to assess the potential for false positive tests in this situation. Of the 3388 individuals who were tested, 984 were HIV positive on two consecutive tests, and 29 were considered positive by a tiebreaker (positive on Determine, negative on STAT-PAK, and positive on Uni-Gold). However, when the 29 samples were further tested using qualitative DNA PCR, 14 (48.2%) were HIV negative. Although this study was not primarily designed to assess the validity of rapid HIV tests and thus only a subset of the samples were retested, the findings show a potential for false positive HIV results in the subset of individuals who test positive when a tiebreaker test is used in serial testing. These findings highlight a need for confirmatory testing for this category of individuals.

Non-invasive determination of glucose directly in raw fruits using a continuous flow system based on microdialysis sampling and amperometric detection at an integrated enzymatic biosensor.

PubMed

Vargas, E; Ruiz, M A; Campuzano, S; Reviejo, A J; Pingarrón, J M

2016-03-31

A non-destructive, rapid and simple to use sensing method for direct determination of glucose in non-processed fruits is described. The strategy involved on-line microdialysis sampling coupled with a continuous flow system with amperometric detection at an enzymatic biosensor. Apart from direct determination of glucose in fruit juices and blended fruits, this work describes for the first time the successful application of an enzymatic biosensor-based electrochemical approach to the non-invasive determination of glucose in raw fruits. The methodology correlates, through previous calibration set-up, the amperometric signal generated from glucose in non-processed fruits with its content in % (w/w). The comparison of the obtained results using the proposed approach in different fruits with those provided by other method involving the same commercial biosensor as amperometric detector in stirred solutions pointed out that there were no significant differences. Moreover, in comparison with other available methodologies, this microdialysis-coupled continuous flow system amperometric biosensor-based procedure features straightforward sample preparation, low cost, reduced assay time (sampling rate of 7 h(-1)) and ease of automation. Copyright © 2016 Elsevier B.V. All rights reserved.

Analytical possibilities of different X-ray fluorescence systems for determination of trace elements in aqueous samples pre-concentrated with carbon nanotubes

NASA Astrophysics Data System (ADS)

Marguí, E.; Zawisza, B.; Skorek, R.; Theato, T.; Queralt, I.; Hidalgo, M.; Sitko, R.

2013-10-01

This study was aimed to achieve improved instrumental sensitivity and detection limits for multielement determination of V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Se, Pb and Cd in liquid samples by using different X-ray fluorescence (XRF) configurations (a benchtop energy-dispersive X-ray fluorescence spectrometer, a benchtop polarised energy-dispersive X-ray fluorescence spectrometer and a wavelength-dispersive X-ray fluorescence spectrometer). The preconcentration of metals from liquid solutions consisted on a solid-phase extraction using carbon nanotubes (CNTs) as solid sorbents. After the extraction step, the aqueous sample was filtered and CNTs with the absorbed elements were collected onto a filter paper which was directly analyzed by XRF. The calculated detection limits in all cases were in the low ng mL- 1 range. Nevertheless, results obtained indicate the benefits, in terms of sensitivity, of using polarized X-ray sources using different secondary targets in comparison to conventional XRF systems, above all if Cd determination is required. The developed methodologies, using the aforementioned equipments, have been applied for multielement determination in water samples from an industrial area of Poland.

Stirring the motivational soup: within-person latent profiles of motivation in exercise.

PubMed

Lindwall, Magnus; Ivarsson, Andreas; Weman-Josefsson, Karin; Jonsson, Linus; Ntoumanis, Nikos; Patrick, Heather; Thøgersen-Ntoumani, Cecilie; Markland, David; Teixeira, Pedro

2017-01-14

The purpose of the present study was to use a person-oriented analytical approach to identify latent motivational profiles, based on the different behavioural regulations for exercise, and to examine differences in satisfaction of basic psychological needs (competence, autonomy and relatedness) and exercise behaviour across these motivational profiles. Two samples, consisting of 1084 and 511 adults respectively, completed exercise-related measures of behavioural regulation and psychological need satisfaction as well as exercise behaviour. Latent profile analyses were used to identify motivational profiles. Six profiles, representing different combinations of regulations for exercise, were found to best represent data in both samples. Some profiles were found in both samples (e.g., low motivation profile, self-determined motivation profile and self-determined with high introjected regulation profile), whereas others were unique to each sample. In line with the Self-Determination Theory, individuals belonging to more self-determined profiles demonstrated higher scores on need satisfaction. The results support the notions of motivation being a multidimensional construct and that people have different, sometimes competing, reasons for engaging in exercise. The benefits of using person-oriented analyses to examine within-person interactions of motivation and different regulations are discussed.