Determination of plutonium-239, thorium-232, and natural uranium isotopic concentrations in biological samples using photofission track analysis

NASA Astrophysics Data System (ADS)

Parry, James Roswell

Fission track analysis (FTA) has many uses in the scientific community including but not limited to geological dating, neutron flux mapping, and dose reconstruction. The common method of fission for FTA is through neutrons from a nuclear reactor. This dissertation investigates the use of bremsstrahlung radiation produced from an electron linear accelerator to induce fission in FTA samples. This provides a means of simultaneously measuring the amount of Pu-239, U-nat, and Th-232 in a single sample. The benefit of measuring the three isotopes simultaneously is the possible elimination of costly and time consuming chemical processing for dose reconstruction samples. Samples containing the three isotopes were irradiated in two different bremsstrahlung spectra and a neutron spectrum to determine the amount of Pu-239, U-nat, and Th-232 in the samples. The reaction rate from the calibration samples and the counted fission tracks on the samples were used in determining the concentration of each isotope in the samples. The results were accurate to within a factor of two or three, showing that the method can work to predict the concentrations of multiple isotopes in a sample. The limitations of current accelerators and detectors limits the application of this specific procedure to higher concentrations of isotopes. The method detection limits for Pu-239, U-nat, and Th-232 are 20 pCi, 1 fCi, and 0.4 flCI respectively. Analysis of extremely low concentrations of isotopes would require the use of different detectors such as quartz due to the embrittlement encountered in the Lexan at high exposures. Cracking of the Texan detectors started to appear at a fluence of about 2 x 1018 electrons from the accelerator. This may be partly due to the beam stop not being an adequate thickness. The procedure is likely limited to specialty applications for the near term. However, with the world concerns of exposure to depleted uranium, this procedure may find applications in this area since it would be simple to adapt the procedure to depleted uranium detection.

Comparison of methods for the enumeration of enterohemorrhagic Escherichia coli from veal hides and carcasses.

PubMed

Luedtke, Brandon E; Bosilevac, Joseph M

2015-01-01

The increased association of enterohemorrhagic Escherichia coli (EHEC) with veal calves has led the United States Department of Agriculture Food Safety and Inspection Service to report results of veal meat contaminated with the Top 7 serogroups separately from beef cattle. However, detection methods that can also provide concentration for determining the prevalence and abundance of EHEC associated with veal are lacking. Here we compared the ability of qPCR and a molecular based most probable number assay (MPN) to detect and enumerate EHEC from veal hides at the abattoir and the resulting pre-intervention carcasses. In addition, digital PCR (dPCR) was used to analyze select samples. The qPCR assay was able to enumerate total EHEC in 32% of the hide samples with a range of approximately 34 to 91,412 CFUs/100 cm(2) (95% CI 4-113,460 CFUs/100 cm(2)). Using the MPN assay, total EHEC was enumerable in 48% of the hide samples and ranged from approximately 1 to greater than 17,022 CFUs/100 cm(2) (95% CI 0.4-72,000 CFUs/100 cm(2)). The carcass samples had lower amounts of EHEC with a range of approximately 4-275 CFUs/100 cm(2) (95% CI 3-953 CFUs/100 cm(2)) from 17% of samples with an enumerable amount of EHEC by qPCR. For the MPN assay, the carcass samples ranged from 0.1 to 1 CFUs/100 cm(2) (95% CI 0.02-4 CFUs/100 cm(2)) from 29% of the samples. The correlation coefficient between the qPCR and MPN enumeration methods indicated a moderate relation (R (2) = 0.39) for the hide samples while the carcass samples had no relation (R (2) = 0.002), which was likely due to most samples having an amount of total EHEC below the reliable limit of quantification for qPCR. Interestingly, after enrichment, 81% of the hide samples and 94% of the carcass samples had a detectable amount of total EHEC by qPCR. From our analysis, the MPN assay provided a higher percentage of enumerable hide and carcass samples, however determining an appropriate dilution range and the limited throughput offer additional challenges.

Validity of the WISC-IV Spanish for a Clinically Referred Sample of Hispanic Children

ERIC Educational Resources Information Center

San Miguel Montes, Liza E.; Allen, Daniel N.; Puente, Antonio E.; Neblina, Cris

2010-01-01

The Wechsler Intelligence Scale for Children (WISC) is the most commonly used intelligence test for children. Five years ago, a Spanish version of the WISC-IV was published (WISC-IV Spanish; Wechsler, 2005), but a limited amount of published information is available regarding its utility when assessing clinical samples. The current study included…

Determination of selected neurotoxic insecticides in small amounts of animal tissue utilizing a newly constructed mini-extractor.

PubMed

Seifertová, Marta; Čechová, Eliška; Llansola, Marta; Felipo, Vicente; Vykoukalová, Martina; Kočan, Anton

2017-10-01

We developed a simple analytical method for the simultaneous determination of representatives of various groups of neurotoxic insecticides (carbaryl, chlorpyrifos, cypermethrin, and α-endosulfan and β-endosulfan and their metabolite endosulfan sulfate) in limited amounts of animal tissues containing different amounts of lipids. Selected tissues (rodent fat, liver, and brain) were extracted in a special in-house-designed mini-extractor constructed on the basis of the Soxhlet and Twisselmann extractors. A dried tissue sample placed in a small cartridge was extracted, while the nascent extract was simultaneously filtered through a layer of sodium sulfate. The extraction was followed by combined clean-up, including gel permeation chromatography (in case of high lipid content), ultrasonication, and solid-phase extraction chromatography using C 18 on silica and aluminum oxide. Gas chromatography coupled with high-resolution mass spectrometry was used for analyte separation, detection, and quantification. Average recoveries for individual insecticides ranged from 82 to 111%. Expanded measurement uncertainties were generally lower than 35%. The developed method was successfully applied to rat tissue samples obtained from an animal model dealing with insecticide exposure during brain development. This method may also be applied to the analytical treatment of small amounts of various types of animal and human tissue samples. A significant advantage achieved using this method is high sample throughput due to the simultaneous treatment of many samples. Graphical abstract Optimized workflow for the determination of selected insecticides in small amounts of animal tissue including newly developed mini-extractor.

7 CFR 58.938 - Physical requirements and microbiological limits for sweetened condensed milk.

Code of Federal Regulations, 2013 CFR

2013-01-01

... retain a definite form. (e) Microbiological limits. (1) Coliforms, less than 10 per gram; (2) yeasts, less than 5 per gram; (3) molds, less than 5 per gram; (4) total plate count, less than 1,000 per gram... amount of sediment retained on a lintine disc after a sample composed of 225 grams of product dissolved...

Determination of phosphorus in small amounts of protein samples by ICP-MS.

PubMed

Becker, J Sabine; Boulyga, Sergei F; Pickhardt, Carola; Becker, J; Buddrus, Stefan; Przybylski, Michael

2003-02-01

Inductively coupled plasma mass spectrometry (ICP-MS) is used for phosphorus determination in protein samples. A small amount of solid protein sample (down to 1 micro g) or digest (1-10 micro L) protein solution was denatured in nitric acid and hydrogen peroxide by closed-microvessel microwave digestion. Phosphorus determination was performed with an optimized analytical method using a double-focusing sector field inductively coupled plasma mass spectrometer (ICP-SFMS) and quadrupole-based ICP-MS (ICP-QMS). For quality control of phosphorus determination a certified reference material (CRM), single cell proteins (BCR 273) with a high phosphorus content of 26.8+/-0.4 mg g(-1), was analyzed. For studies on phosphorus determination in proteins while reducing the sample amount as low as possible the homogeneity of CRM BCR 273 was investigated. Relative standard deviation and measurement accuracy in ICP-QMS was within 2%, 3.5%, 11% and 12% when using CRM BCR 273 sample weights of 40 mg, 5 mg, 1 mg and 0.3 mg, respectively. The lowest possible sample weight for an accurate phosphorus analysis in protein samples by ICP-MS is discussed. The analytical method developed was applied for the analysis of homogeneous protein samples in very low amounts [1-100 micro g of solid protein sample, e.g. beta-casein or down to 1 micro L of protein or digest in solution (e.g., tau protein)]. A further reduction of the diluted protein solution volume was achieved by the application of flow injection in ICP-SFMS, which is discussed with reference to real protein digests after protein separation using 2D gel electrophoresis.The detection limits for phosphorus in biological samples were determined by ICP-SFMS down to the ng g(-1) level. The present work discusses the figure of merit for the determination of phosphorus in a small amount of protein sample with ICP-SFMS in comparison to ICP-QMS.

ABRF-MARG RESEARCH STUDY: EVALUATION OF SMALL SAMPLE NUCLEIC ACID AMPLIFICATION TECHNOLOGIES FOR GENE EXPRESSION PROFILING

EPA Science Inventory

Microarrays have had a significant impact on many areas of biology. However, there are still many fertile research areas that would benefit from microarray analysis but are limited by the amount of biological material that can be obtained (e.g. samples obtained by small biopsy, f...

Ochratoxin A in cereal-based baby foods: occurrence and safety evaluation.

PubMed

Beretta, B; De Domenico, R; Gaiaschi, A; Ballabio, C; Galli, C L; Gigliotti, C; Restani, P

2002-01-01

Ochratoxin A is a typical cereal contaminant with strong nephrotoxic activity. To estimate the quantity of ochratoxin A that can be taken in by a child in the weaning period, several samples of cereal-based baby foods were analysed. Although most samples analysed contained ochratoxin A in undetectable amounts or below the Italian legal limit of 0.5 microg kg(-1), some irregular products were found. In particular, the analyses of the 119 batches (338 samples) of baby foods considered indicated that: 20 batches (16.8%) contained detectable quantities of ochratoxin A and four of these (3.4% of the total) contained ochratoxin A above the Italian permitted value. All samples coming from agricultural practices based on integrated pest management contained undetectable amounts of ochratoxin A, while approximately 5% of batches coming from conventional and organic agricultural practices were above the legal limit. On the basis of the established provisional tolerable weekly intake (PTWI), there is no significant toxicological risk for a child who occasionally consumes a formula with ochratoxin concentration slightly above the permitted level. However, stricter controls have to be applied to reject the batches containing irregular concentrations of ochratoxin A.

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

PubMed

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

2008-01-01

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

Three distinct pneumotypes characterize the microbiome of the lung in BALB/cJ mice.

PubMed

Scheiermann, Julia; Klinman, Dennis M

2017-01-01

Bacteria can rarely be isolated from normal healthy lungs using conventional culture techniques, supporting the traditional belief that the lungs are sterile. Yet recent studies using next generation sequencing report that bacterial DNA commonly found in the upper respiratory tract (URT) is present at lower levels in the lungs. Interpretation of that finding is complicated by the technical limitations and potential for contamination introduced when dealing with low biomass samples. The current work sought to overcome those limitations to clarify the number, type and source of bacteria present in the lungs of normal mice. Results showed that the oral microbiome is diverse and highly conserved whereas murine lung samples fall into three distinct patterns. 33% of the samples were sterile, as they lacked culturable bacteria and their bacterial DNA content did not differ from background. 9% of samples contained comparatively higher amounts of bacterial DNA whose composition mimicked that detected in the URT. A final group (58%) contained smaller amounts of microbial DNA whose composition was correlating to that of rodent chow and cage bedding, likely acquired by inspiration of food and bedding fragments. By analyzing each sample independently rather than working with group averages, this work eliminated the bias introduced by aspiration-contaminated samples to establish that three distinct microbiome pneumotypes are present in normal murine lungs.

Autonomous Sample Acquisition for Planetary and Small Body Explorations

NASA Technical Reports Server (NTRS)

Ghavimi, Ali R.; Serricchio, Frederick; Dolgin, Ben; Hadaegh, Fred Y.

2000-01-01

Robotic drilling and autonomous sample acquisition are considered as the key technology requirements in future planetary or small body exploration missions. Core sampling or subsurface drilling operation is envisioned to be off rovers or landers. These supporting platforms are inherently flexible, light, and can withstand only limited amount of reaction forces and torques. This, together with unknown properties of sampled materials, makes the sampling operation a tedious task and quite challenging. This paper highlights the recent advancements in the sample acquisition control system design and development for the in situ scientific exploration of planetary and small interplanetary missions.

CONDUCTING-POLYMER NANOWIRE IMMUNOSENSOR ARRAYS FOR MICROBIAL PATHOGENS

EPA Science Inventory

The lack of methods for routine rapid and sensitive detection and quantification of specific pathogens has limited the amount of information available on their occurrence in drinking water and other environmental samples. The nanowire biosensor arrays developed in this study w...

A proposed method to minimize waste from institutional radiation safety surveillance programs through the application of expected value statistics.

PubMed

Emery, R J

1997-03-01

Institutional radiation safety programs routinely use wipe test sampling and liquid scintillation counting analysis to indicate the presence of removable radioactive contamination. Significant volumes of liquid waste can be generated by such surveillance activities, and the subsequent disposal of these materials can sometimes be difficult and costly. In settings where large numbers of negative results are regularly obtained, the limited grouping of samples for analysis based on expected value statistical techniques is possible. To demonstrate the plausibility of the approach, single wipe samples exposed to varying amounts of contamination were analyzed concurrently with nine non-contaminated samples. Although the sample grouping inevitably leads to increased quenching with liquid scintillation counting systems, the effect did not impact the ability to detect removable contamination in amounts well below recommended action levels. Opportunities to further improve this cost effective semi-quantitative screening procedure are described, including improvements in sample collection procedures, enhancing sample-counting media contact through mixing and extending elution periods, increasing sample counting times, and adjusting institutional action levels.

[Aluminium content in foods with aluminium-containing food additives].

PubMed

Ogimoto, Mami; Suzuki, Kumi; Kabashima, Junichiro; Nakazato, Mitsuo; Uematsu, Yoko

2012-01-01

The aluminium (Al) content of 105 samples, including bakery products made with baking powder, agricultural products and seafoods treated with alum, was investigated. The amounts of Al detected were as follows (limit of quantification: 0.01 mg/g): 0.01-0.37 mg/g in 26 of 57 bakery products, 0.22-0.57 mg/g in 3 of 6 powder mixes, 0.01-0.05 mg/g in all three agricultural products examined, 0.03-0.90 mg/g in 4 of 6 seafood samples, 0.01-0.03 mg/g in 3 of 11 samples of instant noodles, 0.04-0.14 mg/g in 3 of 4 samples of vermicelli, 0.01 mg/g in 1 of 16 soybean products, but none in soybeans. Amounts equivalent to the PTWI of a 16 kg infant were detected in two samples of bakery products, two samples of powder mixes and one sample of salted jellyfish, if each sample was taken once a week. These results suggest that certain foods, depending on the product and the intake, might exceed the PTWI of children, especially infants.

Development of binding assays in microfabricated picoliter vials: an assay for biotin.

PubMed

Grosvenor, A L; Feltus, A; Conover, R C; Daunert, S; Anderson, K W

2000-06-01

A homogeneous binding assay for the detection of biotin in picoliter vials was developed using the photoprotein aequorin as the label. The binding assay was based on the competition of free biotin with biotinylated aequorin (AEQ-biotin) for avidin. A sequential protocol was used, and modification of the assay to reduce the number of steps was examined. Results showed that detection limits on the order of 10(-14) mol of biotin were possible. Reducing the number of steps provided similar detection limits but only if the amount of avidin used was decreased. These binding assays based on picoliter volumes have potential applications in a variety of fields, including microanalysis and single-cell analysis, where the amount of sample is limited. In addition, these assays are suitable for the high-throughput screening of biopharmaceuticals.

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.

Effects of elevated atmospherical CO2 concentration and nitrogen fertilisation on priming effects in soils

NASA Astrophysics Data System (ADS)

Ohm, H.; Marschner, B.

2009-04-01

It is expected that the biomass production and thus the input of organic carbon to the soil will increase in response to elevated CO¬2 concentrations in the atmosphere. It remains unclear whether this will lead to a long term increased carbon pool, because only little is known about the stability of the additional carbon inputs. The soil samples were taken on an agricultural field at the experimental farm of the Federal Agricultural Research Centre (FAL) in Braunschweig, Germany. A Free-Air Carbon-dioxide Enrichment (FACE) system was installed here in May 2000. It consists of rings with 20 m diameter. Two rings were operated with CO2 enriched air (550 ppm), another two rings received ambient air (370 ppm). One half of each ring received the full amount of nitrogen fertiliser, the remainder received only half of this N-amount. The soil samples were taken after 6 years of operation and were incubated with 14C-labeled fructose and alanine for 21 days. Furthermore, combined additions with the respective substrate and ammonium nitrate or ammonium nitrate alone were conducted. The microbial biomass was determined after 2 and 21 days. In the untreated controls the SOC mineralisation amounted to 0.59 to 0.68%. The addition of fructose, fructose+NH4NO3, alanine and alanine+NH4NO3 to the different soil samples increased SOC mineralization and thus caused priming effects of different extents. For NH4NO3 no priming effects occurred. The addition of fructose induced positive priming effects in all samples. The lowest priming effect was observed in the sample ambient CO2+50% N (+50%), either with fructose alone or in combination with NH4NO3. The addition of alanine caused similar priming effects in the ambient CO2+100% N and the elevated CO2+100% N samples (+92.4 and +95.6%, respectively). Again, the lowest priming effect was observed in the sample ambient CO2+50% N. The microbial biomass showed a clear increase in the substrate treated samples compared to the controls. The addition of NH4NO3 did not change the amount of Cmic. The results show, that in no treatment SOC degradation was N-limited, but always limited by easily available energy substrates. On the other hand, N-fertilization had a stronger effect on the microbial response to alanine addition than the CO2-level. Only with low N-fertilization, soils under elevated CO2 are more substrate limited than under elevated CO2, indicating that biomass C-inputs are of different quality.

Measurement of curium in marine samples

NASA Astrophysics Data System (ADS)

Schneider, D. L.; Livingston, H. D.

1984-06-01

Measurement of environmentally small but detectable amounts of curium requires reliable, accureate, and sensitive analytical methods. The radiochemical separation developed at Woods Hole is briefly reviewed with specific reference to radiochemical interferences in the alpha spectrometric measurement of curium nuclides and to the relative amounts of interferences expected in different oceanic regimes and sample types. Detection limits for 242 Cm and 244 Cm are ultimately limited by their presence in the 243Am used as curium yield monitor. Environmental standard reference materials are evaluated with regard to curium. The marine literature is reviewed and curium measurements are discussed in relation to their source of introduction to the environment. Sources include ocean dumping of low-level radioactive wastes and discharges from nuclear fuel reporcessing activities, In particular, the question of a detectable presence of 244Cm in global fallout from nuclear weapons testing is addressed and shown to be essentially negligible. Analyses of Scottish coastal sedimantes show traces of 242Cm and 244Cm activity which are believed to originate from transport from sources in the Irish Sea.

Prevalence and multiplicity of cutaneous beta papilloma viruses in plucked hairs depend on cellular DNA input.

PubMed

Weissenborn, S J; Neale, R; de Koning, M N C; Waterboer, T; Abeni, D; Bouwes Bavinck, J N; Wieland, U; Pfister, H J

2009-11-01

In view of the low loads of beta human papillomaviruses in skin samples, amounts of cellular DNA used in qualitative PCR may become limiting for virus detection and introduce variations in prevalence and multiplicity. This issue was explored within the context of a multicentre study and increasing prevalence and multiplicity was found with increasing input amounts of cellular DNA extracted from hair bulbs. To improve the quality and comparability between different epidemiologic studies ideally equal amounts of cellular DNA should be employed. When cellular DNA input varies this should be clearly taken into account in assessing viral prevalence and multiplicity.

A Rational Approach for Discovering and Validating Cancer Markers in Very Small Samples Using Mass Spectrometry and ELISA Microarrays

DOE PAGES

Zangar, Richard C.; Varnum, Susan M.; Covington, Chandice Y.; ...

2004-01-01

Identifying useful markers of cancer can be problematic due to limited amounts of sample. Some samples such as nipple aspirate fluid (NAF) or early-stage tumors are inherently small. Other samples such as serum are collected in larger volumes but archives of these samples are very valuable and only small amounts of each sample may be available for a single study. Also, given the diverse nature of cancer and the inherent variability in individual protein levels, it seems likely that the best approach to screen for cancer will be to determine the profile of a battery of proteins. As a result,more » a major challenge in identifying protein markers of disease is the ability to screen many proteins using very small amounts of sample. In this review, we outline some technological advances in proteomics that greatly advance this capability. Specifically, we propose a strategy for identifying markers of breast cancer in NAF that utilizes mass spectrometry (MS) to simultaneously screen hundreds or thousands of proteins in each sample. The best potential markers identified by the MS analysis can then be extensively characterized using an ELISA microarray assay. Because the microarray analysis is quantitative and large numbers of samples can be efficiently analyzed, this approach offers the ability to rapidly assess a battery of selected proteins in a manner that is directly relevant to traditional clinical assays.« less

Acoustic Sample Deposition MALDI-MS (ASD-MALDI-MS): A Novel Process Flow for Quality Control Screening of Compound Libraries.

PubMed

Chin, Jefferson; Wood, Elizabeth; Peters, Grace S; Drexler, Dieter M

2016-02-01

In the early stages of drug discovery, high-throughput screening (HTS) of compound libraries against pharmaceutical targets is a common method to identify potential lead molecules. For these HTS campaigns to be efficient and successful, continuous quality control of the compound collection is necessary and crucial. However, the large number of compound samples and the limited sample amount pose unique challenges. Presented here is a proof-of-concept study for a novel process flow for the quality control screening of small-molecule compound libraries that consumes only minimal amounts of samples and affords compound-specific molecular data. This process employs an acoustic sample deposition (ASD) technique for the offline sample preparation by depositing nanoliter volumes in an array format onto microscope glass slides followed by matrix-assisted laser desorption/ionization mass spectrometric (MALDI-MS) analysis. An initial study of a 384-compound array employing the ASD-MALDI-MS workflow resulted in a 75% first-pass positive identification rate with an analysis time of <1 s per sample. © 2015 Society for Laboratory Automation and Screening.

Radioactivites in returned lunar materials and in meteorites

NASA Technical Reports Server (NTRS)

Fireman, E. L.

1983-01-01

The cosmic-ray, solar-flare, and solar-wind bombardments of lunar rocks and soils and meteorites were studied by measurements of tritium, carbon-14 and argon radioactivity. The radioactivity integrates the bombardment for a time period equal to several half-lines. H-3, Ar-37, Ar-39, C-14. For the interior samples of lunar rocks and for deep lunar soil samples, the amounts of the radioactivities were equal to those calculated for galactic cosmic-ray interactions. The top near-surface samples of lunar rocks and the shallow lunar soil samples show excess amounts of the radioactivities attributable to solar flares. Lunar soil fines contain a large amount of hydrogen due to implanted solar wind. Studies of the H-3 in lunar soils and in recovered Surveyor-3 materials gave an upper limit for the H-3/H ratio in the solar wind of 10 to the -11th power. Solar wind carbon is also implanted on lunar soil fines. Lunar soils collected on the surface contained a 0.14 component attributable to implanted solar wind C-14. The C-14/H ratio attributed to the solar wind from this C-14 excess is approximately 4 x 10 to the -11th power.

OBT analysis method using polyethylene beads for limited quantities of animal tissue.

PubMed

Kim, S B; Stuart, M

2015-08-01

This study presents a polyethylene beads method for OBT determination in animal tissues and animal products for cases where the amount of water recovered by combustion is limited by sample size or quantity. In the method, the amount of water recovered after combustion is enhanced by adding tritium-free polyethylene beads to the sample prior to combustion in an oxygen bomb. The method reduces process time by allowing the combustion water to be easily collected with a pipette. Sufficient water recovery was achieved using the polyethylene beads method when 2 g of dry animal tissue or animal product were combusted with 2 g of polyethylene beads. Correction factors, which account for the dilution due to the combustion water of the beads, are provided for beef, chicken, pork, fish and clams, as well as egg, milk and cheese. The method was tested by comparing its OBT results with those of the conventional method using animal samples collected on the Chalk River Laboratories (CRL) site. The results determined that the polyethylene beads method added no more than 25% uncertainty when appropriate correction factors are used. Crown Copyright © 2015. Published by Elsevier Ltd. All rights reserved.

Levels of organophosphorus pesticides in medicinal plants commonly consumed in Iran

PubMed Central

2012-01-01

The frequent occurrence of pesticide residues in herbal materials was indicated by previous studies. In this study, the concentration of some of the organophosphorus pesticides including parathion, malathion, diazinon and pirimiphos methyl in different kinds of medicinal plants were determined. The samples were collected randomly from ten local markets of different areas of Iran. At the detection limit of 0.5 ng g-1, parathion and pirimiphos methyl were not detected in any of the samples. Some amounts of malathion and diazinon were found in Zataria, Matricaria chamomile, Spearmint and Cumin Seed samples while, the concentrations of target organophosphorus pesticides in Borage samples were below the detection limits of the methods which could be a result of intensive transformation of organophosphorus pesticides by Borage. In addition the organophosphorus pesticides were detected in all of the samples below the maximum residue levels (MRLs) proposed by the international organizations. PMID:23351610

High-speed fixed-target serial virus crystallography

DOE PAGES

Roedig, Philip; Ginn, Helen M.; Pakendorf, Tim; ...

2017-06-19

Here, we report a method for serial X-ray crystallography at X-ray free-electron lasers (XFELs), which allows for full use of the current 120-Hz repetition rate of the Linear Coherent Light Source (LCLS). Using a micropatterned silicon chip in combination with the high-speed Roadrunner goniometer for sample delivery, we were able to determine the crystal structures of the picornavirus bovine enterovirus 2 (BEV2) and the cytoplasmic polyhedrosis virus type 18 polyhedrin, with total data collection times of less than 14 and 10 min, respectively. Our method requires only micrograms of sample and should therefore broaden the applicability of serial femtosecond crystallographymore » to challenging projects for which only limited sample amounts are available. By synchronizing the sample exchange to the XFEL repetition rate, our method allows for most efficient use of the limited beam time available at XFELs and should enable a substantial increase in sample throughput at these facilities.« less

High-speed fixed-target serial virus crystallography

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

Roedig, Philip; Ginn, Helen M.; Pakendorf, Tim

Here, we report a method for serial X-ray crystallography at X-ray free-electron lasers (XFELs), which allows for full use of the current 120-Hz repetition rate of the Linear Coherent Light Source (LCLS). Using a micropatterned silicon chip in combination with the high-speed Roadrunner goniometer for sample delivery, we were able to determine the crystal structures of the picornavirus bovine enterovirus 2 (BEV2) and the cytoplasmic polyhedrosis virus type 18 polyhedrin, with total data collection times of less than 14 and 10 min, respectively. Our method requires only micrograms of sample and should therefore broaden the applicability of serial femtosecond crystallographymore » to challenging projects for which only limited sample amounts are available. By synchronizing the sample exchange to the XFEL repetition rate, our method allows for most efficient use of the limited beam time available at XFELs and should enable a substantial increase in sample throughput at these facilities.« less

High-speed fixed-target serial virus crystallography

PubMed Central

Roedig, Philip; Ginn, Helen M.; Pakendorf, Tim; Sutton, Geoff; Harlos, Karl; Walter, Thomas S.; Meyer, Jan; Fischer, Pontus; Duman, Ramona; Vartiainen, Ismo; Reime, Bernd; Warmer, Martin; Brewster, Aaron S.; Young, Iris D.; Michels-Clark, Tara; Sauter, Nicholas K.; Kotecha, Abhay; Kelly, James; Rowlands, David J.; Sikorsky, Marcin; Nelson, Silke; Damiani, Daniel S.; Alonso-Mori, Roberto; Ren, Jingshan; Fry, Elizabeth E.; David, Christian; Stuart, David I.; Wagner, Armin; Meents, Alke

2017-01-01

We report a method for serial X-ray crystallography at X-ray free electron lasers (XFELs), which allows for full use of the current 120 Hz repetition rate of the Linear Coherent Light Source (LCLS). Using a micro-patterned silicon chip in combination with the high-speed Roadrunner goniometer for sample delivery we were able to determine the crystal structures of a picornavirus, bovine enterovirus 2 (BEV2), and the cytoplasmic polyhedrosis virus type 18 polyhedrin. Total data collection times were less than 14 and 10 minutes, respectively. Our method requires only micrograms of sample and will therefore broaden the applicability of serial femtosecond crystallography to challenging projects for which only limited sample amounts are available. By synchronizing the sample exchange to the XFEL repetition rate, our method allows for the most efficient use of the limited beamtime available at XFELs and should enable a substantial increase in sample throughput at these facilities. PMID:28628129

Open tubular lab-on-column/mass spectrometry for targeted proteomics of nanogram sample amounts.

PubMed

Hustoft, Hanne Kolsrud; Vehus, Tore; Brandtzaeg, Ole Kristian; Krauss, Stefan; Greibrokk, Tyge; Wilson, Steven Ray; Lundanes, Elsa

2014-01-01

A novel open tubular nanoproteomic platform featuring accelerated on-line protein digestion and high-resolution nano liquid chromatography mass spectrometry (LC-MS) has been developed. The platform features very narrow open tubular columns, and is hence particularly suited for limited sample amounts. For enzymatic digestion of proteins, samples are passed through a 20 µm inner diameter (ID) trypsin + endoproteinase Lys-C immobilized open tubular enzyme reactor (OTER). Resulting peptides are subsequently trapped on a monolithic pre-column and transferred on-line to a 10 µm ID porous layer open tubular (PLOT) liquid chromatography LC separation column. Wnt/ß-catenein signaling pathway (Wnt-pathway) proteins of potentially diagnostic value were digested+detected in targeted-MS/MS mode in small cell samples and tumor tissues within 120 minutes. For example, a potential biomarker Axin1 was identifiable in just 10 ng of sample (protein extract of ∼1,000 HCT15 colon cancer cells). In comprehensive mode, the current OTER-PLOT set-up could be used to identify approximately 1500 proteins in HCT15 cells using a relatively short digestion+detection cycle (240 minutes), outperforming previously reported on-line digestion/separation systems. The platform is fully automated utilizing common commercial instrumentation and parts, while the reactor and columns are simple to produce and have low carry-over. These initial results point to automated solutions for fast and very sensitive MS based proteomics, especially for samples of limited size.

Quality and loudness judgments for music subjected to compression limiting.

PubMed

Croghan, Naomi B H; Arehart, Kathryn H; Kates, James M

2012-08-01

Dynamic-range compression (DRC) is used in the music industry to maximize loudness. The amount of compression applied to commercial recordings has increased over time due to a motivating perspective that louder music is always preferred. In contrast to this viewpoint, artists and consumers have argued that using large amounts of DRC negatively affects the quality of music. However, little research evidence has supported the claims of either position. The present study investigated how DRC affects the perceived loudness and sound quality of recorded music. Rock and classical music samples were peak-normalized and then processed using different amounts of DRC. Normal-hearing listeners rated the processed and unprocessed samples on overall loudness, dynamic range, pleasantness, and preference, using a scaled paired-comparison procedure in two conditions: un-equalized, in which the loudness of the music samples varied, and loudness-equalized, in which loudness differences were minimized. Results indicated that a small amount of compression was preferred in the un-equalized condition, but the highest levels of compression were generally detrimental to quality, whether loudness was equalized or varied. These findings are contrary to the "louder is better" mentality in the music industry and suggest that more conservative use of DRC may be preferred for commercial music.

Going bananas in the radiation laboratory

NASA Astrophysics Data System (ADS)

Hoeling, Barbara; Reed, Douglas; Siegel, P. B.

1999-05-01

A simple setup for measuring the amount of potassium in foods is described. A 3-in. NaI detector is used to measure samples that are 3000 cm3 in size. With moderate shielding, the potassium content can be measured down to a detection limit of a few parts per 10 000.

A Forensic Workshop Report Concerning (1) The Measurement and Analysis of Energetic Materials and (2) Databasing

DTIC Science & Technology

1999-01-01

contaminating the surface. Research efforts to develop an improved sampling method have previously been limited to deposits made from solutions of explosives...explosive per fingerprint calculated in this way has too much variation to allow determination of sampling efficiency or to use this method to prepare...crystals is put into suspension, the actual amount is determined by usual methods including high-performance liquid chromatography (HPLC), gas

Aflatoxin M1 Concentration in Various Dairy Products: Evidence for Biologically Reduced Amount of AFM1 in Yoghurt

PubMed Central

RAHIMIRAD, Amir; MAALEKINEJAD, Hassan; OSTADI, Araz; YEGANEH, Samal; FAHIMI, Samira

2014-01-01

Abstract Background Aflatoxin M1 (AFM1), a carcinogenic substance is found in milk and dairy products. The effect of season and type of dairy products on AFMi level in northern Iran was investigated in this study. Methods Three hundred samples (each season 75 samples) including raw and pasteurized milk, yoghurt, cheese, and cream samples were collected from three distinct milk producing farms. The samples were subjected to chemical and solid phase extractions and were analyzed by using HPLC technique. Recovery percentages, limit of detection and limit of quantification values were determined. Results Seventy percent and 98% were the minimum and maximum recoveries for cheese and raw milk, respectively and 0.021 and 0.063 ppb were the limit of detection and limit of quantification values for AFM1. We found that in autumn and winter the highest level (0.121 ppb) of AFM1 in cheese and cream samples and failed to detect any AFM1 in spring samples. Interestingly, our data showed that the yoghurt samples had the lowest level of AFM1 in all seasons. Conclusion There are significant differences between the AFM1 levels in dairy products in various seasons and also various types of products, suggesting spring and summer yoghurt samples as the safest products from AFM1 level point of view. PMID:25927044

Development of a high-sensitivity BGO well counter for small animal PET studies.

PubMed

Yamamoto, Seiichi; Watabe, Hiroshi; Kanai, Yasukazu; Watabe, Tadashi; Imaizumi, Masao; Shimosegawa, Eku; Hatazawa, Jun

2012-01-01

In quantitative measurements of small animal PET studies, blood sampling is limited due to the small amounts of blood such animals can provide. In addition, injection doses are quite limited. In this situation, a high-sensitivity well counter would be useful for reducing the amount of the blood sample needed from small animals. Bismuth germinate (BGO) has a high stopping power for high-energy gamma rays compared to NaI(Tl), which is commonly used for conventional well counters. We have developed a BGO well counter and have tested it for blood-sampling measurements in small animals. The BGO well counter uses a square BGO block (59 × 59 × 50 mm) with a square open space (27 × 27 × 34 mm) in the center of the block. The BGO block was optically coupled to a 59-mm square-shaped photomultiplier tube (PMT). Signals from the PMT were digitally processed for the integration and energy window setting. The results showed that the energy spectrum of the BGO well counter measured with a Na-22 point source provided counts that were about 6 times higher for a 1022-keV (511 keV × 2) gamma peak than the spectrum of a 2-in. NaI(Tl) well counter. The relative sensitivity of the developed BGO well counter was 3.4 times higher than that of a NaI(Tl) well counter. The time activity curve of arterial blood was obtained successfully with the BGO well counter for a F-18-FDG study on rat. The BGO well counter will contribute to reducing the amount of sampled blood and to improving the throughput of quantitative measurements in small animal PET studies.

Applications of organo-silica nanocomposites for SPNE of Hg(II)

NASA Astrophysics Data System (ADS)

Kaur, Anupreet

2016-02-01

An analytical method using modified SiO2 nanoparticles as solid-phase extractant has been developed for the preconcentration of trace amounts of Hg(II) in different water samples. Conditions of the analysis such as preconcentration factor, effect of pH, sample volume, shaking time, elution conditions and effects of interfering ions for the recovery of analyte were investigated. The adsorption capacity of nanometer SiO2-APTMS was found to be 181.42 µmol g-1 at optimum pH and the detection limit (3σ) was 0.45 µg L-1. The extractant showed rapid kinetic sorption. The adsorption equilibrium of Hg(II) on nanometer SiO2-APTMS was achieved just in 15 min. Adsorbed Hg(II) was easily eluted with 4 mL of 2.0 M hydrochloric acid. The maximum preconcentration factor was 75. The method was applied for the determination of trace amounts of Hg(II) in various synthetic samples and water samples.

Multiplex cDNA quantification method that facilitates the standardization of gene expression data

PubMed Central

Gotoh, Osamu; Murakami, Yasufumi; Suyama, Akira

2011-01-01

Microarray-based gene expression measurement is one of the major methods for transcriptome analysis. However, current microarray data are substantially affected by microarray platforms and RNA references because of the microarray method can provide merely the relative amounts of gene expression levels. Therefore, valid comparisons of the microarray data require standardized platforms, internal and/or external controls and complicated normalizations. These requirements impose limitations on the extensive comparison of gene expression data. Here, we report an effective approach to removing the unfavorable limitations by measuring the absolute amounts of gene expression levels on common DNA microarrays. We have developed a multiplex cDNA quantification method called GEP-DEAN (Gene expression profiling by DCN-encoding-based analysis). The method was validated by using chemically synthesized DNA strands of known quantities and cDNA samples prepared from mouse liver, demonstrating that the absolute amounts of cDNA strands were successfully measured with a sensitivity of 18 zmol in a highly multiplexed manner in 7 h. PMID:21415008

Be-7 as a tracer for short-term soil surface changes - opportunities and limitations

NASA Astrophysics Data System (ADS)

Baumgart, Philipp

2013-04-01

Within the last 20 years the cosmogenic nuclide Beryllium-7 was successfully established as a suitable tracer element to detect soil surface changes with a high accuracy. Particularly soil erosion rates from single precipitation events are in the focus of different studies due to the short radioactive half-life of the Be-7 isotope. High sorption at topmost soil particles and immobility at given pH-values enable fine-scaled erosion modelling down to 2 mm increments. But some important challenging limitations require particular attention, starting from sampling up to the final data evaluation. E.g. these are the realisation of the fine increment soil collection, the limiting amount of measurable samples per campaign due to the short radioactive half-life and the specific requirements for the detector measurements. Both, the high potential and the challenging limitations are presented as well as future perspectives of that tracer method.

A Nationwide Survey of the Quality of Antimalarials in Retail Outlets in Tanzania

PubMed Central

Kaur, Harparkash; Goodman, Catherine; Thompson, Eloise; Thompson, Katy-Anne; Masanja, Irene; Kachur, S. Patrick; Abdulla, Salim

2008-01-01

Introduction Retail pharmaceutical products are commonly used to treat fever and malaria in sub-Saharan African countries. Small scale studies have suggested that poor quality antimalarials are widespread throughout the region, but nationwide data are not available that could lead to generalizable conclusions about the extent to which poor quality drugs are available in African communities. This study aimed to assess the quality of antimalarials available from retail outlets across mainland Tanzania. Methods and Findings We systematically purchased samples of oral antimalarial tablets from retail outlets across 21 districts in mainland Tanzania in 2005. A total of 1080 antimalarial formulations were collected including 679 antifol antimalarial samples (394 sulfadoxine/pyrimethamine and 285 sulfamethoxypyrazine/pyrimethamine), 260 amodiaquine samples, 63 quinine samples, and 51 artemisinin derivative samples. A systematic subsample of 304 products was assessed for quality by laboratory based analysis to determine the amount of the active ingredient and dissolution profile by following the published United States Pharmacopoeia (USP) monogram for the particular tablet being tested. Products for which a published analytical monogram did not exist were assessed on amount of active ingredient alone. Overall 38 or 12.2% of the samples were found to be of poor quality. Of the antifolate antimalarial drugs tested 13.4% were found to be of poor quality by dissolution and content analysis using high-performance liquid chromatography (HPLC). Nearly one quarter (23.8%) of quinine tablets did not comply within the tolerance limits of the dissolution and quantification analysis. Quality of amodiaquine drugs was relatively better but still unacceptable as 7.5% did not comply within the tolerance limits of the dissolution analysis. Formulations of the artemisinin derivatives all contained the stated amount of active ingredient when analysed using HPLC alone. Conclusions Substandard antimalarial formulations were widely available in Tanzania at the time of this study. No products were detected that did not contain any amount of the stated active ingredient. Quinine and sulfadoxine/pyrimethamine products were the most widely available and also the most likely to be of poor quality. Substandard products were identified in all parts of the country and were labeled as made by both domestic and international manufacturers. With the expansion of the retail pharmaceutical sector as a delivery channel for antimalarial formulations the need for regular nationwide monitoring of their quality will become increasingly important. PMID:18923672

A nationwide survey of the quality of antimalarials in retail outlets in Tanzania.

PubMed

Kaur, Harparkash; Goodman, Catherine; Thompson, Eloise; Thompson, Katy-Anne; Masanja, Irene; Kachur, S Patrick; Abdulla, Salim

2008-01-01

Retail pharmaceutical products are commonly used to treat fever and malaria in sub-Saharan African countries. Small scale studies have suggested that poor quality antimalarials are widespread throughout the region, but nationwide data are not available that could lead to generalizable conclusions about the extent to which poor quality drugs are available in African communities. This study aimed to assess the quality of antimalarials available from retail outlets across mainland Tanzania. We systematically purchased samples of oral antimalarial tablets from retail outlets across 21 districts in mainland Tanzania in 2005. A total of 1080 antimalarial formulations were collected including 679 antifol antimalarial samples (394 sulfadoxine/pyrimethamine and 285 sulfamethoxypyrazine/pyrimethamine), 260 amodiaquine samples, 63 quinine samples, and 51 artemisinin derivative samples. A systematic subsample of 304 products was assessed for quality by laboratory based analysis to determine the amount of the active ingredient and dissolution profile by following the published United States Pharmacopoeia (USP) monogram for the particular tablet being tested. Products for which a published analytical monogram did not exist were assessed on amount of active ingredient alone. Overall 38 or 12.2% of the samples were found to be of poor quality. Of the antifolate antimalarial drugs tested 13.4% were found to be of poor quality by dissolution and content analysis using high-performance liquid chromatography (HPLC). Nearly one quarter (23.8%) of quinine tablets did not comply within the tolerance limits of the dissolution and quantification analysis. Quality of amodiaquine drugs was relatively better but still unacceptable as 7.5% did not comply within the tolerance limits of the dissolution analysis. Formulations of the artemisinin derivatives all contained the stated amount of active ingredient when analysed using HPLC alone. Substandard antimalarial formulations were widely available in Tanzania at the time of this study. No products were detected that did not contain any amount of the stated active ingredient. Quinine and sulfadoxine/pyrimethamine products were the most widely available and also the most likely to be of poor quality. Substandard products were identified in all parts of the country and were labeled as made by both domestic and international manufacturers. With the expansion of the retail pharmaceutical sector as a delivery channel for antimalarial formulations the need for regular nationwide monitoring of their quality will become increasingly important.

An investigation of potential applications of OP-SAPS: Operational sampled analog processors

NASA Technical Reports Server (NTRS)

Parrish, E. A.; Mcvey, E. S.

1976-01-01

The impact of charge-coupled device (CCD) processors on future instrumentation was investigated. The CCD devices studied process sampled analog data and are referred to as OP-SAPS - operational sampled analog processors. Preliminary studies into various architectural configurations for systems composed of OP-SAPS show that they have potential in such diverse applications as pattern recognition and automatic control. It appears probable that OP-SAPS may be used to construct computing structures which can serve as special peripherals to large-scale computer complexes used in real time flight simulation. The research was limited to the following benchmark programs: (1) face recognition, (2) voice command and control, (3) terrain classification, and (4) terrain identification. A small amount of effort was spent on examining a method by which OP-SAPS may be used to decrease the limiting ground sampling distance encountered in remote sensing from satellites.

Ultrasound-Assisted Emulsification Microextraction Based on Solidification Floating Organic Drop Trace Amounts of Manganese Prior to Graphite Furnace Atomic Absorption Spectrometry Determination

PubMed Central

Mohadesi, Alireza; Falahnejad, Masoumeh

2012-01-01

In the present study, an ultrasound-assisted emulsification microextraction based on solidification floating organic drop method is described for preconcentration of trace amounts of Mn (II). 2-(5-Bromo-2-pyridylazo)-5 diethylaminophenol was added to a solution of Mn+2 at ph = 10.0. After this, 1-undecanol was added to the solution as an extraction solvent, and solution was stirred. Several factors influencing the microextraction efficiency, such as pH, the amount of chelating agent, nature and volume of extraction solvent, the volume of sample solution, stirring rate, and extraction time were investigated and optimized. Then sample vial was cooled by inserting into an ice bath, and the solidified was transferred into a suitable vial for immediate melting. Finally the sample was injected into a graphite furnace atomic absorption spectrometry. Under the optimum condition the linear dynamic range was 0.50–10.0 ng mL−1 with a correlation coefficient of 0.9926, and the detection limit of 0.3 ng mL−1 was obtained. The enrichment factor was 160. The proposed method was successfully applied for separation and determination of manganese in sea, rain, tap, and river water samples. PMID:22645504

Vocational Assessment of Students with Disadvantages: Their Peculiar Needs.

ERIC Educational Resources Information Center

Nolte, Deborah

A study examined the underlying factor structure of the aptitude tests and work samples being completed by students with educational disadvantages (limited reading and mathematics skills) who were assessed with the current assessment model in the Akron (Ohio) Public Schools. The amount of variance accounted for by the factors was also…

Utility of solid phase spectrophotometry for the modified determination of trace amounts of cadmium in food samples.

PubMed

Amin, Alaa S; Gouda, Ayman A

2012-05-01

A modified selective, highly sensitive and accurate procedure for the determination of trace amounts of cadmium which reacts with 1-(2-benzothiazolylazo)-2-hydroxy-3-naphthoic acid (BTAHNA) to give a deep violet complex with high molar absorptivity (7.05×10(6)Lmol(-1) cm(-1), 3.92×10(7)Lmol(-1)cm(-1), 1.78×10(8)Lmol(-1)cm(-1), and 4.10×10(8)Lmol(-1)cm(-1)), fixed on a Dowex 1-X8 type anion-exchange resin for 10mL, 100mL, 500mL, and 1000mL, respectively. Calibration is linear over the range 0.2-3.5μgL(-1) with RSD of ⩽1.14% (n=10). The detection and quantification limits were calculated. Increasing the sample volume can enhance the sensitivity. The method has been successfully applied for the determination of Cd(II) in food samples, water samples and some salts samples without interfering effect of various cations and anions. Copyright © 2011 Elsevier Ltd. All rights reserved.

Estimation of methanogen biomass via quantitation of coenzyme M

USGS Publications Warehouse

Elias, Dwayne A.; Krumholz, Lee R.; Tanner, Ralph S.; Suflita, Joseph M.

1999-01-01

Determination of the role of methanogenic bacteria in an anaerobic ecosystem often requires quantitation of the organisms. Because of the extreme oxygen sensitivity of these organisms and the inherent limitations of cultural techniques, an accurate biomass value is very difficult to obtain. We standardized a simple method for estimating methanogen biomass in a variety of environmental matrices. In this procedure we used the thiol biomarker coenzyme M (CoM) (2-mercaptoethanesulfonic acid), which is known to be present in all methanogenic bacteria. A high-performance liquid chromatography-based method for detecting thiols in pore water (A. Vairavamurthy and M. Mopper, Anal. Chim. Acta 78:363–370, 1990) was modified in order to quantify CoM in pure cultures, sediments, and sewage water samples. The identity of the CoM derivative was verified by using liquid chromatography-mass spectroscopy. The assay was linear for CoM amounts ranging from 2 to 2,000 pmol, and the detection limit was 2 pmol of CoM/ml of sample. CoM was not adsorbed to sediments. The methanogens tested contained an average of 19.5 nmol of CoM/mg of protein and 0.39 ± 0.07 fmol of CoM/cell. Environmental samples contained an average of 0.41 ± 0.17 fmol/cell based on most-probable-number estimates. CoM was extracted by using 1% tri-(N)-butylphosphine in isopropanol. More than 90% of the CoM was recovered from pure cultures and environmental samples. We observed no interference from sediments in the CoM recovery process, and the method could be completed aerobically within 3 h. Freezing sediment samples resulted in 46 to 83% decreases in the amounts of detectable CoM, whereas freezing had no effect on the amounts of CoM determined in pure cultures. The method described here provides a quick and relatively simple way to estimate methanogenic biomass.

Empirically Optimized Flow Cytometric Immunoassay Validates Ambient Analyte Theory

PubMed Central

Parpia, Zaheer A.; Kelso, David M.

2010-01-01

Ekins’ ambient analyte theory predicts, counter intuitively, that an immunoassay’s limit of detection can be improved by reducing the amount of capture antibody. In addition, it also anticipates that results should be insensitive to the volume of sample as well as the amount of capture antibody added. The objective of this study is to empirically validate all of the performance characteristics predicted by Ekins’ theory. Flow cytometric analysis was used to detect binding between a fluorescent ligand and capture microparticles since it can directly measure fractional occupancy, the primary response variable in ambient analyte theory. After experimentally determining ambient analyte conditions, comparisons were carried out between ambient and non-ambient assays in terms of their signal strengths, limits of detection, and their sensitivity to variations in reaction volume and number of particles. The critical number of binding sites required for an assay to be in the ambient analyte region was estimated to be 0.1VKd. As predicted, such assays exhibited superior signal/noise levels and limits of detection; and were not affected by variations in sample volume and number of binding sites. When the signal detected measures fractional occupancy, ambient analyte theory is an excellent guide to developing assays with superior performance characteristics. PMID:20152793

Preconcentration of Sn (II) using the methylene blue on the activated carbon and its determination by spectrophotometry method.

PubMed

Khodadoust, Saeid; Cham Kouri, Narges

2014-04-05

A simple and accurate spectrophotometric method for determination of trace amounts of Sn (II) ion in soil sample was developed by using the methylene blue (MB) in the presence of activated carbon (AC) as the adsorbent Solid Phase Extraction (SPE) of Sn (II) and then determined by UV-Vis. The Beer's law is obeyed over the concentration range of 1-80ngmL(-1) of Sn (II) with the detection limits of 0.34ngmL(-1). The influence of type and volume of eluent, concentration of MB, pH, and amount of AC on sensitivity of spectrophotometric method were optimized. The method has been successfully applied for Sn (II) ion determination in soil sample. Copyright © 2013 Elsevier B.V. All rights reserved.

On-fiber furan formation from volatile precursors: a critical example of artefact formation during Solid-Phase Microextraction.

PubMed

Adams, An; Van Lancker, Fien; De Meulenaer, Bruno; Owczarek-Fendor, Agnieszka; De Kimpe, Norbert

2012-05-15

For the analysis of furan, a possible carcinogen formed during thermal treatment of food, Solid-Phase Microextraction (SPME) is a preferred and validated sampling method. However, when volatile furan precursors are adsorbed on the carboxen/PDMS fiber, additional amounts of furan can be formed on the fiber during thermal desorption, as shown here for 2-butenal and furfural. No significant increase in furan amounts was found upon heating the furan precursor 2-butenal, indicating that the furan amounts formed during precursor heating experiments are negligible as compared to the additional amounts of furan formed during fiber desorption. This artefactual furan formation increased with increasing desorption time, but especially with increasing desorption temperature. Although this effect was most pronounced on the Carboxen/PDMS SPME-fiber, it was also noted on two other SPME-fibers tested (PDMS and DVB/Carboxen/PDMS). The general impact on furan data from food and model systems in literature will depend on the amounts of volatile precursors present, but will probably remain limited. However, considering the importance of this worldwide food contaminant, special care has to be taken during SPME-analysis of furan. Especially when performing precursor studies, static headspace sampling should preferably be applied for furan analysis. Copyright © 2012 Elsevier B.V. All rights reserved.

Importance of the efficiency of double-stranded DNA formation in cDNA synthesis for the imprecision of microarray expression analysis.

PubMed

Thormar, Hans G; Gudmundsson, Bjarki; Eiriksdottir, Freyja; Kil, Siyoen; Gunnarsson, Gudmundur H; Magnusson, Magnus Karl; Hsu, Jason C; Jonsson, Jon J

2013-04-01

The causes of imprecision in microarray expression analysis are poorly understood, limiting the use of this technology in molecular diagnostics. Two-dimensional strandness-dependent electrophoresis (2D-SDE) separates nucleic acid molecules on the basis of length and strandness, i.e., double-stranded DNA (dsDNA), single-stranded DNA (ssDNA), and RNA·DNA hybrids. We used 2D-SDE to measure the efficiency of cDNA synthesis and its importance for the imprecision of an in vitro transcription-based microarray expression analysis. The relative amount of double-stranded cDNA formed in replicate experiments that used the same RNA sample template was highly variable, ranging between 0% and 72% of the total DNA. Microarray experiments showed an inverse relationship between the difference between sample pairs in probe variance and the relative amount of dsDNA. Approximately 15% of probes showed between-sample variation (P < 0.05) when the dsDNA percentage was between 12% and 35%. In contrast, only 3% of probes showed between-sample variation when the dsDNA percentage was 69% and 72%. Replication experiments of the 35% dsDNA and 72% dsDNA samples were used to separate sample variation from probe replication variation. The estimated SD of the sample-to-sample variation and of the probe replicates was lower in 72% dsDNA samples than in 35% dsDNA samples. Variation in the relative amount of double-stranded cDNA synthesized can be an important component of the imprecision in T7 RNA polymerase-based microarray expression analysis. © 2013 American Association for Clinical Chemistry

Determination of exposure to respirable quartz in the stone crushing units at Azendarian-West of Iran.

PubMed

Bahrami, Abdul Rahman; Golbabai, Faridah; Mahjub, Hossien; Qorbani, Farshid; Aliabadi, Mohsan; Barqi, Mohamadali

2008-08-01

The purpose of this study is to describe the personal exposure to respirable dust and quartz and in stone crushing units located at west of Iran. A size of 40 personal samples and 40 stationary samples were obtained and analysis was done by X-ray diffraction (XRD). The results of personal sampling were shown the concentrations of respirable dust exposure level in workers of process, hopper and drivers were 1.90, 2.22, 1.41 times greater than Occupational Safety and Health Administration permissible exposure limit (OSHA PEL). The average value of total dust and respirable dust emission from stationary sources was 9.46 mg/m(3), 1.24 mg/m(3) respectively, showing that 13.8 % of total dust is respirable. The efficiency of local exhaust ventilation (LEV) to control of particles inside of industrial units was greater than 99%. It is concluded from this research the particulate generated from stone crushing activities contain a significant amount of respirable particle. The amount of free silica in stone quartz is 85 to 97 percent that emission of particles effect to health workers. LEV has important effect in the removal of silica particles in stone crushing units. The worker of hoppers still exposed to silica more than standard limits.

Relationship between environmental factors, dry matter loss and mycotoxin levels in stored wheat and maize infected with Fusarium species.

PubMed

Mylona, Kalliopi; Sulyok, Michael; Magan, Naresh

2012-01-01

This study examined the relationship between storage environmental factors (water activity (a(w)) (0.89-0.97) and temperature (15°C-30°C)), colonisation of wheat and maize by Fusarium graminearum and F. verticillioides respectively and the dry matter losses (DMLs) caused and quantified by contamination with deoxynivalenol (DON), zearalenone (ZEA) and fumonisins (FUMs) during storage. Fungal growth was assessed by the amount of CO(2) produced under different interacting conditions of a(w) and temperature. DMLs were quantified using the cumulative CO(2) data, and these were shown to increase as temperature and a(w) increased. The amount of DON, ZEA (wheat for human consumption) and FUMs (feed maize) produced was significantly affected by the storage conditions. The three toxins however showed different patterns of production. Optimum for DON was at the wettest conditions (0.97a(w)) and the highest temperature assessed (30°C), whereas for ZEA this shifted to 25°C. FUMs were produced in higher amounts in maize at 30°C and 0.97a(w); however, at intermediate a(w) levels (0.955a(w)), the highest production occurred at 25°C followed by 20°C. Polynomial models were developed for the effect of the storage factors on DMLs and toxin production. DMLs under different environmental conditions were significantly correlated with DON and FUMs. DON contamination was above the EU limits in at least 80% of the wheat samples with DMLs >1%, whereas at least 70% of the same samples contained ZEA above the respective EU legislative limits. Similarly, at least 75% of the maize samples with DMLs ≥ 0.9% exceeded the EU limits for the sum of FUMs in feed. These results show that it may be possible to use temporal CO(2) production during storage of grains as an indicator of the level of contamination of the grain with mycotoxins.

Evaluation of heavy metals content in dietary supplements in Lebanon.

PubMed

Korfali, Samira Ibrahim; Hawi, Tamer; Mroueh, Mohamad

2013-01-18

The consumption of dietary supplements is widely spread and on the rise. These dietary supplements are generally used without prescriptions, proper counseling or any awareness of their health risk. The current study aimed at analyzing the metals in 33 samples of imported dietary supplements highly consumed by the Lebanese population, using 3 different techniques, to ensure the safety and increase the awareness of the citizen to benefit from these dietary supplements. Some samples had levels of metals above their maximum allowable levels (Fe: 24%, Zn: 33%, Mn: 27%, Se: 15%, Mo: 12% of samples), but did not pose any health risk because they were below permitted daily exposure limit and recommended daily allowance except for Fe in 6% of the samples. On the other hand, 34% of the samples had Cu levels above allowable limit where 18% of them were above their permitted daily exposure and recommended daily allowance. In contrast, all samples had concentration of Cr, Hg, and Pb below allowable limits and daily exposure. Whereas, 30% of analyzed samples had levels of Cd above allowable levels, and were statistically correlated with Ca, and Zn essential minerals. Similarly 62% of the samples had levels of As above allowable limits and As levels were associated with Fe and Mn essential minerals. Dietary supplements consumed as essential nutrients for their Ca, Zn, Fe and Mn content should be monitored for toxic metal levels due to their natural geochemical association with these essential metals to provide citizens the safe allowable amounts.

Aptamer functionalized magnetic nanoparticles for effective extraction of ultratrace amounts of aflatoxin M1 prior its determination by HPLC.

PubMed

Khodadadi, Mohammad; Malekpour, Akbar; Mehrgardi, Masoud A

2018-06-09

Aptamers, due to the inherently high selectivity towards target analytes, are promising candidate for surface modification of the nanoparticles. Therefore, aptamer-functionalized magnetic nanoparticles (AMNPs) was prepared and used to develop a magnetic solid-phase extraction procedure for clean-up of milk and dairy products samples before measuring the aflatoxin M1 (AFM1) contents by the high-performance liquid chromatography. The prepared sorbent was characterized by different instrumental methods such as FT-IR, FESEM, TEM, EDX and AGFM. The AMNPs was used in extraction and pre-concentration of ultratrace amounts AFM1 from local milk samples. The amount of sorbent, elution volume, extraction time, and salt addition were optimized. Based on the results, calibration plot is linear over the 0.3 to 1 ng·L -1 and 5 to 50 ng·L -1 AFM1 concentration ranges. The limits of detection of the developed method were obtained 0.2 ng·L -1 which is the smallest value that has been reported up to now. The results show that this new superior sorbent has a large potential to simplify the complex matrix of the samples and can used for detection, preconcentration and accurate determination of ultratrace amounts of the AFM1 from milk and dairy products. Copyright © 2018 Elsevier B.V. All rights reserved.

The Potential of Graphene as an Adsorbent for Five Pesticides from Different Classes in Rape Oil Samples Using Dispersive Solid-Phase Extraction.

PubMed

Madej, Katarzyna; Janiga, Katarzyna; Piekoszewski, Wojciech

2018-01-01

Isolation conditions for five pesticides (metazachlor, tebuconazole, λ -cyhalothrin, chlorpyrifos, and deltamethrin) from rape oil samples were examined using the dispersive solid-phase graphene extraction technique. To determine the optimal extraction conditions, a number of experimental factors (amount of graphene, amount of salt, type and volume of the desorbing solvent, desorption time with and without sonication energy, and temperature during desorption) were studied. The compounds of interest were separated and detected by an HPLC-UV employing a Kinetex XB-C18 column and a mobile phase consisting of acetonitrile and water flowing in a gradient mode. The optimized extraction conditions were: the amount of graphene 15 mg, desorbing solvent (acetonitrile) 5 mL, time desorption 10 min at 40°C, and amount of NaCl 1 g. The detection limit for metazachlor, tebuconazole, λ -cyhalothrin, and chlorpyrifos was 62.5 ng·g -1 , and for deltamethrin, it was 500 ng·g -1 . The obtained results lead to the conclusion that graphene may be successfully used for the isolation of the five pesticides from rape oil. However, their determination at low concentration levels, as they occur in real oil samples, requires the employment of appropriately highly sensitive analytical methods, as well as a more suitable graphene form (e.g., magnetically modified graphene).

20 CFR 663.420 - Can the duration and amount of ITA's be limited?

Code of Federal Regulations, 2010 CFR

2010-04-01

... Training Accounts § 663.420 Can the duration and amount of ITA's be limited? (a) Yes, the State or Local Board may impose limits on ITA's, such as limitations on the dollar amount and/or duration. (b) Limits... 20 Employees' Benefits 3 2010-04-01 2010-04-01 false Can the duration and amount of ITA's be...

Determination of rhodamine B in soft drink, waste water and lipstick samples after solid phase extraction.

PubMed

Soylak, Mustafa; Unsal, Yunus Emre; Yilmaz, Erkan; Tuzen, Mustafa

2011-08-01

A new solid phase extraction method is described for sensitive and selective determination of trace levels of rhodamine B in soft drink, food and industrial waste water samples. The method is based on the adsorption of rhodamine B on the Sepabeads SP 70 resin and its elution with 5 mL of acetonitrile in a mini chromatographic column. Rhodamine B was determined by using UV visible spectrophotometry at 556 nm. The effects of different parameters such as pH, amount of rhodamine B, flow rates of sample and eluent solutions, resin amount, and sample volume were investigated. The influences of some alkali, alkali earth and transition metals on the recoveries of rhodamine B were investigated. The preconcentration factor was found 40. The detection limit based on three times the standard deviation of the reagent blank for rhodamine B was 3.14 μg L⁻¹. The relative standard deviations of the procedure were found as 5% in 1×10⁻⁵ mol L⁻¹ rhodamine B. The presented procedure was successfully applied to real samples including soft drink, food and industrial waste water and lipstick samples. Copyright © 2011 Elsevier Ltd. All rights reserved.

Ptychographic overlap constraint errors and the limits of their numerical recovery using conjugate gradient descent methods.

PubMed

Tripathi, Ashish; McNulty, Ian; Shpyrko, Oleg G

2014-01-27

Ptychographic coherent x-ray diffractive imaging is a form of scanning microscopy that does not require optics to image a sample. A series of scanned coherent diffraction patterns recorded from multiple overlapping illuminated regions on the sample are inverted numerically to retrieve its image. The technique recovers the phase lost by detecting the diffraction patterns by using experimentally known constraints, in this case the measured diffraction intensities and the assumed scan positions on the sample. The spatial resolution of the recovered image of the sample is limited by the angular extent over which the diffraction patterns are recorded and how well these constraints are known. Here, we explore how reconstruction quality degrades with uncertainties in the scan positions. We show experimentally that large errors in the assumed scan positions on the sample can be numerically determined and corrected using conjugate gradient descent methods. We also explore in simulations the limits, based on the signal to noise of the diffraction patterns and amount of overlap between adjacent scan positions, of just how large these errors can be and still be rendered tractable by this method.

Detection limits of Legionella pneumophila in environmental samples after co-culture with Acanthamoeba polyphaga

PubMed Central

2013-01-01

Background The efficiency of recovery and the detection limit of Legionella after co-culture with Acanthamoeba polyphaga are not known and so far no investigations have been carried out to determine the efficiency of the recovery of Legionella spp. by co-culture and compare it with that of conventional culturing methods. This study aimed to assess the detection limits of co-culture compared to culture for Legionella pneumophila in compost and air samples. Compost and air samples were spiked with known concentrations of L. pneumophila. Direct culturing and co-culture with amoebae were used in parallel to isolate L. pneumophila and recovery standard curves for both methods were produced for each sample. Results The co-culture proved to be more sensitive than the reference method, detecting 102-103 L. pneumophila cells in 1 g of spiked compost or 1 m3 of spiked air, as compared to 105-106 cells in 1 g of spiked compost and 1 m3 of spiked air. Conclusions Co-culture with amoebae is a useful, sensitive and reliable technique to enrich L. pneumophila in environmental samples that contain only low amounts of bacterial cells. PMID:23442526

N-nitrosodimethylamine, nitrate and nitrate-reducing microorganisms in human milk.

PubMed

Uibu, J; Tauts, O; Levin, A; Shimanovskaya, N; Matto, R

1996-10-01

Of 54 milk samples from 54 healthy nursing women analysed for volatile N-nitrosamines, 42 appeared negative. Trace amounts (below the detection limit 0.5 microgram l-1) of N-nitrosodimethylamine were detected in the milk of 10 mothers and two samples contained this compound at 1.1 and 1.2 micrograms 1-1 respectively. Almost all samples investigated contained nitrate (mean 2.9 +/- 2.3 mg1-1 and nitrate reducing microorganisms (mean 4.2 +/- 1.0 log ml-1). The recent finding of N-nitrosodimethylamine in human milk gives evidence of the continuous endogenous formation of N-nitrosamines.

Virtual harm reduction efforts for Internet gambling: effects of deposit limits on actual Internet sports gambling behavior

PubMed Central

Broda, Anja; LaPlante, Debi A; Nelson, Sarah E; LaBrie, Richard A; Bosworth, Leslie B; Shaffer, Howard J

2008-01-01

Background In an attempt to reduce harm related to gambling problems, an Internet sports betting service provider, bwin Interactive Entertainment, AG (bwin), imposes limits on the amount of money that users can deposit into their online gambling accounts. We examined the effects of these limits on gambling behavior. Methods We compared (1) gambling behavior of those who exceeded deposit limits with those who did not, and (2) gambling behavior before and after exceeding deposit limits. We analyzed 2 years of the actual sports gambling behavior records of 47000 subscribers to bwin. Results Only 160 (0.3%) exceeded deposit limits at least once. Gamblers who exceeded deposit limits evidenced higher average number of bets per active betting day and higher average size of bets than gamblers who did not exceed deposit limits. Comparing the gambling behavior before and after exceeding deposit limits revealed slightly more unfavorable gambling behavior after exceeding deposit limits. Conclusion Our findings indicate that Internet gamblers who exceed deposit limits constitute a group of bettors willing to take high risks; yet, surprisingly, they appear to do this rather successfully because their percentage of losses is lower than others in the sample. However, some of these gamblers exhibit some poor outcomes. Deposit limits might be necessary harm reduction measures to prevent the loss of extremely large amounts of money and cases of bankruptcy. We discuss how these limits might be modified based on our findings. PMID:18684323

Virtual harm reduction efforts for Internet gambling: effects of deposit limits on actual Internet sports gambling behavior.

PubMed

Broda, Anja; LaPlante, Debi A; Nelson, Sarah E; LaBrie, Richard A; Bosworth, Leslie B; Shaffer, Howard J

2008-08-06

In an attempt to reduce harm related to gambling problems, an Internet sports betting service provider, bwin Interactive Entertainment, AG (bwin), imposes limits on the amount of money that users can deposit into their online gambling accounts. We examined the effects of these limits on gambling behavior. We compared (1) gambling behavior of those who exceeded deposit limits with those who did not, and (2) gambling behavior before and after exceeding deposit limits. We analyzed 2 years of the actual sports gambling behavior records of 47000 subscribers to bwin. Only 160 (0.3%) exceeded deposit limits at least once. Gamblers who exceeded deposit limits evidenced higher average number of bets per active betting day and higher average size of bets than gamblers who did not exceed deposit limits. Comparing the gambling behavior before and after exceeding deposit limits revealed slightly more unfavorable gambling behavior after exceeding deposit limits. Our findings indicate that Internet gamblers who exceed deposit limits constitute a group of bettors willing to take high risks; yet, surprisingly, they appear to do this rather successfully because their percentage of losses is lower than others in the sample. However, some of these gamblers exhibit some poor outcomes. Deposit limits might be necessary harm reduction measures to prevent the loss of extremely large amounts of money and cases of bankruptcy. We discuss how these limits might be modified based on our findings.

How College Students Understand Their Self-Control Development: A Qualitative Analysis

ERIC Educational Resources Information Center

Cliburn Allen, Cara; Glanzer, Perry

2017-01-01

Recent research has shown the importance of the positive benefits of high-levels of self-control for both individuals and society. Yet, we know only a limited amount about how college students understand and apply self-control. This qualitative study examined how a national sample of 75 students defined self-control, whether or not they believed…

Attenuation of species abundance distributions by sampling

PubMed Central

Shimadzu, Hideyasu; Darnell, Ross

2015-01-01

Quantifying biodiversity aspects such as species presence/ absence, richness and abundance is an important challenge to answer scientific and resource management questions. In practice, biodiversity can only be assessed from biological material taken by surveys, a difficult task given limited time and resources. A type of random sampling, or often called sub-sampling, is a commonly used technique to reduce the amount of time and effort for investigating large quantities of biological samples. However, it is not immediately clear how (sub-)sampling affects the estimate of biodiversity aspects from a quantitative perspective. This paper specifies the effect of (sub-)sampling as attenuation of the species abundance distribution (SAD), and articulates how the sampling bias is induced to the SAD by random sampling. The framework presented also reveals some confusion in previous theoretical studies. PMID:26064626

Sensitive trace enrichment of environmental andiandrogen vinclozolin from natural waters and sediment samples using hollow-fiber liquid-phase microextraction.

PubMed

Lambropoulou, Dimitra A; Albanis, Triantafyllos A

2004-12-17

The presence of vinclozolin in the environment as far as the endocrine disruption effects in biota are concerned has raised interest in the environmental fate of this compound. In this respect, the present study attempts to investigate the feasibility of applying a novel quantitative method, liquid-phase microextraction (LPME), so as to determine this environmental andiandrogen in environmental samples such as water and sediment samples. The technique involved the use of a small amount (3 microL) of organic solvent impregnated in a hollow fiber membrane, which was attached to the needle of a conventional GC syringe. The extracted samples were analyzed by gas chromatography coupled with electron-capture detection. Experimental LPME conditions such as extraction solvent, stirring rate, content of NaCl and pH were tested. Once LPME was optimized, the performance of the proposed technique was evaluated for the determination of vinclozolin in different types of natural water samples. The recovery of spiked water samples was from 80 to 99%. The procedure was adequate for quantification of vinclozolin in waters at levels of 0.010 to 50 microg/L (r> 0.994) with a detection limit of 0.001 microg/L (S/N= 3). Natural sediment samples from the Aliakmonas River area (Macedonia, Greece) spiked with the target andiandrogen compound were liquid-liquid extracted and analyzed by the methodology developed in this work. No significant interferences from the samples matrix were noticed, indicating that the reported methodology is an innovative tactic for sample preparation in sediment analysis, with a considerable improvement in the achieved detection limits. The results demonstrated that apart from analyte enrichment, the proposed LPME procedure also serves as clean-up method and could be successfully performed to determine trace amounts of vinclozolin in water and sediment samples.

Ionic liquid based dispersive liquid-liquid microextraction for the extraction of pesticides from bananas.

PubMed

Ravelo-Pérez, Lidia M; Hernández-Borges, Javier; Asensio-Ramos, María; Rodríguez-Delgado, Miguel Angel

2009-10-23

This paper describes a dispersive liquid-liquid microextraction (DLLME) procedure using room temperature ionic liquids (RTILs) coupled to high-performance liquid chromatography with diode array detection capable of quantifying trace amounts of eight pesticides (i.e. thiophanate-methyl, carbofuran, carbaryl, tebuconazole, iprodione, oxyfluorfen, hexythiazox and fenazaquin) in bananas. Fruit samples were first homogenized and extracted (1g) with acetonitrile and after suitable evaporation and reconstitution of the extract in 10 mL of water, a DLLME procedure using 1-hexyl-3-methylimidazolium hexafluorophosphate ([C(6)MIM][PF(6)]) as extraction solvent was used. Experimental conditions affecting the DLLME procedure (sample pH, sodium chloride percentage, ionic liquid amount and volume of disperser solvent) were optimized by means of an experimental design. In order to determine the presence of a matrix effect, calibration curves for standards and fortified banana extracts (matrix matched calibration) were studied. Mean recovery values of the extraction of the pesticides from banana samples were in the range of 69-97% (except for thiophanate-methyl and carbofuran, which were 53-63%) with a relative standard deviation lower than 8.7% in all cases. Limits of detection achieved (0.320-4.66 microg/kg) were below the harmonized maximum residue limits established by the European Union (EU). The proposed method, was also applied to the analysis of this group of pesticides in nine banana samples taken from the local markets of the Canary Islands (Spain). To the best of our knowledge, this is the first application of RTILs as extraction solvents for DLLME of pesticides from samples different than water.

Phytochemical fingerprints of lime honey collected in serbia.

PubMed

Gašić, Uroš; Šikoparija, Branko; Tosti, Tomislav; Trifković, Jelena; Milojković-Opsenica, Dušanka; Natić, Maja; Tešić, Živoslav

2014-01-01

Composition of phenolic compounds and the sugar content were determined as the basis for characterization of lime honey from Serbia. Particular attention was given to differences in phytochemical profiles of ripe and unripe lime honey and lime tree nectar. Melissopalynological analysis confirmed domination of Tilia nectar in all analyzed samples. Phenolic acids, abscisic acid, flavonoids, and flavonoid glycosides were determined by means of ultra-HPLC coupled with a hybrid mass spectrometer (UHPLC-OrbiTrap). Sugar content was determined using high-performance anion-exchange chromatography with amperometric detection. Similar phenolic compounds characterized unripe and ripe honeys, while the lime tree nectar profile showed notable differences. Compared to lime tree nectar, a high amount of chrysin, pinocembrin, and galangin were detected in both ripe and unripe lime honey. Fructose and glucose were the major constituents of all investigated samples, and amounts were within the limits established by European Union legislation. Sucrose content in the nectar sample was up to two-fold higher when compared to all honey samples. Isomaltose and gentiobiose with turanose content were different in analyzed production stages of lime honey.

Application of Chitosan-Zinc Oxide Nanoparticles for Lead Extraction From Water Samples by Combining Ant Colony Optimization with Artificial Neural Network

NASA Astrophysics Data System (ADS)

Khajeh, M.; Pourkarami, A.; Arefnejad, E.; Bohlooli, M.; Khatibi, A.; Ghaffari-Moghaddam, M.; Zareian-Jahromi, S.

2017-09-01

Chitosan-zinc oxide nanoparticles (CZPs) were developed for solid-phase extraction. Combined artificial neural network-ant colony optimization (ANN-ACO) was used for the simultaneous preconcentration and determination of lead (Pb2+) ions in water samples prior to graphite furnace atomic absorption spectrometry (GF AAS). The solution pH, mass of adsorbent CZPs, amount of 1-(2-pyridylazo)-2-naphthol (PAN), which was used as a complexing agent, eluent volume, eluent concentration, and flow rates of sample and eluent were used as input parameters of the ANN model, and the percentage of extracted Pb2+ ions was used as the output variable of the model. A multilayer perception network with a back-propagation learning algorithm was used to fit the experimental data. The optimum conditions were obtained based on the ACO. Under the optimized conditions, the limit of detection for Pb2+ ions was found to be 0.078 μg/L. This procedure was also successfully used to determine the amounts of Pb2+ ions in various natural water samples.

[Assessment of Cyto- and Genotoxicity of Underground Waters from the Far Eastern Center on Radioactive Waste Treatment Site].

PubMed

Oudalova, A A; Pyatkova, S V; Geras'kin, S A; Kiselev, S M; Akhromeev, S V

2016-01-01

This study has been completed in the frames of activities on the environment assessment in the vicinity of the Far Eastern center (FEC) on radioactive waste treatment (a branch of Fokino, Sysoev Bay). Underground waters collected at the FEC technical site were surveyed both with instrumental techniques and bioassays. Concentrations of some chemicals (ranged to the third hazard category) in the samples collected are over the permitted limits. Activities of 137Cs and 90Sr in waters amount up to 3.8 and 16.2 Bq/l, correspondingly. The integral pollution index is over 1 in all the samples and could amount up to 165. The Allium-test application allows the detection of the sample points where underground waters have an enhanced mutagenic potential. Dependencies between biological effects and pollution levels are analyzed. The findings obtained could be used for the monitoring optimized and decision making on rehabilitation measures to decrease negative influence of the enterprise on the environment.

Solidified Floating Organic Drop Microextraction for the Detection of Trace Amount of Lead in Various Samples by Electrothermal Atomic Absorption Spectrometry.

PubMed

Aydın Urucu, Oya; Dönmez, Şeyda; Kök Yetimoğlu, Ece

2017-01-01

A novel method was developed for determination of trace amounts of lead in water and food samples. Solidified floating organic drop microextraction was used to preconcentrate the lead ion. After the analyte was complexed with 1-(2-pyridylazo)-2-naphthol, undecanol and acetonitrile were added as extraction and dispersive solvent, respectively. Variables such as pH, volumes of extraction and dispersive solvents, and concentration of chelating agent were optimized. Under the optimum conditions, the detection limit of Pb (II) was determined as 0.042  µ g L -1 with an enrichment factor of 300. The relative standard deviation is <10%. Accuracy of the developed procedure was evaluated by the analysis of certified reference material of human hair (NCS DC 73347) and wastewater (SPS-WW2) with satisfactory results. The developed procedure was then successfully applied to biscuit and water samples for detection of Pb (II) ions.

Solvent microextraction-flame atomic absorption spectrometry (SME-FAAS) for determination of ultratrace amounts of cadmium in meat and fish samples.

PubMed

Goudarzi, Nasser

2009-02-11

A simple, low cost and highly sensitive method based on solvent microextraction (SME) for separation/preconcentration and flame atomic absorption spectrometry (FAAS) was proposed for the determination of ultratrace amounts of cadmium in meat and fish samples. The analytical procedure involved the formation of a hydrophobic complex by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution. In suitable conditions, the complex of cadmium-APDC entered the micro organic phase, and thus, separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, a detection limit (3 sigma) of 0.8 ng L(-1) and an enrichment factor of 93 were achieved. The relative standard deviation for the method was found to be 2.2% for Cd. The interference effects of some anions and cations were also investigated. The developed method has been applied to the determination of trace Cd in meat and fish samples.

Solid phase extraction of trace amounts of Ag, Cd, Cu, and Zn in environmental samples using magnetic nanoparticles coated by 3-(trimethoxysilyl)-1-propantiol and modified with 2-amino-5-mercapto-1,3,4-thiadiazole and their determination by ICP-OES.

PubMed

Mashhadizadeh, Mohammad Hossein; Karami, Zahra

2011-06-15

A fast, sensitive, and simple method using magnetic nanoparticles (MNPs) coated by 3-(trimethoxysilyl)-1-propantiol and modified with 2-amino-5-mercapto-1,3,4-thiadiazole, as an adsorbent has been successfully developed for extraction, preconcentration, and determination of trace amounts of Ag, Cd, Cu, and Zn from environmental samples. The prepared nanoparticles were characterized by Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). These magnetic nanoparticles can be easily dispersed in aqueous samples and retrieved by the application of external magnetic field via a piece of permanent magnet. The main factors affecting the extraction efficiency such as pH value, sample volume, eluent concentration and volume, ultrasonication time, and coexisting ions have been investigated and established. Under the optimal conditions, high concentration factors (194, 190, 170, and 182) were achieved for Ag, Cd, Cu, and Zn with relative standard deviations of 5.31%, 4.03%, 3.62%, and 4.20%, respectively. The limits of detection for Ag, Cd, Cu, and Zn were as low as 0.12, 0.12, 0.13 and 0.11 ng mL(-1). The prepared sorbent was applied for preconcentration of trace amounts of Ag, Cd, Cu, and Zn in the various water samples with satisfactory results. Copyright © 2011 Elsevier B.V. All rights reserved.

The MPLEx Protocol for Multi-omic Analyses of Soil Samples

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

Nicora, Carrie D.; Burnum-Johnson, Kristin E.; Nakayasu, Ernesto S.

Mass spectrometry (MS)-based integrated metaproteomic, metabolomic and lipidomic (multi-omic) studies are transforming our ability to understand and characterize microbial communities in environmental and biological systems. These measurements are even enabling enhanced analyses of complex soil microbial communities, which are the most complex microbial systems known to date. Multi-omic analyses, however, do have sample preparation challenges since separate extractions are typically needed for each omic study, thereby greatly amplifying the preparation time and amount of sample required. To address this limitation, a 3-in-1 method for simultaneous metabolite, protein, and lipid extraction (MPLEx) from the exact same soil sample was created bymore » adapting a solvent-based approach. This MPLEx protocol has proven to be simple yet robust for many sample types and even when utilized for limited quantities of complex soil samples. The MPLEx method also greatly enabled the rapid multi-omic measurements needed to gain a better understanding of the members of each microbial community, while evaluating the changes taking place upon biological and environmental perturbations.« less

Ultrasound-assisted dispersive magnetic solid phase extraction based on amino-functionalized Fe3O4 adsorbent for recovery of clomipramine from human plasma and its determination by high performance liquid chromatography: Optimization by experimental design.

PubMed

Hamidi, Fatemeh; Hadjmohammadi, Mohammad Reza; Aghaie, Ali B G

2017-09-15

The applicability of Amino-functionalized Fe 3 O 4 nanoparticles (NPs) as an effective adsorbent was developed for the extraction and determination of clomipramine (CLP) in plasma sample by ultrasound-assisted dispersive magnetic solid phase extraction (UADM-SPE) and high-performance liquid chromatography-ultraviolet (HPLC-UV) detection. Fabrication of the Fe 3 O 4 @SiO 2 -NH 2 magnetic nanoparticles confirmed by Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The effect of different extraction parameters (i.e. pH of the sample solution, the amount of magnetic nanoparticles (MNPs), sample volume, temperature and sonication time) on the extraction recovery of CLP were investigated by response surface methodology through central composite design (CCD). The optimum condition is obtained when the affecting parameters are set to: pH of the sample solution=9, the amount of MNPs=37mg, sample volume=23mL, 25°C temperature and sonication time=1min. Under the optimum condition, extraction recovery was 90.6% with relative standard deviation of 3.5%, and enrichment factor of 117. The linear range for determination of CLP was 0.017-0.70mgL -1 with a determination coefficient (R 2 ) of 0.999. Limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.0167mgL -1 , respectively. The established UADM-SPE-HPLC-UV method was rapid, simple and efficient for determination of CLP in human plasma samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of heavy metals content in dietary supplements in Lebanon

PubMed Central

2013-01-01

Background The consumption of dietary supplements is widely spread and on the rise. These dietary supplements are generally used without prescriptions, proper counseling or any awareness of their health risk. The current study aimed at analyzing the metals in 33 samples of imported dietary supplements highly consumed by the Lebanese population, using 3 different techniques, to ensure the safety and increase the awareness of the citizen to benefit from these dietary supplements. Results Some samples had levels of metals above their maximum allowable levels (Fe: 24%, Zn: 33%, Mn: 27%, Se: 15%, Mo: 12% of samples), but did not pose any health risk because they were below permitted daily exposure limit and recommended daily allowance except for Fe in 6% of the samples. On the other hand, 34% of the samples had Cu levels above allowable limit where 18% of them were above their permitted daily exposure and recommended daily allowance. In contrast, all samples had concentration of Cr, Hg, and Pb below allowable limits and daily exposure. Whereas, 30% of analyzed samples had levels of Cd above allowable levels, and were statistically correlated with Ca, and Zn essential minerals. Similarly 62% of the samples had levels of As above allowable limits and As levels were associated with Fe and Mn essential minerals. Conclusion Dietary supplements consumed as essential nutrients for their Ca, Zn, Fe and Mn content should be monitored for toxic metal levels due to their natural geochemical association with these essential metals to provide citizens the safe allowable amounts. PMID:23331553

Multiplexed Microsphere Suspension-Array Assay for Urine Mitochondrial DNA Typing by C-Stretch Length in Hypervariable Regions.

PubMed

Aoki, Kimiko; Tanaka, Hiroyuki; Kawahara, Takashi

2018-07-01

The standard method for personal identification and verification of urine samples in doping control is short tandem repeat (STR) analysis using nuclear DNA (nDNA). The DNA concentration of urine is very low and decreases under most conditions used for sample storage; therefore, the amount of DNA from cryopreserved urine samples may be insufficient for STR analysis. We aimed to establish a multiplexed assay for urine mitochondrial DNA typing containing only trace amounts of DNA, particularly for Japanese populations. A multiplexed suspension-array assay using oligo-tagged microspheres (Luminex MagPlex-TAG) was developed to measure C-stretch length in hypervariable region 1 (HV1) and 2 (HV2), five single nucleotide polymorphisms (SNPs), and one polymorphic indel. Based on these SNPs and the indel, the Japanese population can be classified into five major haplogroups (D4, B, M7a, A, D5). The assay was applied to DNA samples from urine cryopreserved for 1 - 1.5 years (n = 63) and fresh blood (n = 150). The assay with blood DNA enabled Japanese subjects to be categorized into 62 types, exhibiting a discriminatory power of 0.960. The detection limit for cryopreserved urine was 0.005 ng of nDNA. Profiling of blood and urine pairs revealed that 5 of 63 pairs showed different C-stretch patterns in HV1 or HV2. The assay described here yields valuable information in terms of the verification of urine sample sources employing only trace amounts of recovered DNA. However, blood cannot be used as a reference sample.

The role of parenting in the prediction of criminal involvement: findings from a nationally representative sample of youth and a sample of adopted youth.

PubMed

Beaver, Kevin M; Schwartz, Joseph A; Connolly, Eric J; Al-Ghamdi, Mohammed Said; Kobeisy, Ahmed Nezar

2015-03-01

The role of parenting in the development of criminal behavior has been the source of a vast amount of research, with the majority of studies detecting statistically significant associations between dimensions of parenting and measures of criminal involvement. An emerging group of scholars, however, has drawn attention to the methodological limitations-mainly genetic confounding-of the parental socialization literature. The current study addressed this limitation by analyzing a sample of adoptees to assess the association between 8 parenting measures and 4 criminal justice outcome measures. The results revealed very little evidence of parental socialization effects on criminal behavior before controlling for genetic confounding and no evidence of parental socialization effects on criminal involvement after controlling for genetic confounding. (PsycINFO Database Record (c) 2015 APA, all rights reserved).

Monitoring of chlorsulfuron in biological fluids and water samples by molecular fluorescence using rhodamine B as fluorophore.

PubMed

Alesso, Magdalena; Escudero, Luis A; Talio, María Carolina; Fernández, Liliana P

2016-11-01

A new simple methodology is proposed for chlorsufuron (CS) traces quantification based upon enhancement of rhodamine B (RhB) fluorescent signal. Experimental variables that influence fluorimetric sensitivity have been studied and optimized. The zeroth order regression calibration was linear from 0.866 to 35.800µgL(-1) CS, with a correlation coefficient of 0.99. At optimal experimental conditions, a limit of detection of 0.259µgL(-1) and a limit of quantification of 0.866µgL(-1) were obtained. The method showed good sensitivity and adequate selectivity and was applied to the determination of trace amounts of CS in plasma, serum and water samples with satisfactory results analyzed by ANOVA test. The proposed methodology represents an alternative to traditional chromatographic techniques for CS monitoring in complex samples, using an accessible instrument in control laboratories. Copyright © 2016 Elsevier B.V. All rights reserved.

Probabilistic dietary exposure assessment taking into account variability in both amount and frequency of consumption.

PubMed

Slob, Wout

2006-07-01

Probabilistic dietary exposure assessments that are fully based on Monte Carlo sampling from the raw intake data may not be appropriate. This paper shows that the data should first be analysed by using a statistical model that is able to take the various dimensions of food consumption patterns into account. A (parametric) model is discussed that takes into account the interindividual variation in (daily) consumption frequencies, as well as in amounts consumed. Further, the model can be used to include covariates, such as age, sex, or other individual attributes. Some illustrative examples show how this model may be used to estimate the probability of exceeding an (acute or chronic) exposure limit. These results are compared with the results based on directly counting the fraction of observed intakes exceeding the limit value. This comparison shows that the latter method is not adequate, in particular for the acute exposure situation. A two-step approach for probabilistic (acute) exposure assessment is proposed: first analyse the consumption data by a (parametric) statistical model as discussed in this paper, and then use Monte Carlo techniques for combining the variation in concentrations with the variation in consumption (by sampling from the statistical model). This approach results in an estimate of the fraction of the population as a function of the fraction of days at which the exposure limit is exceeded by the individual.

An atomic-absorption method for the determination of gold in large samples of geologic materials

USGS Publications Warehouse

VanSickle, Gordon H.; Lakin, Hubert William

1968-01-01

A laboratory method for the determination of gold in large (100-gram) samples has been developed for use in the study of the gold content of placer deposits and of trace amounts of gold in other geologic materials. In this method the sample is digested with bromine and ethyl ether, the gold is extracted into methyl isobutyl ketone, and the determination is made by atomicabsorption spectrophotometry. The lower limit of detection is 0.005 part per million in the sample. The few data obtained so far by this method agree favorably with those obtained by assay and by other atomic-absorption methods. About 25 determinations can be made per man-day.

Cancer classification through filtering progressive transductive support vector machine based on gene expression data

NASA Astrophysics Data System (ADS)

Lu, Xinguo; Chen, Dan

2017-08-01

Traditional supervised classifiers neglect a large amount of data which not have sufficient follow-up information, only work with labeled data. Consequently, the small sample size limits the advancement of design appropriate classifier. In this paper, a transductive learning method which combined with the filtering strategy in transductive framework and progressive labeling strategy is addressed. The progressive labeling strategy does not need to consider the distribution of labeled samples to evaluate the distribution of unlabeled samples, can effective solve the problem of evaluate the proportion of positive and negative samples in work set. Our experiment result demonstrate that the proposed technique have great potential in cancer prediction based on gene expression.

Using bio-dispersive solution of chitosan for green dispersive liquid-liquid microextraction of trace amounts of Cu(II) in edible oils prior to analysis by ICP-OES.

PubMed

Limchoowong, Nunticha; Sricharoen, Phitchan; Techawongstien, Suchila; Chanthai, Saksit

2017-09-01

A green approach using chitosan solution as a novel bio-dispersive agent for the dispersive liquid-liquid microextraction (DLLME) of trace amounts of Cu(II) in edible oils is presented. An emulsion was formed by mixing the oil sample with 300µL of 0.25% (w/v) chitosan solution containing 200µL of 6molL -1 HCl. Deionized water was used to induce emulsion breaking without centrifugation. The centrifuged Cu(II) extract was collected and analyzed using an inductively coupled plasma-optical emission spectrometer. The detection and quantitation limits were 2.1 and 6.8µgL -1 , respectively. Trace amounts of Cu(II) in six edible oil samples were tested under optimum conditions for DLLME, with a recovery ranging from 90.3% to 109.3%. Therefore, the new dispersive agent in DLLME offers superior performance owing to the non-toxic nature of the solvent, short extraction time, high sensitivity, and easy operation. Copyright © 2017 Elsevier Ltd. All rights reserved.

Physical education and academic achievement in elementary school: data from the early childhood longitudinal study.

PubMed

Carlson, Susan A; Fulton, Janet E; Lee, Sarah M; Maynard, L Michele; Brown, David R; Kohl, Harold W; Dietz, William H

2008-04-01

We examined the association between time spent in physical education and academic achievement in a longitudinal study of students in kindergarten through fifth grade. We used data from the Early Childhood Longitudinal Study, Kindergarten Class of 1998 to 1999, which employed a multistage probability design to select a nationally representative sample of students in kindergarten (analytic sample = 5316). Time spent in physical education (minutes per week) was collected from classroom teachers, and academic achievement (mathematics and reading) was scored on an item response theory scale. A small but significant benefit for academic achievement in mathematics and reading was observed for girls enrolled in higher amounts (70-300 minutes per week) of physical education (referent: 0-35 minutes per week). Higher amounts of physical education were not positively or negatively associated with academic achievement among boys. Among girls, higher amounts of physical education may be associated with an academic benefit. Physical education did not appear to negatively affect academic achievement in elementary school students. Concerns about adverse effects on achievement may not be legitimate reasons to limit physical education programs.

40 CFR 761.353 - Second level of sample selection.

Code of Federal Regulations, 2012 CFR

2012-07-01

... reduction is to limit the amount of time required to manually cut up larger particles of the waste to pass through a 9.5 millimeter (mm) screen. (a) Selecting a portion of the subsample for particle size reduction... table to select one of these quarters. (b) Reduction of the particle size by the use of a 9.5 mm screen...

40 CFR 761.353 - Second level of sample selection.

Code of Federal Regulations, 2014 CFR

2014-07-01

... reduction is to limit the amount of time required to manually cut up larger particles of the waste to pass through a 9.5 millimeter (mm) screen. (a) Selecting a portion of the subsample for particle size reduction... table to select one of these quarters. (b) Reduction of the particle size by the use of a 9.5 mm screen...

40 CFR 761.353 - Second level of sample selection.

Code of Federal Regulations, 2013 CFR

2013-07-01

... reduction is to limit the amount of time required to manually cut up larger particles of the waste to pass through a 9.5 millimeter (mm) screen. (a) Selecting a portion of the subsample for particle size reduction... table to select one of these quarters. (b) Reduction of the particle size by the use of a 9.5 mm screen...

Coarse woody debris assay in northern Arizona mixed-conifer and ponderosa pine forests

Treesearch

Joseph L. Ganey; Scott C. Vojta

2010-01-01

Coarse woody debris (CWD) provides important ecosystem services in forests and affects fire behavior, yet information on amounts and types of CWD typically is limited. To provide such information, we sampled logs and stumps in mixed-conifer and ponderosa pine (Pinus ponderosa) forests in north-central Arizona. Spatial variability was prominent for all CWD parameters....

Development of a testing method for asbestos fibers in treated materials of asbestos containing wastes by transmission electron microscopy

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

Yamamoto, Takashi, E-mail: tyama@nies.go.jp; Kida, Akiko; Noma, Yukio

Highlights: • A high sensitive and selective testing method for asbestos in treated materials of asbestos containing wastes was developed. • Asbestos can be determined at a limits are a few million fibers per gram and a few μg g{sup −1}. • High temperature melting treatment samples were determined by this method. Asbestos fiber concentration were below the quantitation limit in all samples, and total fiber concentrations were determined as 47–170 × 10{sup 6} g{sup −1}. - Abstract: Appropriate treatment of asbestos-containing wastes is a significant problem. In Japan, the inertization of asbestos-containing wastes based on new treatment processes approvedmore » by the Minister of the Environment is promoted. A highly sensitive method for testing asbestos fibers in inertized materials is required so that these processes can be approved. We developed a method in which fibers from milled treated materials are extracted in water by shaking, and are counted and identified by transmission electron microscopy. Evaluation of this method by using asbestos standards and simulated slag samples confirmed that the quantitation limits are a few million fibers per gram and a few μg/g in a sample of 50 mg per filter. We used this method to assay asbestos fibers in slag samples produced by high-temperature melting of asbestos-containing wastes. Fiber concentrations were below the quantitation limit in all samples, and total fiber concentrations were determined as 47–170 × 10{sup −6} f/g. Because the evaluation of treated materials by TEM is difficult owing to the limited amount of sample observable, this testing method should be used in conjunction with bulk analytical methods for sure evaluation of treated materials.« less

Fast identification of microplastics in complex environmental samples by a thermal degradation method.

PubMed

Dümichen, Erik; Eisentraut, Paul; Bannick, Claus Gerhard; Barthel, Anne-Kathrin; Senz, Rainer; Braun, Ulrike

2017-05-01

In order to determine the relevance of microplastic particles in various environmental media, comprehensive investigations are needed. However, no analytical method exists for fast identification and quantification. At present, optical spectroscopy methods like IR and RAMAN imaging are used. Due to their time consuming procedures and uncertain extrapolation, reliable monitoring is difficult. For analyzing polymers Py-GC-MS is a standard method. However, due to a limited sample amount of about 0.5 mg it is not suited for analysis of complex sample mixtures like environmental samples. Therefore, we developed a new thermoanalytical method as a first step for identifying microplastics in environmental samples. A sample amount of about 20 mg, which assures the homogeneity of the sample, is subjected to complete thermal decomposition. The specific degradation products of the respective polymer are adsorbed on a solid-phase adsorber and subsequently analyzed by thermal desorption gas chromatography mass spectrometry. For certain identification, the specific degradation products for the respective polymer were selected first. Afterwards real environmental samples from the aquatic (three different rivers) and the terrestrial (bio gas plant) systems were screened for microplastics. Mainly polypropylene (PP), polyethylene (PE) and polystyrene (PS) were identified for the samples from the bio gas plant and PE and PS from the rivers. However, this was only the first step and quantification measurements will follow. Copyright © 2017 Elsevier Ltd. All rights reserved.

Solid-phase extraction of iridium from soil and water samples by using activated carbon cloth prior to its spectrophotometric determination.

PubMed

Ozkantar, Nebiye; Yilmaz, Erkan; Soylak, Mustafa; Tuzen, Mustafa

2015-08-01

A solid-phase extraction method for separation and preconcentration of Ir(IV) ion by using activated carbon cloth (ACC) has been presented. Ir(IV) as their 1-(2-pyridylazo) 2-naphtol (PAN) chelate was adsorbed on ACC at pH 2.0 and was eluted from ACC with acidic dimethylformamide (DMF). The Ir(IV) concentration was determined at 536 nm as Ir(IV)-PAN complex by using UV-vis spectrophotometer. The analytical parameters including pH, sample and eluent flow rates, amount of PAN, eluent type, concentration, and sample volume were optimized. The effects of foreign ions on the recoveries of iridium were also investigated. The preconcentration factor was calculated as 60. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were found as 0.039 and 0.129 μg L(-1), respectively. The method was applied to soil and water samples for iridium determination.

NMR Confirmation and HPLC Quantification of Javamide-I and Javamide-II in Green Coffee Extract Products Available in the Market.

PubMed

Park, Jae B

2017-01-01

Javamide-I/javamide-II are phenolic amides found in coffee. Recent reports suggested that they may contain several biological activities related to human health. Therefore, there is emergent interest about their quantities in coffee-related products. Green coffee extract is a powder extract made of unroasted green coffee beans, available as a dietary supplement. However, there is little information about the amounts of javamide-I/javamide-II in green coffee extract products in the market. Therefore, in this paper, javamide-I/javamide-II were extracted from green coffee extract products and their identifications were confirmed by NMR. After that, the amounts of javamide-I/javamide-II were individually quantified from seven different green coffee extract samples using the HPLC method coupled to an electrochemical detector. The HPLC method provided accurate and reliable measurement of javamide-I/javamide-II with excellent peak resolution and low detection limit. In all seven green coffee extract samples, javamide-II was found to be between 0.28 and 2.96 mg/g, but javamide-I was detected in only five samples in the concentration levels of 0.15-0.52 mg/g, suggesting that green coffee extract products contain different amounts of javamide-I/javamide-II. In summary, javamide-I/javamide-II can be found in green coffee extract products sold in the market, but their amounts are likely to be comparatively different in between green coffee extract brands.

Development of a magnetic solid-phase extraction coupled with high-performance liquid chromatography method for the analysis of polyaromatic hydrocarbons.

PubMed

Ma, Yan; Xie, Jiawen; Jin, Jing; Wang, Wei; Yao, Zhijian; Zhou, Qing; Li, Aimin; Liang, Ying

2015-07-01

A novel magnetic solid phase extraction coupled with high-performance liquid chromatography method was established to analyze polyaromatic hydrocarbons in environmental water samples. The extraction conditions, including the amount of extraction agent, extraction time, pH and the surface structure of the magnetic extraction agent, were optimized. The results showed that the amount of extraction agent and extraction time significantly influenced the extraction performance. The increase in the specific surface area, the enlargement of pore size, and the reduction of particle size could enhance the extraction performance of the magnetic microsphere. The optimized magnetic extraction agent possessed a high surface area of 1311 m(2) /g, a large pore size of 6-9 nm, and a small particle size of 6-9 μm. The limit of detection for phenanthrene and benzo[g,h,i]perylene in the developed analysis method was 3.2 and 10.5 ng/L, respectively. When applied to river water samples, the spiked recovery of phenanthrene and benzo[g,h,i]perylene ranged from 89.5-98.6% and 82.9-89.1%, respectively. Phenanthrene was detected over a concentration range of 89-117 ng/L in three water samples withdrawn from the midstream of the Huai River, and benzo[g,h,i]perylene was below the detection limit. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of alkaloids in onion nectar by micellar electrokinetic chromatography.

PubMed

Carolina Soto, Verónica; Jofré, Viviana Patricia; Galmarini, Claudio Romulo; Silva, María Fernanda

2016-07-01

Nectar is the most important floral reward offered by plants to insects. Minor components such as alkaloid compounds in nectar affect bee foraging, with great influence in seed production. CE is an advantageous tool for the analysis of unexplored samples such as onion nectar due to the limited amounts of samples. Considering the importance of these compounds, a simultaneous determination of nicotine, theophylline, theobromine, caffeine, harmaline, piperine in onion nectar by MEKC-UV is herein reported. The extraction of alkaloid compounds in nectar was performed by SPE using a homemade miniaturized column (C18 ). Effects of several important factors affecting extraction efficiency as well as electrophoretic performance were investigated to acquire optimum conditions. Under the proposed conditions, the analytes can be separated within 15 min in a 50 cm effective length capillary (75 μm id) at a separation voltage of 20 kV in 20 mmol/L sodium tretraborate, 100 mmol/L SDS. The amount of sample requirement was reduced up to 2000 times, when compared to traditional methods, reaching limits of detection as low as 0.0153 ng/L. For the first time, this study demonstrates that there are marked qualitative and quantitative differences in nectar alkaloids between open pollinated and male sterile lines (MSLs) and also within MSLs. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Polycyclic Aromatic Hydrocarbons in Electrocautery Smoke during Peritonectomy Procedures

PubMed Central

Näslund Andréasson, Sara; Mahteme, Haile; Sahlberg, Bo; Anundi, Helena

2012-01-01

Objective. This study identified and quantified polycyclic aromatic hydrocarbons (PAHs) in electrocautery smoke during 40 peritonectomy procedures and investigated any correlations and/or differences between levels of PAHs and perioperative variables. Methods. PAHs were measured in personal and stationary sampling by 40 mm Millipore cassettes, for adsorption of both gaseous and particle-bound PAHs. Results. All 16 USEPA priority pollutant PAHs were detected during peritonectomy procedures, naphthalene being the most abundant. For the only two PAHs with Swedish occupational exposure limits (OELs), benzo[a]pyrene and naphthalene, limits were never exceeded. Amount of bleeding was the only perioperative variable that correlated with levels of PAHs. Conclusions. Low levels of PAHs were detected in electrocautery smoke during peritonectomy procedures, and an increased amount of bleeding correlated with higher levels of PAHs. For evaluation of long-term health effects, more studies are needed. PMID:22685482

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.

Targeted Analyte Detection by Standard Addition Improves Detection Limits in MALDI Mass Spectrometry

PubMed Central

Eshghi, Shadi Toghi; Li, Xingde; Zhang, Hui

2014-01-01

Matrix-assisted laser desorption/ionization has proven an effective tool for fast and accurate determination of many molecules. However, the detector sensitivity and chemical noise compromise the detection of many invaluable low-abundance molecules from biological and clinical samples. To challenge this limitation, we developed a targeted analyte detection (TAD) technique. In TAD, the target analyte is selectively elevated by spiking a known amount of that analyte into the sample, thereby raising its concentration above the noise level, where we take advantage of the improved sensitivity to detect the presence of the endogenous analyte in the sample. We assessed TAD on three peptides in simple and complex background solutions with various exogenous analyte concentrations in two MALDI matrices. TAD successfully improved the limit of detection (LOD) of target analytes when the target peptides were added to the sample in a concentration close to optimum concentration. The optimum exogenous concentration was estimated through a quantitative method to be approximately equal to the original LOD for each target. Also, we showed that TAD could achieve LOD improvements on an average of 3-fold in a simple and 2-fold in a complex sample. TAD provides a straightforward assay to improve the LOD of generic target analytes without the need for costly hardware modifications. PMID:22877355

Targeted analyte detection by standard addition improves detection limits in matrix-assisted laser desorption/ionization mass spectrometry.

PubMed

Toghi Eshghi, Shadi; Li, Xingde; Zhang, Hui

2012-09-18

Matrix-assisted laser desorption/ionization (MALDI) has proven an effective tool for fast and accurate determination of many molecules. However, the detector sensitivity and chemical noise compromise the detection of many invaluable low-abundance molecules from biological and clinical samples. To challenge this limitation, we developed a targeted analyte detection (TAD) technique. In TAD, the target analyte is selectively elevated by spiking a known amount of that analyte into the sample, thereby raising its concentration above the noise level, where we take advantage of the improved sensitivity to detect the presence of the endogenous analyte in the sample. We assessed TAD on three peptides in simple and complex background solutions with various exogenous analyte concentrations in two MALDI matrices. TAD successfully improved the limit of detection (LOD) of target analytes when the target peptides were added to the sample in a concentration close to optimum concentration. The optimum exogenous concentration was estimated through a quantitative method to be approximately equal to the original LOD for each target. Also, we showed that TAD could achieve LOD improvements on an average of 3-fold in a simple and 2-fold in a complex sample. TAD provides a straightforward assay to improve the LOD of generic target analytes without the need for costly hardware modifications.

Solid phase extraction of trace amounts of cadmium(II) ions in water and food samples using iron magnetite nanoparticles modified by sodium dodecyl sulfate and 2-mercaptobenzothiazole.

PubMed

Abbasi, Shahriar; ShanbehDehbalai, Mehdi; Khani, Hossein

2017-03-01

A new, simple and rapid method for solid phase extraction and preconcentration of trace amounts of cadmium ions using 2-mercaptobenzothiazole/sodium dodecyl sulfate immobilized on magnetite nanoparticles (MBT-SDS-MNPs) was proposed. The method is based on the extraction of cadmium ions via complexation with MBT immobilized on SDS-coated MNPs and their determination by flame atomic absorption spectrometry. The effects of different parameters - pH; eluent type, concentration and volume; amounts of salt and adsorbent; contact time and interfering ions - on the adsorption of cadmium ions were studied. Under optimized conditions, the calibration curve was linear in the range of 10-5,000 μg L -1 . Detection limit and relative standard deviation of the proposed method were 0.009 μg L -1 and 2.2%, respectively. The adsorption data were analyzed by Langmuir and Freundlich isotherm models and a maximum adsorption amount of 24.80 mg g -1 , a Langmuir adsorption equilibrium constant (b) of 4.62 and Freundlich constants K f and n of 6.075 mg 1-1/n L 1/n g -1 and 2.391, respectively, were obtained. Finally, this adsorbent was successfully used for extraction of cadmium from water and food samples.

The Health Risk of Cd Released from Low-Cost Jewelry.

PubMed

Pouzar, Miloslav; Zvolská, Magdalena; Jarolím, Oldřich; Audrlická Vavrušová, Lenka

2017-05-12

The composition of the surface layer of 13 low-cost jewelry samples with a high Cd content was analyzed using an energy-dispersive X-ray fluorescence spectrometer (ED XRF). The analyzed jewels were obtained in cooperation with the Czech Environmental Inspectorate. The jewels were leached in two types of artificial sweat (acidic and alkaline) for 7 days. Twenty microliters of the resulting solution was subsequently placed on a paper carrier and analyzed by an LIBS (Laser-Induced Breakdown Spectrometry) spectrometer after drying. The Cd content in the jewelry surface layer detected by using ED XRF ranged from 13.4% to 44.6% (weight per weight-w/w). The samples were subsequently leached in artificial alkaline, and the acidic sweat and leachates were analyzed using laser-induced breakdown spectrometry (LIBS). The amount of released Cd into alkaline sweat ranged from 24.0 to 370 µg Cd per week, respectively 3.23-61.7 µg/cm²/week. The amount of released Cd into acidic sweat ranged from 16.4 to 1517 µg Cd per week, respectively 3.53-253 µg/cm²/week. The limit of Cd for dermal exposure is not unequivocally determined in the countries of the EU (European Union) or in the U.S. Based on the US EPA (United States Environmental Protection Agency) approach used to establish the reference dose (RfD) for Cd contained in food and information about the bioavailability of Cd after dermal exposure, we assessed our own value of dermal RfD. The value was compared with the theoretical amount of Cd, which can be absorbed into the organism from jewelry in contact with the skin. The calculation was based on the amount of Cd that was released into acidic and alkaline sweat. The highest amount of Cd was released into acidic sweat, which represents 0.1% of dermal RfD and into alkaline sweat, 0.5% of dermal RfD. These results indicate that the analyzed jewelry contains Cd over the limit for composition of jewelry available within the territory of the EU. The determined amount of Cd in analyzed jewelry does not, however, pose a threat in terms of carcinogenic toxic effects.

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.

Validated method for quantification of genetically modified organisms in samples of maize flour.

PubMed

Kunert, Renate; Gach, Johannes S; Vorauer-Uhl, Karola; Engel, Edwin; Katinger, Hermann

2006-02-08

Sensitive and accurate testing for trace amounts of biotechnology-derived DNA from plant material is the prerequisite for detection of 1% or 0.5% genetically modified ingredients in food products or raw materials thereof. Compared to ELISA detection of expressed proteins, real-time PCR (RT-PCR) amplification has easier sample preparation and detection limits are lower. Of the different methods of DNA preparation CTAB method with high flexibility in starting material and generation of sufficient DNA with relevant quality was chosen. Previous RT-PCR data generated with the SYBR green detection method showed that the method is highly sensitive to sample matrices and genomic DNA content influencing the interpretation of results. Therefore, this paper describes a real-time DNA quantification based on the TaqMan probe method, indicating high accuracy and sensitivity with detection limits of lower than 18 copies per sample applicable and comparable to highly purified plasmid standards as well as complex matrices of genomic DNA samples. The results were evaluated with ValiData for homology of variance, linearity, accuracy of the standard curve, and standard deviation.

Physicochemical characteristics and pollen spectra of organic and non-organic honey samples of Apis mellifera L.

PubMed

Sereia, Maria Josiane; Alves, Eloi M; Toledo, Vagner A A; Marchini, Luis C; Serine, Elizabete S; Faquinello, Patricia; Almeida, Daniela de; Moreti, Augusta C C C

2011-09-01

The aim of this research was to analyze and compare 17 honey samples, 11 organic and six non-organic Apis mellifera honey. The samples were analyzed concerning moisture, hydroxymethylfurfural, diastase index, water activity, color, total sugar, reducing sugar, sucrose, ash, viscosity, electrical conductivity, pH, acidity, and formol index. With the exception of acidity, reducing sugar and diastase index, the averages of other parameters were different between the two groups. All samples of organic honey presented moisture values between 23.50 and 24.40%. Among the nonorganic honey samples, two presented apparent sucrose amount upper the maximum limit established by the Brazilian Legislation. According to the quantitative analysis of pollen sediments in the honey samples and frequency of pollen types in 17 honey samples, 41.20% were classified as unifioral, and the remainder as polifioral.

A novel task specific magnetic polymeric ionic liquid for selective preconcentration of potassium in oil samples using centrifuge-less dispersive liquid-liquid microextraction technique and its determination by flame atomic emission spectroscopy.

PubMed

Beiraghi, Asadollah; Shokri, Masood

2018-02-01

In the present study a new centrifuge-less dispersive liquid-liquid microextraction technique based on application of a new task specific magnetic polymeric ionic liquid (TSMPIL) as a chelating and extraction solvent for selective preconcentration of trace amounts of potassium from oil samples is developed, for the first time. After extraction, the fine droplets of TSMPIL were transferred into an eppendorf tube and diluted to 500µL using distilled water. Then, the enriched analyte was determined by flame atomic emission spectroscopy (FAES). Several important factors affecting both the complexation and extraction efficiency including extraction time, rate of vortex agitator, amount of carbonyl iron powder, pH of sample solution, volume of ionic liquid as well as effects of interfering species were investigated and optimized. Under the optimal conditions, the limits of detection (LOD) and quantification (LOQ) were 0.5 and 1.6µgL -1 respectively with the preconcentration factor of 128. The precision (RSD %) for seven replicate determinations at 10µgL -1 of potassium was better than 3.9%. The relative recoveries for the spiked samples were in the acceptable range of 95-104%. The results demonstrated that no remarkable interferences are created by other various ions in the determination of potassium, so that the tolerance limits (W Ion /W K ) of major cations and anions were in the range of 2500-10,000. The purposed method was successfully applied for the analysis of potassium in some oil samples. Copyright © 2017 Elsevier B.V. All rights reserved.

A simple quantitative diagnostic alternative for MGMT DNA-methylation testing on RCL2 fixed paraffin embedded tumors using restriction coupled qPCR.

PubMed

Pulverer, Walter; Hofner, Manuela; Preusser, Matthias; Dirnberger, Elisabeth; Hainfellner, Johannes A; Weinhaeusel, Andreas

2014-01-01

MGMT promoter methylation is associated with favorable prognosis and chemosensitivity in glioblastoma multiforme (GBM), especially in elderly patients. We aimed to develop a simple methylation-sensitive restriction enzyme (MSRE)-based quantitative PCR (qPCR) assay, allowing the quantification of MGMT promoter methylation. DNA was extracted from non-neoplastic brain (n = 24) and GBM samples (n = 20) upon 3 different sample conservation conditions (-80 °C, formalin-fixed and paraffin-embedded (FFPE); RCL2-fixed). We evaluated the suitability of each fixation method with respect to the MSRE-coupled qPCR methylation analyses. Methylation data were validated by MALDITOF. qPCR was used for evaluation of alternative tissue conservation procedures. DNA from FFPE tissue failed reliable testing; DNA from both RCL2-fixed and fresh frozen tissues performed equally well and was further used for validation of the quantitative MGMT methylation assay (limit of detection (LOD): 19.58 pg), using individual's undigested sample DNA for calibration. MGMT methylation analysis in non-neoplastic brain identified a background methylation of 0.10 ± 11% which we used for defining a cut-off of 0.32% for patient stratification. Of GBM patients 9 were MGMT methylationpositive (range: 0.56 - 91.95%), and 11 tested negative. MALDI-TOF measurements resulted in a concordant classification of 94% of GBM samples in comparison to qPCR. The presented methodology allows quantitative MGMT promoter methylation analyses. An amount of 200 ng DNA is sufficient for triplicate analyses including control reactions and individual calibration curves, thus excluding any DNA qualityderived bias. The combination of RCL2-fixation and quantitative methylation analyses improves pathological routine examination when histological and molecular analyses on limited amounts of tumor samples are necessary for patient stratification.

Sensitive, accurate and rapid detection of trace aliphatic amines in environmental samples with ultrasonic-assisted derivatization microextraction using a new fluorescent reagent for high performance liquid chromatography.

PubMed

Chen, Guang; Liu, Jianjun; Liu, Mengge; Li, Guoliang; Sun, Zhiwei; Zhang, Shijuan; Song, Cuihua; Wang, Hua; Suo, Yourui; You, Jinmao

2014-07-25

A new fluorescent reagent, 1-(1H-imidazol-1-yl)-2-(2-phenyl-1H-phenanthro[9,10-d]imidazol-1-yl)ethanone (IPPIE), is synthesized, and a simple pretreatment based on ultrasonic-assisted derivatization microextraction (UDME) with IPPIE is proposed for the selective derivatization of 12 aliphatic amines (C1: methylamine-C12: dodecylamine) in complex matrix samples (irrigation water, river water, waste water, cultivated soil, riverbank soil and riverbed soil). Under the optimal experimental conditions (solvent: ACN-HCl, catalyst: none, molar ratio: 4.3, time: 8 min and temperature: 80°C), micro amount of sample (40 μL; 5mg) can be pretreated in only 10 min, with no preconcentration, evaporation or other additional manual operations required. The interfering substances (aromatic amines, aliphatic alcohols and phenols) get the derivatization yields of <5%, causing insignificant matrix effects (<4%). IPPIE-analyte derivatives are separated by high performance liquid chromatography (HPLC) and quantified by fluorescence detection (FD). The very low instrumental detection limits (IDL: 0.66-4.02 ng/L) and method detection limits (MDL: 0.04-0.33 ng/g; 5.96-45.61 ng/L) are achieved. Analytes are further identified from adjacent peaks by on-line ion trap mass spectrometry (MS), thereby avoiding additional operations for impurities. With this UDME-HPLC-FD-MS method, the accuracy (-0.73-2.12%), precision (intra-day: 0.87-3.39%; inter-day: 0.16-4.12%), recovery (97.01-104.10%) and sensitivity were significantly improved. Successful applications in environmental samples demonstrate the superiority of this method in the sensitive, accurate and rapid determination of trace aliphatic amines in micro amount of complex samples. Copyright © 2014 Elsevier B.V. All rights reserved.

31 CFR 353.10 - Amounts which may be purchased.

Code of Federal Regulations, 2010 CFR

2010-07-01

... UNITED STATES SAVINGS BONDS, SERIES EE AND HH Limitations on Annual Purchases § 353.10 Amounts which may be purchased. The amount of savings bonds of Series EE and HH which may be purchased and held, in the... and is limited as follows: (a) Series EE—(1) General annual limitation. $5,000 (principal amount). (2...

31 CFR 353.10 - Amounts which may be purchased.

Code of Federal Regulations, 2011 CFR

2011-07-01

... STATES SAVINGS BONDS, SERIES EE AND HH Limitations on Annual Purchases § 353.10 Amounts which may be purchased. The amount of savings bonds of Series EE and HH which may be purchased and held, in the name of... limited as follows: (a) Series EE—(1) General annual limitation. $5,000 (principal amount). (2) Special...

31 CFR 353.10 - Amounts which may be purchased.

Code of Federal Regulations, 2013 CFR

2013-07-01

... STATES SAVINGS BONDS, SERIES EE AND HH Limitations on Annual Purchases § 353.10 Amounts which may be purchased. The amount of savings bonds of Series EE and HH which may be purchased and held, in the name of... limited as follows: (a) Series EE—(1) General annual limitation. $5,000 (principal amount). (2) Special...

31 CFR 353.10 - Amounts which may be purchased.

Code of Federal Regulations, 2014 CFR

2014-07-01

... UNITED STATES SAVINGS BONDS, SERIES EE AND HH Limitations on Annual Purchases § 353.10 Amounts which may be purchased. The amount of savings bonds of Series EE and HH which may be purchased and held, in the... and is limited as follows: (a) Series EE—(1) General annual limitation. $5,000 (principal amount). (2...

31 CFR 353.10 - Amounts which may be purchased.

Code of Federal Regulations, 2012 CFR

2012-07-01

... STATES SAVINGS BONDS, SERIES EE AND HH Limitations on Annual Purchases § 353.10 Amounts which may be purchased. The amount of savings bonds of Series EE and HH which may be purchased and held, in the name of... limited as follows: (a) Series EE—(1) General annual limitation. $5,000 (principal amount). (2) Special...

Long-term drought sensitivity of trees in second-growth forests in a humid region

Treesearch

Neil Pederson; Kacie Tackett; Ryan W. McEwan; Stacy Clark; Adrienne Cooper; Glade Brosi; Ray Eaton; R. Drew Stockwell

2012-01-01

Classical field methods of reconstructing drought using tree rings in humid, temperate regions typically target old trees from drought-prone sites. This approach limits investigators to a handful of species and excludes large amounts of data that might be useful, especially for coverage gaps in large-scale networks. By sampling in more “typical” forests, network...

Application of cotton as a solid phase extraction sorbent for on-line preconcentration of copper in water samples prior to inductively coupled plasma optical emission spectrometry determination.

PubMed

Faraji, Mohammad; Yamini, Yadollah; Shariati, Shahab

2009-07-30

Copper, as a heavy metal, is toxic for many biological systems. Thus, the determination of trace amounts of copper in environmental samples is of great importance. In the present work, a new method was developed for the determination of trace amounts of copper in water samples. The method is based on the formation of ternary Cu(II)-CAS-CTAB ion-pair and adsorption of it into a mini-column packed with cotton prior applying inductively coupled plasma optical emission spectrometry (ICP-OES). The experimental parameters that affected the extraction efficiency of the method such as pH, flow rate and volume of the sample solution, concentration of chromazurol S (CAS) and cethyltrimethylammonium bromide (CTAB) as well as type and concentration of eluent were investigated and optimized. The ion-pair (Cu(II)-CAS-CTAB) was quantitatively retained on the cotton under the optimum conditions, then eluted completely using a solution of 25% (v/v) 1-propanol in 0.5 mol L(-1) HNO(3) and directly introduced into the nebulizer of the ICP-OES. The detection limit (DL) of the method for copper was 40 ng L(-1) (V(sample)=100mL) and the relative standard deviation (R.S.D.) for the determination of copper at 10 microg L(-1) level was found to be 1.3%. The method was successfully applied to determine the trace amounts of copper in tap water, deep well water, seawater and two different mineral waters, and suitable recoveries were obtained (92-106%).

Combination of solid phase extraction and dispersive liquid-liquid microextraction for separation/preconcentration of ultra trace amounts of uranium prior to its fiber optic-linear array spectrophotometry determination.

PubMed

Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji; Shakerian, Farid; Shiralian Esfahani, Golnaz

2013-12-15

A simple and sensitive method for the separation and preconcentration of the ultra trace amounts of uranium and its determination by spectrophotometry was developed. The method is based on the combination of solid phase extraction and dispersive liquid-liquid microextraction. Thus, by passing the sample through the basic alumina column, the uranyl ion and some cations are separated from the sample matrix. The retained uranyl ion along with the cations are eluted with 5 mL of nitric acid (2 mol L(-1)) and after neutralization of the eluent, the extracted uranyl ion is converted to its anionic benzoate complex and is separated from other cations by extraction of its ion pair with malachite green into small volume of chloroform using dispersive liquid-liquid microextraction. The amount of uranium is then determined by the absorption measurement of the extracted ion pair at 621 nm using flow injection spectrophotometry. Under the optimum conditions, with 500 mL of the sample, a preconcentration factor of 1980, a detection limit of 40 ng L(-1), and a relative standard deviation of 4.1% (n=6) at 400 ng L(-1) were obtained. The method was successfully applied to the determination of uranium in mineral water, river water, well water, spring water and sea water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Determination of fluorine in herbs and water samples by molecular absorption spectrometry after preconcentration on nano-TiO2 using ultrasound-assisted dispersive micro solid phase extraction.

PubMed

Krawczyk-Coda, Magdalena; Stanisz, Ewa

2017-11-01

This work presents ultrasound-assisted dispersive micro solid phase extraction (USA DMSPE) for preconcentration of fluorine (F) in water and herb samples. TiO 2 nanoparticles (NPs) were used as an adsorbent. The determination with slurry sampling was performed via molecular absorption of calcium monofluoride (CaF) at 606.440 nm using a high-resolution continuum source electrothermal absorption spectrometry (HR-CS ET MAS). Several factors influencing the efficiency of the preconcentration technique, such as the amount of TiO 2 , pH of sample solution, ultrasonication and centrifugation time and TiO 2 slurry solution preparation before injection to HR-CS ET MAS, were investigated in detail. The conditions of detection step (wavelength, calcium amount, pyrolysis and molecule-forming temperatures) were also studied. After extraction, adsorbent with the analyte was mixed with 200 μL of H 2 O to prepare a slurry solution. The concentration limit of detection was 0.13 ng mL -1 . The achieved preconcentration factor was 7. The relative standard deviations (RSDs, %) for F in real samples were 3-15%. The accuracy of this method was evaluated by analyses of certified reference materials after spiking: INCT-MPH-2 (Mixed Polish Herbs), INCT-SBF-4 (Soya Bean Flour), ERM-CAO11b (Hard Drinking Water) and TMDA-54.5 (Lake Ontario Water). The measured F contents in reference materials were in satisfactory agreement with the added amounts, and the recoveries were found to be 97-109%. Under the developed extraction conditions, the proposed method has been successfully applied for the determination of F in real water samples (lake, sea, tap water) and herbs.

Digital second-order phase-locked loop

NASA Technical Reports Server (NTRS)

Holes, J. K.; Carl, C.; Tegnelia, C. R. (Inventor)

1973-01-01

A digital second-order phase-locked loop is disclosed in which a counter driven by a stable clock pulse source is used to generate a reference waveform of the same frequency as an incoming waveform, and to sample the incoming waveform at zero-crossover points. The samples are converted to digital form and accumulated over M cycles, reversing the sign of every second sample. After every M cycles, the accumulated value of samples is hard limited to a value SGN = + or - 1 and multiplied by a value delta sub 1 equal to a number of n sub 1 of fractions of a cycle. An error signal is used to advance or retard the counter according to the sign of the sum by an amount equal to the sum.

Quantification of organic solvents in aquatic toys and swimming learning devices and evaluation of their influence on the smell properties of the corresponding products.

PubMed

Wiedmer, Christoph; Buettner, Andrea

2018-04-01

Based on the observation that the characteristic odour of inflatable aquatic toys for children is predominantly caused by residues of hazardous organic solvents, the concentrations of cyclohexanone, isophorone and phenol were determined in a selection of 20 products obtained from online suppliers located in Germany. Analytes were extracted with dichloromethane after the addition of non-labelled internal standards, and the volatile fraction was isolated using solvent-assisted flavour evaporation (SAFE). Extracts were then concentrated by Vigreux distillation and analysed by means of gas chromatography with mass spectrometric detection (GC-MS). Furthermore, each sample was evaluated regarding its specific olfactory properties by an expert sensory panel. While some samples did not contain significant amounts of solvents, cyclohexanone concentrations above the lower limit of quantification (LLOQ) were determined in nine samples with six samples containing high concentrations ranging from about 1 to 7 g/kg cyclohexanone. Isophorone concentrations above the LLOQ were observed in eight samples. Thereby, six products contained between 0.3 and 1.6 g/kg isophorone and the remaining two samples contained even about 5 g/kg isophorone, each. Likewise, phenol concentrations exceeded the LLOQ in 14 cases, with four samples containing elevated amounts ranging from about 140 to 280 mg/kg phenol.

Potentially harmful elements released by volcanic ashes: Examples from the Mediterranean area

NASA Astrophysics Data System (ADS)

Cangemi, Marianna; Speziale, Sergio; Madonia, Paolo; D'Alessandro, Walter; Andronico, Daniele; Bellomo, Sergio; Brusca, Lorenzo; Kyriakopoulos, Konstantinos

2017-05-01

We have performed leaching experiments on the fine (< 2 mm) particulate sampled in seven active and quiescent volcanic systems in the Mediterranean area. We reacted the particulate both in pure water and in a synthetic gastric solution. The amount of As, Mn, Pb, Ba, U and Ni leached by pure water exceeded the MAC limits for drinking water in all the materials under investigation. We defined a tolerable ash intake index (TAI) to evaluate the impact of ash ingestion, and we find that 0.2 g and 12 g of ingested fine ash from Vesuvius and Vulcano are enough to exceed the safety limits for Pb and As. Six grams of fine ashes from Stromboli are sufficient to overstep the safety limits for As. Based on our mineralogical characterisation of the particulate, we expect that the submillimetric ash fraction, with a higher surface/volume ratio, releases a greater relative amount of trace metals, which are concentrated in the thin surface layer produced by the reaction of the pristine volcanic particles with coexisting volcanic gases. This means that our measurements represent lower bounds to the actual amount of metal released in aqueous solutions by the volcanic ashes from the locations under investigation. Our results place the first constraints on the mobilisation of toxic elements from volcanic ash, which are necessary to assess the associated potential health risk of volcanic areas.

Correlations of Apparent Cellulose Crystallinity Determined by XRD, NMR, IR, Raman, and SFG Methods

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

Johnson, David K; Lee, Christopher; Dazen, Kevin

2015-07-04

Although the cellulose crystallinity index (CI) is used widely, its limitations have not been adequately described. In this study, the CI values of a set of reference samples were determined from X-ray diffraction (XRD), nuclear magnetic resonance (NMR), and infrared (IR), Raman, and vibrational sum frequency generation (SFG) spectroscopies. The intensities of certain crystalline peaks in IR, Raman, and SFG spectra positively correlated with the amount of crystalline cellulose in the sample, but the correlation with XRD was nonlinear as a result of fundamental differences in detection sensitivity to crystalline cellulose and improper baseline corrections for amorphous contributions. It ismore » demonstrated that the intensity and shape of the XRD signal is affected by both the amount of crystalline cellulose and crystal size, which makes XRD analysis complicated. It is clear that the methods investigated show the same qualitative trends for samples, but the absolute CI values differ depending on the determination method. This clearly indicates that the CI, as estimated by different methods, is not an absolute value and that for a given set of samples the CI values can be compared only as a qualitative measure.« less

Correlations of Apparent Cellulose Crystallinity Determined by XRD, NMR, IR, Raman, and SFG Methods

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

Lee, Christopher M; Dazen, Kevin; Kafle, Kabindra

2015-01-01

Although the cellulose crystallinity index (CI) is used widely, its limitations have not been adequately described. In this study, the CI values of a set of reference samples were determined from X-ray diffraction (XRD), nuclear magnetic resonance (NMR), and infrared (IR), Raman, and vibrational sum frequency generation (SFG) spectroscopies. The intensities of certain crystalline peaks in IR, Raman, and SFG spectra positively correlated with the amount of crystalline cellulose in the sample, but the correlation with XRD was nonlinear as a result of fundamental differences in detection sensitivity to crystalline cellulose and improper baseline corrections for amorphous contributions. It ismore » demonstrated that the intensity and shape of the XRD signal is affected by both the amount of crystalline cellulose and crystal size, which makes XRD analysis complicated. It is clear that the methods investigated show the same qualitative trends for samples, but the absolute CI values differ depending on the determination method. This clearly indicates that the CI, as estimated by different methods, is not an absolute value and that for a given set of samples the CI values can be compared only as a qualitative measure.« less

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

PubMed

Mehdinia, Ali; Khodaee, Nader; Jabbari, Ali

2015-04-08

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

[Analysis of preservatives used in cosmetic products: salicylic acid, sodium benzoate, sodium dehydroacetate, potassium sorbate, phenoxyethanol, and parabens].

PubMed

Ikarashi, Yoshiaki; Uchino, Tadashi; Nishimura, Tetsuji

2010-01-01

Preservatives are used to inhibit the growth of microorganisms in cosmetic products. The Japanese standards for cosmetics set restrictions on the maximum amount of each preservative added to cosmetics as per the purpose of use of cosmetics. For the investigation into the actual conditions of commonly used preservatives in commercial cosmetics, we analyzed parabens, phenoxyethanol, sodium benzoate, sodium dehydroacetate, salicylic acid, and potassium sorbate by high-performance liquid chromatography (HPLC). Twenty-one samples were obtained from cosmetic product manufacturers located in 14 prefectures in Japan. Among different acid- and salt-based preservatives, sodium benzoate was observed to have been used in many products. These acid- and salt-based preservatives were used with parabens in personal washing products, such as shampoo and soap. The labels of two of the cosmetic product samples displayed inaccurate ingredient information, that is, a preservative other than the one used in the corresponding product was listed on them. The amount of preservatives used did not exceed regulatory limits in any of the analyzed samples.

Rapid quantification and sex determination of forensic evidence materials.

PubMed

Andréasson, Hanna; Allen, Marie

2003-11-01

DNA quantification of forensic evidence is very valuable for an optimal use of the available biological material. Moreover, sex determination is of great importance as additional information in criminal investigations as well as in identification of missing persons, no suspect cases, and ancient DNA studies. While routine forensic DNA analysis based on short tandem repeat markers includes a marker for sex determination, analysis of samples containing scarce amounts of DNA is often based on mitochondrial DNA, and sex determination is not performed. In order to allow quantification and simultaneous sex determination on minute amounts of DNA, an assay based on real-time PCR analysis of a marker within the human amelogenin gene has been developed. The sex determination is based on melting curve analysis, while an externally standardized kinetic analysis allows quantification of the nuclear DNA copy number in the sample. This real-time DNA quantification assay has proven to be highly sensitive, enabling quantification of single DNA copies. Although certain limitations were apparent, the system is a rapid, cost-effective, and flexible assay for analysis of forensic casework samples.

Electronic nicotine delivery systems: regulatory and safety challenges: Singapore perspective.

PubMed

Cheah, Nuan Ping; Chong, Norman Wee Lin; Tan, Jing; Morsed, Faridatul Akmam; Yee, Shen Kuan

2014-03-01

Many electronic nicotine delivery systems (ENDS) are marketed as safer tobacco alternative products or effective cessation therapies. ENDS samples were evaluated for design features, including nicotine and glycols content. This could be useful in developing a legal framework to handle ENDS. Identification of the nicotine, glycerol and propylene glycol (PPG) contents was conducted using gas chromatography mass spectrometry with quantification performed using flame ionisation techniques. Varying nicotine amounts were found in ENDS cartridges which were labelled with the same concentration. Chemicals such as PPG and glycerol were found to be present in the nicotine-containing liquid of the cartridges. ENDS varied in their contents and packaging information. Limited information was available on the contents of nicotine and other chemicals present in a variety of ENDS sampled. Based on samples tested in this study, many contain misleading information on product ingredients. The results show poor consistency between actual nicotine content analysed on ENDS cartridges and the amount labelled. These findings raise safety and efficacy concerns for current and would-be recreational users or those trying to quit smoking.

Gold in natural water: A method of determination by solvent extraction and electrothermal atomization

USGS Publications Warehouse

McHugh, J.B.

1984-01-01

A method has been developed using electrothermal atomization to effectively determine the amount of gold in natural water within the nanogram range. The method has four basic steps: (1) evaporating a 1-L sample; (2) putting it in hydrobromic acid-bromine solution; (3) extracting the sample with methyl-isobutyl-ketone; and (4) determining the amount of gold using an atomic absorption spectrophotometer. The limit of detection is 0.001 ??g gold per liter. Results from three studies indicate, respectively, that the method is precise, effective, and free of interference. Specifically, a precision study indicates that the method has a relative standard deviation of 16-18%; a recovery study indicates that the method recovers gold at an average of 93%; and an interference study indicates that the interference effects are eliminated with solvent extraction and background correction techniques. Application of the method to water samples collected from 41 sites throughout the Western United States and Alaska shows a gold concentration range of < 0.001 to 0.036 ??g gold per liter, with an average of 0.005 ??g/L. ?? 1984.

Enhanced DNA Profiling of the Semen Donor in Late Reported Sexual Assaults: Use of Y-Chromosome-Targeted Pre-amplification and Next Generation Y-STR Amplification Systems.

PubMed

Hanson, Erin K; Ballantyne, Jack

2016-01-01

In some cases of sexual assault the victim may not report the assault for several days after the incident due to various factors. The ability to obtain an autosomal STR profile of the semen donor from a living victim rapidly diminishes as the post-coital interval is extended due to the presence of only a small amount of male DNA amidst an overwhelming amount of female DNA. Previously, we have utilized various technological tools to overcome the limitations of male DNA profiling in extended interval post-coital samples including the use of Y-chromosome STR profiling, cervical sample, and post-PCR purification permitting the recovery of Y-STR profiles of the male DNA from samples collected 5-6 days after intercourse. Despite this success, the reproductive biology literature reports the presence of spermatozoa in the human cervix up to 7-10 days post-coitus. Therefore, novel and improved methods for recovery of male profiles in extended interval post-coital samples were required. Here, we describe enhanced strategies, including Y-chromosome-targeted pre-amplification and next generation Y-STR amplification kits, that have resulted in the ability to obtain probative male profiles from samples collected 6-9 days after intercourse.

Multielemental analysis in small amounts of environmental reference materials with inductively coupled plasma mass spectrometry.

PubMed

Dombovári, J; Becker, J S; Dietze, H J

2000-07-01

The lowest possible sample weight for performing multielemental trace element analysis on environmental and biological samples by ICP-MS has been investigated. The certified reference materials Bovine Liver NIST SRM 1577b, Human Hair NCS DC 73347 and Oriental Tobacco Leaves CTA-OTL-1 were applied at sample weights (1, 5, 20 and 50 mg aliquots, n = 10) which were significantly lower than those recommended with most recoveries in the range of 95-110%. Samples were digested in a mixture of nitric acid, hydrogen peroxide and hydrogen fluoride by closed-vessel microwave digestion. Multielemental analysis was performed with an optimized ICP-QMS method. Aqueous standard solutions were applied for external calibration with rhodium as the internal standard element. The detection limits varied between 0.02-0.38 microg/g for Li, Na, Cr, Mn, Ni, Cu, Zn, Sr, Cd, Ba and Pb, and up to 1.92 microg/g for Mg, Al, Ca, Fe and Ni. Digested human plasma samples were spiked with multielemental solution (0.5-10 microg/L) to test the analytical method and the recoveries were 95-105% for most analytes. Our results show that in the case of homogeneous SRMs it is possible to use them in very low amounts (1-5 mg) for method development and quality control.

Fuzziness-based active learning framework to enhance hyperspectral image classification performance for discriminative and generative classifiers

PubMed Central

2018-01-01

Hyperspectral image classification with a limited number of training samples without loss of accuracy is desirable, as collecting such data is often expensive and time-consuming. However, classifiers trained with limited samples usually end up with a large generalization error. To overcome the said problem, we propose a fuzziness-based active learning framework (FALF), in which we implement the idea of selecting optimal training samples to enhance generalization performance for two different kinds of classifiers, discriminative and generative (e.g. SVM and KNN). The optimal samples are selected by first estimating the boundary of each class and then calculating the fuzziness-based distance between each sample and the estimated class boundaries. Those samples that are at smaller distances from the boundaries and have higher fuzziness are chosen as target candidates for the training set. Through detailed experimentation on three publically available datasets, we showed that when trained with the proposed sample selection framework, both classifiers achieved higher classification accuracy and lower processing time with the small amount of training data as opposed to the case where the training samples were selected randomly. Our experiments demonstrate the effectiveness of our proposed method, which equates favorably with the state-of-the-art methods. PMID:29304512

Determination of small quantities of fluoride in water: A modified zirconium-alizarin method

USGS Publications Warehouse

Lamar, W.L.; Seegmiller, C.G.

1941-01-01

The zirconium-alizarin method has been modified to facilitate the convenient and accurate determination of small amounts of fluoride in a large number of water samples. Sulfuric acid is used to acidify the samples to reduce the interference of sulfate. The pH is accurately controlled to give the most sensitive comparisons. Most natural waters can be analyzed by the modified procedure without resorting to correction curves. The fluoride content of waters containing less than 500 parts per million of sulfate, 500 parts per million of bicarbonate, and 1000 parts per million of chloride may be determined within a limit of about 0.1 part per million when a 100-ml. sample is used.

Determination of trace amounts of tin in geological materials by atomic absorption spectrometry

USGS Publications Warehouse

Welsch, E.P.; Chao, T.T.

1976-01-01

An atomic absorption method is described for the determination of traces of tin in rocks, soils, and stream sediments. A dried mixture of the sample and ammonium iodide is heated to volatilize tin tetraiodide -which is then dissolved in 5 % hydrochloric acid, extracted into TOPO-MIBK, and aspirated into a nitrous oxide-acetylene flame. The limit of determination is 2 p.p.m. tin and the relative standard deviation ranges from 2 to 14 %. Up to 20 % iron and 1000 p.p.m. Cu, Pb, Zn, Mn, Hg, Mo, V, or W in the sample do not interfere. As many as 50 samples can be easily analyzed per man-day. ?? 1976.

Multiplex Amplification Coupled with COLD-PCR and High Resolution Melting Enables Identification of Low-Abundance Mutations in Cancer Samples with Low DNA Content

PubMed Central

Milbury, Coren A.; Chen, Clark C.; Mamon, Harvey; Liu, Pingfang; Santagata, Sandro; Makrigiorgos, G. Mike

2011-01-01

Thorough screening of cancer-specific biomarkers, such as DNA mutations, can require large amounts of genomic material; however, the amount of genomic material obtained from some specimens (such as biopsies, fine-needle aspirations, circulating-DNA or tumor cells, and histological slides) may limit the analyses that can be performed. Furthermore, mutant alleles may be at low-abundance relative to wild-type DNA, reducing detection ability. We present a multiplex-PCR approach tailored to amplify targets of interest from small amounts of precious specimens, for extensive downstream detection of low-abundance alleles. Using 3 ng of DNA (1000 genome-equivalents), we amplified the 1 coding exons (2-11) of TP53 via multiplex-PCR. Following multiplex-PCR, we performed COLD-PCR (co-amplification of major and minor alleles at lower denaturation temperature) to enrich low-abundance variants and high resolution melting (HRM) to screen for aberrant melting profiles. Mutation-positive samples were sequenced. Evaluation of mutation-containing dilutions revealed improved sensitivities after COLD-PCR over conventional-PCR. COLD-PCR improved HRM sensitivity by approximately threefold to sixfold. Similarly, COLD-PCR improved mutation identification in sequence-chromatograms over conventional PCR. In clinical specimens, eight mutations were detected via conventional-PCR-HRM, whereas 12 were detected by COLD-PCR-HRM, yielding a 33% improvement in mutation detection. In summary, we demonstrate an efficient approach to increase screening capabilities from limited DNA material via multiplex-PCR and improve mutation detection sensitivity via COLD-PCR amplification. PMID:21354058

Prediction of internal and external noise fields for blowdown wind tunnels.

NASA Technical Reports Server (NTRS)

Hosier, R. N.; Mayes, W. H.

1972-01-01

Empirical methods have been developed to estimate the test section noise levels and the outside noise radiation patterns of blowdown wind tunnels. Included are considerations of noise generation by control valves, burners, turbulent boundary layers, and exhaust jets as appropriate. Sample test section and radiation field noise estimates are presented. The external estimates are noted to be in good agreement with the limited amount of available measurements.

Estimating carbon and nitrogen pools in a forest soil: Influence of soil bulk density methods and rock content

Treesearch

Martin F. Jurgensen; Deborah S. Page-Dumroese; Robert E. Brown; Joanne M. Tirocke; Chris A. Miller; James B. Pickens; Min Wang

2017-01-01

Soils with high rock content are common in many US forests, and contain large amounts of stored C. Accurate measurements of soil bulk density and rock content are critical for calculating and assessing changes in both C and nutrient pool size, but bulk density sampling methods have limitations and sources of variability. Therefore, we evaluated the use of small-...

Effect of cooking on total mercury content in Norway lobster and European hake and public health impact.

PubMed

Perugini, Monia; Zezza, Daniela; Tulini, Serena Maria Rita; Abete, Maria Cesarina; Monaco, Gabriella; Conte, Annamaria; Olivieri, Vincenzo; Amorena, Michele

2016-08-15

The risk of Hg poisoning by eating seafood is considered real from the several international agencies that recommended, by fish consumption advisories, to pregnant women and young children to avoid or severely limit the consumption of the fish and shellfish with a high-range mercury levels. The analyses of two common species, European hake and Norway lobster, collected from an area of Central Adriatic Sea, reported high mercury levels in crustaceans. For Norway lobster total mercury exceeded, in six out of ten analysed pools, the recommended 0.5mg/kg wet weight European limit. Moreover the increased amount of Hg concentrations in Norway lobster cooked samples suggests the necessity to review current procedures of Hg control in food, considering also consumption habits of consumers. The Hg values found in all European hake samples are below the legal limits and, in this species, the boiling did not modify the concentrations in fish tissues. Copyright © 2016 Elsevier Ltd. All rights reserved.

Molecular barcodes detect redundancy and contamination in hairpin-bisulfite PCR

PubMed Central

Miner, Brooks E.; Stöger, Reinhard J.; Burden, Alice F.; Laird, Charles D.; Hansen, R. Scott

2004-01-01

PCR amplification of limited amounts of DNA template carries an increased risk of product redundancy and contamination. We use molecular barcoding to label each genomic DNA template with an individual sequence tag prior to PCR amplification. In addition, we include molecular ‘batch-stamps’ that effectively label each genomic template with a sample ID and analysis date. This highly sensitive method identifies redundant and contaminant sequences and serves as a reliable method for positive identification of desired sequences; we can therefore capture accurately the genomic template diversity in the sample analyzed. Although our application described here involves the use of hairpin-bisulfite PCR for amplification of double-stranded DNA, the method can readily be adapted to single-strand PCR. Useful applications will include analyses of limited template DNA for biomedical, ancient DNA and forensic purposes. PMID:15459281

Laser fluorometric analysis of plants for uranium exploration

USGS Publications Warehouse

Harms, T.F.; Ward, F.N.; Erdman, J.A.

1981-01-01

A preliminary test of biogeochemical exploration for locating uranium occurrences in the Marfa Basin, Texas, was conducted in 1978. Only 6 of 74 plant samples (mostly catclaw mimosa, Mimosa biuncifera) contained uranium in amounts above the detection limit (0.4 ppm in the ash) of the conventional fluorometric method. The samples were then analyzed using a Scintrex UA-3 uranium analyzer* * Use of trade names in this paper is for descriptive purposes only and does not constitute endorsement by the U.S. Geological Survey. - an instrument designed for direct analysis of uranium in water, and which can be conveniently used in a mobile field laboratory. The detection limit for uranium in plant ash (0.05 ppm) by this method is almost an order of magnitude lower than with the fluorometric conventional method. Only 1 of the 74 samples contained uranium below the detection limit of the new method. Accuracy and precision were determined to be satisfactory. Samples of plants growing on mineralized soils and nonmineralized soils show a 15-fold difference in uranium content; whereas the soils themselves (analyzed by delayed neutron activation analysis) show only a 4-fold difference. The method involves acid digestion of ashed tissue, extraction of uranium into ethyl acetate, destruction of the ethyl acetate, dissolution of the residue in 0.005% nitric acid, and measurement. ?? 1981.

Sediment loads and transport at constructed chutes along the Missouri River - Upper Hamburg Chute near Nebraska City, Nebraska, and Kansas Chute near Peru, Nebraska

USGS Publications Warehouse

Densmore, Brenda K.; Rus, David L.; Moser, Matthew T.; Hall, Brent M.; Andersen, Michael J.

2016-02-04

Comparisons of concentrations and loads from EWI samples collected from different transects within a study site resulted in few significant differences, but comparisons are limited by small sample sizes and large within-transect variability. When comparing the Missouri River upstream transect to the chute inlet transect, similar results were determined in 2012 as were determined in 2008—the chute inlet affected the amount of sediment entering the chute from the main channel. In addition, the Kansas chute is potentially affecting the sediment concentration within the Missouri River main channel, but small sample size and construction activities within the chute limit the ability to fully understand either the effect of the chute in 2012 or the effect of the chute on the main channel during a year without construction. Finally, some differences in SSC were detected between the Missouri River upstream transects and the chute downstream transects; however, the effect of the chutes on the Missouri River main-channel sediment transport was difficult to isolate because of construction activities and sampling variability.

Space Density Of Optically-Selected Type II Quasars From The SDSS

NASA Astrophysics Data System (ADS)

Reyes, Reinabelle; Zakamska, N. L.; Strauss, M. A.; Green, J.; Krolik, J. H.; Shen, Y.; Richards, G. T.

2007-12-01

Type II quasars are luminous Active Galactic Nuclei (AGN) whose central regions are obscured by large amounts of gas and dust. In this poster, we present a catalog of 887 type II quasars with redshifts z<0.83 from the Sloan Digital Sky Survey (SDSS), selected based on their emission lines, and derive the 1/Vmax [OIII] 5007 luminosity function from this sample. Since some objects may not be included in the sample because they lack strong emission lines, the derived luminosity function is only a lower limit. We also derive the [OIII] 5007 luminosity function for a sample of type I (broad-line) quasars in the same redshift range. Taking [OIII] 5007 luminosity as a tracer of intrinsic luminosity in both type I and type II quasars, we obtain lower limits to the type II quasar fraction as a function of [OIII] 5007 luminosity, from L[OIII] = 108.3 to 1010 Lsun, which roughly correspond to bolometric luminosities of 1044 to 1046 erg/s.

Elution of lead from lead zirconate titanate ceramics to acid rain

NASA Astrophysics Data System (ADS)

Tsurumi, Takaaki; Takezawa, Shuhei; Hoshina, Takuya; Takeda, Hiroaki

2017-10-01

The amount of lead that eluted from lead zirconate titanate (PZT) ceramics to artificial acid rain was evaluated. Four kinds of PZT ceramics, namely, pure PZT at MPB composition, CuO-added PZT, PZT with 10 mol % substitution of Ba for Pb, and CuO-added PZT with 10 mol % substitution of Ba for Pb, were used as samples of the elution test. These PZT ceramics of 8 mm2 and 1.1-1.2 mm thickness were suspended in 300 ml of H2SO4 solution of pH 4.0. The concentration of lead eluted from PZT was in the range from 0.2 to 0.8 ppm. It was found that both liquid phase formation by the addition of CuO and the substitution of Ba for Pb were effective to reduce the amount of lead that eluted. By fitting the leaching out curve with a classical equation, a master curve assuming no sampling effect was obtained. The lead concentration evaluated from the amount of lead that eluted from a commercial PZT plate to H2SO4 solution of pH 5.3 was almost the same as the limit in city water. It is concluded that PZT is not harmful to health and the environment and the amount of lead that eluted from PZT can be controlled by modifying PZT composition.

Determination of trace amount of formaldehyde base on a bromate-Malachite Green system.

PubMed

Tang, Yufang; Chen, Hao; Weng, Chao; Tang, Xiaohui; Zhang, Miaoling; Hu, Tao

2015-01-25

A novel catalytic kinetic spectrophotometric method for determination of trace amount of formaldehyde (FA) has been established, based on catalytic effect of trace amount of FA on the oxidation of Malachite Green (MG) by potassium bromate in presence of sulfuric acid medium, and was reported for the first time. The method was monitored by measuring the decrease in absorbance of MG at 617 nm and allowed a precise determination of FA in the range of 0.003-0.08 μg mL(-1), with a limit of detection down to 1 ng mL(-1). The relative standard deviation of 10 replicate measurements was 1.63%. The method developed was approved to be sensitive, selective and accurate, and adopted to determinate free FA in samples directly with good accuracy and reproducibility. Copyright © 2014 Elsevier B.V. All rights reserved.

Copper(II)-rubeanic acid coprecipitation system for separation-preconcentration of trace metal ions in environmental samples for their flame atomic absorption spectrometric determinations.

PubMed

Soylak, Mustafa; Erdogan, Nilgun D

2006-09-21

A simple and facile preconcentration procedure based on the coprecipitation of trace heavy metal ions with copper(II)-rubeanic acid complex has been developed. The analytical parameters including pH, amounts of rubeanic acid, sample volume, etc. was investigated for the quantitative recoveries of Pb(II), Fe(III), Cd(II), Au(III), Pd(II) and Ni(II). No interferic effects were observed from the concomitant ions. The detection limits for analyte ions by 3 sigma were in the range of 0.14 microg/l for iron-3.4 microg/l for lead. The proposed coprecipitation method was successfully applied to water samples from Palas Lake-Kayseri, soil and sediment samples from Kayseri and Yozgat-Turkey.

Nitromethane K-9 Detection Limit

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

Strobel, R; Kury, J

2003-08-29

The Bureau of Alcohol, Tobacco and Firearms (ATF) trains canine/handler teams to detect explosives for government and other agencies worldwide. After completing the training program the teams are tested on an array containing explosives and numerous other samples designed to distract a canine. Passing this test results in a team's certification. These teams can be considered as ''detection instruments'' freshly calibrated just before leaving the ''factory''. Using these teams to examine special experimental arrays immediately following certification can lead to a better understanding of a canine's detection capabilities. Forty-one of these ''detection instruments'' were used in four test series withmore » arrays containing dilute nitromethane-in-water solutions. (The canines had been trained on the amount of nitromethane vapor in equilibrium with the undiluted liquid explosive.) By diluting liquid nitromethane with water, the amount of explosive vapor can be reduced many orders of magnitude to test the lower limit of the canine's nitromethane vapor detection response. The results are presented in this paper.« less

A standardized method for sampling and extraction methods for quantifying microplastics in beach sand.

PubMed

Besley, Aiken; Vijver, Martina G; Behrens, Paul; Bosker, Thijs

2017-01-15

Microplastics are ubiquitous in the environment, are frequently ingested by organisms, and may potentially cause harm. A range of studies have found significant levels of microplastics in beach sand. However, there is a considerable amount of methodological variability among these studies. Methodological variation currently limits comparisons as there is no standard procedure for sampling or extraction of microplastics. We identify key sampling and extraction procedures across the literature through a detailed review. We find that sampling depth, sampling location, number of repeat extractions, and settling times are the critical parameters of variation. Next, using a case-study we determine whether and to what extent these differences impact study outcomes. By investigating the common practices identified in the literature with the case-study, we provide a standard operating procedure for sampling and extracting microplastics from beach sand. Copyright © 2016 Elsevier Ltd. All rights reserved.

Microvolume protein concentration determination using the NanoDrop 2000c spectrophotometer.

PubMed

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

2009-11-04

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

31 CFR 342.5 - Limitations.

Code of Federal Regulations, 2011 CFR

2011-07-01

... savings plan, purchases of notes could not exceed $350 (face amount) a quarter, and in no event could the annual limitation of $1,350 (face amount) be exceeded. (b) Holdings. The face amount of savings notes...

31 CFR 342.5 - Limitations.

Code of Federal Regulations, 2013 CFR

2013-07-01

... savings plan, purchases of notes could not exceed $350 (face amount) a quarter, and in no event could the annual limitation of $1,350 (face amount) be exceeded. (b) Holdings. The face amount of savings notes...

31 CFR 342.5 - Limitations.

Code of Federal Regulations, 2014 CFR

2014-07-01

... savings plan, purchases of notes could not exceed $350 (face amount) a quarter, and in no event could the annual limitation of $1,350 (face amount) be exceeded. (b) Holdings. The face amount of savings notes...

Electrospun biocompatible Chitosan/MIL-101 (Fe) composite nanofibers for solid-phase extraction of Δ9-tetrahydrocannabinol in whole blood samples using Box-Behnken experimental design.

PubMed

Asiabi, Mina; Mehdinia, Ali; Jabbari, Ali

2017-01-06

The nanofibers of biocompatible Chitosan/MIL-101 (Fe) composite were synthesized by a simple, cheap and accessible electrospining method and applied for mat-based extraction of trace amount of Δ9-tetrahydrocannabinol (THC) from human whole blood sample following its combination by high performance liquid chromatography-ultraviolet detection. The composite nanofibres were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and N 2 adsorption-desorption experiments. The volume of eluting solvent, sorbent amount, pH and% NaCl (w/v) influencing on the responses were investigated using factorial experimental design. The optimum point was achieved by analysis of the results according to design expert (DX) software. The volume of eluting solvent, sorbent amount and pH were significant variables, and 150μL, 7mg and 7.0 were respectively chosen for obtaining the best extraction response. Under the optimum conditions, the method was exhibited a linear range of 0.1-100μgL -1 (R 2 =0.9943) for THC with a detection limit of 0.04μgL -1 . Acceptable values for intra-day (3.2%) and inter-day (4.8%) relative standard deviations were obtained. The high preconcentration factor (970) and satisfactory recoveries (88.2%-92.4%) in whole blood samples were achieved which proved the capability of the method for trace determination of THC in the human whole blood samples. Copyright © 2016 Elsevier B.V. All rights reserved.

The simulation of the LANFOS-H food radiation contamination detector using Geant4 package

NASA Astrophysics Data System (ADS)

Piotrowski, Lech Wiktor; Casolino, Marco; Ebisuzaki, Toshikazu; Higashide, Kazuhiro

2015-02-01

Recent incident in the Fukushima power plant caused a growing concern about the radiation contamination and resulted in lowering the Japanese limits for the permitted amount of 137Cs in food to 100 Bq/kg. To increase safety and ease the concern we are developing LANFOS (Large Food Non-destructive Area Sampler)-a compact, easy to use detector for assessment of radiation in food. Described in this paper LANFOS-H has a 4 π coverage to assess the amount of 137Cs present, separating it from the possible 40K food contamination. Therefore, food samples do not have to be pre-processed prior to a test and can be consumed after measurements. It is designed for use by non-professionals in homes and small institutions such as schools, showing safety of the samples, but can be also utilized by specialists providing radiation spectrum. Proper assessment of radiation in food in the apparatus requires estimation of the γ conversion factor of the detectors-how many γ photons will produce a signal. In this paper we show results of the Monte Carlo estimation of this factor for various approximated shapes of fish, vegetables and amounts of rice, performed with Geant4 package. We find that the conversion factor combined from all the detectors is similar for all food types and is around 37%, varying maximally by 5% with sample length, much less than for individual detectors. The different inclinations and positions of samples in the detector introduce uncertainty of 1.4%. This small uncertainty validates the concept of a 4 π non-destructive apparatus.

A direct immersion solid-phase microextraction gas chromatography/mass spectrometry method for the simultaneous detection of levamisole and minor cocaine congeners in hair samples from chronic abusers.

PubMed

Fucci, Nadia; Gambelunghe, Cristiana; Aroni, Kyriaki; Rossi, Riccardo

2014-12-01

Because levamisole has been increasingly found as a component of illicit drugs, a robust method to detect its presence in hair samples is needed. However, no systematic research on the detection of levamisole in hair samples has been published. The method presented here uses direct immersion solid-phase microextraction coupled with gas chromatography and mass spectrometry (DI-SPME-GC/MS) to detect levamisole and minor cocaine congeners in hair samples using a single-extraction method. Fifty hair samples taken in the last 4 years were obtained from cocaine abusers, along with controls taken from drug-free volunteers. Sampling was performed using direct immersion with a 30-μm polydimethylsiloxane fused silica/stainless steel fiber. Calibration curves were prepared by adding known amounts of analytes and deuterated internal standards to the hair samples taken from drug-free volunteers. This study focused on the adulterant levamisole and some minor cocaine congeners (tropococaine, norcocaine, and cocaethylene). Levamisole was detected in 38% of the hair samples analyzed; its concentration ranged from 0.2 to 0.8 ng/mg. The limit of quantification and limit of detection for levamisole, tropococaine, norcocaine, and cocaine were 0.2 and 0.1 ng/mg, respectively. DI-SPME-GC/MS is a sensitive and specific method to detect the presence of levamisole and cocaine congeners in hair samples.

Evaluation of laboratory powder X-ray micro-diffraction for applications in the fields of cultural heritage and forensic science.

PubMed

Svarcová, Silvie; Kocí, Eva; Bezdicka, Petr; Hradil, David; Hradilová, Janka

2010-09-01

The uniqueness and limited amounts of forensic samples and samples from objects of cultural heritage together with the complexity of their composition requires the application of a wide range of micro-analytical methods, which are non-destructive to the samples, because these must be preserved for potential late revision. Laboratory powder X-ray micro-diffraction (micro-XRD) is a very effective non-destructive technique for direct phase analysis of samples smaller than 1 mm containing crystal constituents. It compliments optical and electron microscopy with elemental micro-analysis, especially in cases of complicated mixtures containing phases with similar chemical composition. However, modification of X-ray diffraction to the micro-scale together with its application for very heterogeneous real samples leads to deviations from the standard procedure. Knowledge of both the limits and the phenomena which can arise during the analysis is crucial for the meaningful and proper application of the method. We evaluated basic limits of micro-XRD equipped with a mono-capillary with an exit diameter of 0.1 mm, for example the size of irradiated area, appropriate grain size, and detection limits allowing identification of given phases. We tested the reliability and accuracy of quantitative phase analysis based on micro-XRD data in comparison with conventional XRD (reflection and transmission), carrying out experiments with two-phase model mixtures simulating historic colour layers. Furthermore, we demonstrate the wide use of micro-XRD for investigation of various types of micro-samples (contact traces, powder traps, colour layers) and we show how to enhance data quality by proper choice of experiment geometry and conditions.

Adaptive optics in spinning disk microscopy: improved contrast and brightness by a simple and fast method.

PubMed

Fraisier, V; Clouvel, G; Jasaitis, A; Dimitrov, A; Piolot, T; Salamero, J

2015-09-01

Multiconfocal microscopy gives a good compromise between fast imaging and reasonable resolution. However, the low intensity of live fluorescent emitters is a major limitation to this technique. Aberrations induced by the optical setup, especially the mismatch of the refractive index and the biological sample itself, distort the point spread function and further reduce the amount of detected photons. Altogether, this leads to impaired image quality, preventing accurate analysis of molecular processes in biological samples and imaging deep in the sample. The amount of detected fluorescence can be improved with adaptive optics. Here, we used a compact adaptive optics module (adaptive optics box for sectioning optical microscopy), which was specifically designed for spinning disk confocal microscopy. The module overcomes undesired anomalies by correcting for most of the aberrations in confocal imaging. Existing aberration detection methods require prior illumination, which bleaches the sample. To avoid multiple exposures of the sample, we established an experimental model describing the depth dependence of major aberrations. This model allows us to correct for those aberrations when performing a z-stack, gradually increasing the amplitude of the correction with depth. It does not require illumination of the sample for aberration detection, thus minimizing photobleaching and phototoxicity. With this model, we improved both signal-to-background ratio and image contrast. Here, we present comparative studies on a variety of biological samples. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Active sampling technique to enhance chemical signature of buried explosives

NASA Astrophysics Data System (ADS)

Lovell, John S.; French, Patrick D.

2004-09-01

Deminers and dismounted countermine engineers commonly use metal detectors, ground penetrating radar and probes to locate mines. Many modern landmines have a very low metal content, which severely limits the effectiveness of metal detectors. Canines have also been used for landmine detection for decades. Experiments have shown that canines smell the explosives which are known to leak from most types of landmines. The fact that dogs can detect landmines indicates that vapor sensing is a viable approach to landmine detection. Several groups are currently developing systems to detect landmines by "sniffing" for the ultra-trace explosive vapors above the soil. The amount of material that is available to passive vapor sensing systems is limited to no more than the vapor in equilibrium with the explosive related chemicals (ERCs) distributed in the surface soils over and near the landmine. The low equilibrium vapor pressure of TNT in the soil/atmosphere boundary layer and the limited volume of the boundary layer air imply that passive chemical vapor sensing systems require sensitivities in the picogram range, or lower. ADA is working to overcome many of the limitations of passive sampling methods, by the use of an active sampling method that employs a high-powered (1,200+ joules) strobe lamp to create a highly amplified plume of vapor and/or ERC-bearing fine particulates. Initial investigations have demonstrated that this approach can amplify the detectability of TNT by two or three orders of magnitude. This new active sampling technique could be used with any suitable explosive sensor.

Using multi-spectral landsat imagery to examine forest health trends at Fort Benning, Georgia

Treesearch

Shawna L. Reid; Joan L. Walker; Abigail Schaaf

2016-01-01

Assessing vegetation health attributes like canopy density or live crown ratio and ecological processes such as growth or succession ultimately requires direct measures of plant communities. However, on-theground sampling is labor and time intensive, effectively limiting the amount of forest that can be evaluated. Radiometric data collected with a variety of sensors ...

Highly sensitive spectrofluorimetric determination of trace amounts NADP using Europium ion-doxycycline complex probe

NASA Astrophysics Data System (ADS)

Peng, Qian; Hou, Faju; Jiang, Chongqiu

2006-09-01

A new spectrofluorimetric method was developed for determination of trace amount of Coenzyme II (NADP). Using europium ion-doxycycline (DC) as a fluorescent probe, in the buffer solution of pH 8.44, NADP can remarkably enhance the fluorescence intensity of the Eu 3+-DC complex at λ = 612 nm and the enhanced fluorescence intensity is in proportion to the concentration of NADP. Optimum conditions for the determination of NADP were also investigated. The dynamic range for the determination of NADP is 3.3 × 10 -7 to 6.1 × 10 -6 mol l -1 with detection limit of 6.8 × 10 -8 mol l -1. This method is simple, practical and relatively free interference from coexisting substances and can be successfully applied to determination of NADP in synthetic water samples and in serum samples. Moreover, the enhancement mechanisms of the fluorescence intensity in the Eu 3+-DC system and the Eu 3+-DC-NADP system have been also discussed.

Dynamic microwave assisted extraction coupled with dispersive micro-solid-phase extraction of herbicides in soybeans.

PubMed

Li, Na; Wu, Lijie; Nian, Li; Song, Ying; Lei, Lei; Yang, Xiao; Wang, Kun; Wang, Zhibing; Zhang, Liyuan; Zhang, Hanqi; Yu, Aimin; Zhang, Ziwei

2015-09-01

Non-polar solvent dynamic microwave assisted extraction was firstly applied to the treatment of high-fat soybean samples. In the dispersive micro-solid-phase extraction (D-µ-SPE), the herbicides in the high-fat extract were directly adsorbed on metal-organic frameworks MIL-101(Cr). The effects of several experimental parameters, including extraction solvent, microwave absorption medium, microwave power, volume and flow rate of extraction solvent, amount of MIL-101(Cr), and D-µ-SPE time, were investigated. At the optimal conditions, the limits of detection for the herbicides ranged from 1.56 to 2.00 μg kg(-1). The relative recoveries of the herbicides were in the range of 91.1-106.7%, and relative standard deviations were equal to or lower than 6.7%. The present method was simple, rapid and effective. A large amount of fat was also removed. This method was demonstrated to be suitable for treatment of high-fat samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Leaching for recovery of copper from municipal solid waste incineration fly ash: influence of ash properties and metal speciation.

PubMed

Lassesson, Henric; Fedje, Karin Karlfeldt; Steenari, Britt-Marie

2014-08-01

Recovery of metals occurring in significant amounts in municipal solid waste incineration fly ash, such as copper, could offer several advantages: a decreased amount of potentially mobile metal compounds going to landfill, saving of natural resources and a monetary value. A combination of leaching and solvent extraction may constitute a feasible recovery path for metals from municipal solid waste incineration fly ash. However, it has been shown that the initial dissolution and leaching is a limiting step in such a recovery process. The work described in this article was focused on elucidating physical and chemical differences between two ash samples with the aim of explaining the differences in copper release from these samples in two leaching methods. The results showed that the chemical speciation is an important factor affecting the release of copper. The occurrence of copper as phosphate or silicate will hinder leaching, while sulphate and chloride will facilitate leaching. © The Author(s) 2014.

Spectrophotometric catalytic determination of small amounts of rhenium in mineralized rocks and molybdenite

USGS Publications Warehouse

Simon, F.O.; Grimaldi, F.S.

1962-01-01

Rhenium is determined by spectrophotometry of the tellurium sol formed by the reduction of tellurate by stannous chloride under the catalytic influence of rhenium. A detailed investigation of the conditions for high sensitivity and stability at lowest concentration levels of rhenium is presented as well as the behavior of 26 ions. The method is applied to the determination of some tenths of 1 p.p.m. or more of rhenium in a 1-mg. aliquot of mineralized rocks, mixtures of molybdenite and rocks, and molybdenite concentrates. The practical quantity limit of detection is 2 ?? 10-10 gram of rhenium. Samples are decomposed with a mixture of CaO, CaCl2, and MgO. On leaching, most constituents of the sample are precipitated either as calcium salts or hydroxides, except for rhenium and a small amount of molybdenum which pass into the filtrate. Residual molybdenum is removed by extraction with 8-quinolinol in chloroform. Better than 95% recoveries are obtained with two fusions with flux.

Simultaneous spectrophotometric determination of trace amounts of uranium, thorium, and zirconium using the partial least squares method after their preconcentration by alpha-benzoin oxime modified Amberlite XAD-2000 resin.

PubMed

Ghasemi, Jahan B; Zolfonoun, E

2010-01-15

A new solid phase extraction method for separation and preconcentration of trace amounts of uranium, thorium, and zirconium in water samples is proposed. The procedure is based on the adsorption of U(VI), Th(IV) and Zr(IV) ions on a column of Amberlite XAD-2000 resin loaded with alpha-benzoin oxime prior to their simultaneous spectrophotometric determination with Arsenazo III using orthogonal signal correction partial least squares method. The enrichment factor for preconcentration of uranium, thorium, and zirconium was found to be 100. The detection limits for U(VI), Th(IV) and Zr(IV) were 0.50, 0.54, and 0.48microgL(-1), respectively. The precision of the method, evaluated as the relative standard deviation obtained by analyzing a series of 10 replicates, was below 4% for all elements. The practical applicability of the developed sorbent was examined using synthetic seawater, natural waters and ceramic samples.

Super-Nyquist White Dwarf Pulsations in K2 Long-Cadence Data

NASA Astrophysics Data System (ADS)

Bell, Keaton J.; Hermes, JJ; Montgomery, Michael H.; Vanderbosch, Zach

2017-06-01

The Kepler and K2 missions have recently revolutionized the field of white dwarf asteroseismology. Since white dwarfs pulsate on timescales of order 10 minutes, we aim to observe these objects at K2’s short cadence (1 minute). Occasionally we find signatures of pulsations in white dwarf targets that were only observed by K2 at long cadence (30 minute). These signals suffer extreme aliasing since the intrinsic frequencies exceed the Nyquist sampling limit. We present our work to recover accurate frequency determinations for these targets, guided by a limited amount of supplementary, ground-based photometry from McDonald Observatory.

Time-course measurements of caffeine and its metabolites extracted from fingertips after coffee intake: a preliminary study for the detection of drugs from fingerprints.

PubMed

Kuwayama, Kenji; Tsujikawa, Kenji; Miyaguchi, Hajime; Kanamori, Tatsuyuki; Iwata, Yuko T; Inoue, Hiroyuki

2013-05-01

The aim of this study was to determine whether an ingested drug and its metabolites could be detected in the subject's fingerprints. Caffeine (CF) was chosen as the model drug. Three healthy subjects were asked to consume a cup of coffee (ca. 100 mL) containing 80 micro micro mg CF as the total dose, which is the normal amount in one cup of coffee. After washing hands with water to remove external contaminants, each subject pressed the index fingertip to a collecting matrix just before consuming the test cup of coffee, and then again pressed the index fingertip to the collecting matrix after 1, 3, 5, and 7 h. The time curve of the amounts of CF and its metabolites-theobromine (TB), paraxanthine (PX), and theophylline (TP)-in fingerprints and blood was determined using liquid chromatography/tandem mass spectrometry (LC/MS). A filter paper wetted with water (50 μL) was an efficient collecting matrix for extracting the analytes from the fingertip. With optimized sample preparation and LC/MS conditions, the total operating time, from taking the fingerprints to obtaining the analytical result, was approximately 10 min. The lower limits of quantification for CF, TB, PX, and TP were 0.5, 5, 0.5, and 5 ng/fingerprint, respectively. The amount of CF or PX determined in fingerprints obtained over 7 h after coffee intake was significantly greater than the amount determined in fingerprints taken before drinking coffee. Fingerprints were a more efficient source for drug testing than other biological samples, such as blood and sweat, because the procedures for sampling and extracting the drugs were simpler and took less time. The method could be used to prove drug intake in criminal investigations.

Quantification of fluorine traces in solid samples using CaF molecular emission bands in atmospheric air Laser-Induced Breakdown Spectroscopy

NASA Astrophysics Data System (ADS)

Alvarez-Llamas, C.; Pisonero, J.; Bordel, N.

2016-09-01

Direct solid determination of trace amounts of fluorine using Laser-Induced Breakdown Spectroscopy (LIBS) is a challenging task due to the low excitation efficiency of this element. Several strategies have been developed to improve the detection capabilities, including the use of LIBS in a He atmosphere to enhance the signal to background ratios of F atomic emission lines. An alternative method is based on the detection of the molecular compounds that are formed with fluorine in the LIBS plasma. In this work, the detection of CaF molecular emission bands is investigated to improve the analytical capabilities of atmospheric air LIBS for the determination of fluorine traces in solid samples. In particular, Cu matrix samples containing different fluorine concentration (between 50 and 600 μg/g), and variable amounts of Ca, are used to demonstrate the linear relationships between CaF emission signal and F concentration. Limits of detection for fluorine are improved by more than 1 order of magnitude using CaF emission bands versus F atomic lines, in atmospheric-air LIBS. Furthermore, a toothpaste powder sample is used to validate this analytical method. Good agreement is observed between the nominal and the predicted fluorine mass-content.

Rapid determination of caffeine in one drop of beverages and foods using drop-to-drop solvent microextraction with gas chromatography/mass spectrometry.

PubMed

Shrivas, Kamlesh; Wu, Hui-Fen

2007-11-02

A simple and rapid sample cleanup and preconcentration method for the quantitative determination of caffeine in one drop of beverages and foods by gas chromatography/mass spectrometry (GC/MS) has been proposed using drop-to-drop solvent microextraction (DDSME). The best optimum experimental conditions for DDSME were: chloroform as the extraction solvent, 5 min extraction time, 0.5 microL exposure volume of the extraction phase and no salt addition at room temperature. The optimized methodology exhibited good linearity between 0.05 and 5.0 microg/mL with correlation coefficient of 0.980. The relative standard deviation (RSD) and limits of detection (LOD) of the DDSME/GC/MS method were 4.4% and 4.0 ng/mL, respectively. Relative recovery of caffeine in beverages and foods were found to be 96.6-101%, which showing good reliability of this method. This DDSME excludes the major disadvantages of conventional method of caffeine extraction, like large amount of organic solvent and sample consumption and long sample pre-treatment process. So, this approach proves that the DDSME/GC/MS technique can be applied as a simple, fast and feasible diagnosis tool for environmental, food and biological application for extremely small amount of real sample analysis.

Application of a thiourea-containing task-specific ionic liquid for the solid-phase extraction cleanup of lead ions from red lipstick, pine leaves, and water samples.

PubMed

Saljooqi, Asma; Shamspur, Tayebeh; Mohamadi, Maryam; Mostafavi, Ali

2014-07-01

Here, task-specific ionic liquid solid-phase extraction is proposed for the first time. In this approach, a thiourea-functionalized ionic liquid is immobilized on the solid sorbent, multiwalled carbon nanotubes. These modified nanotubes packed into a solid-phase extraction column are used for the selective extraction and preconcentration of ultra-trace amounts of lead(II) from aqueous samples prior to electrothermal atomic absorption spectroscopy determination. The thiourea functional groups act as chelating agents for lead ions retaining them and so, give the selectivity to the sorbent. Elution of the retained ions can be performed using an acidic thiourea solution. The effects of experimental parameters including pH of the aqueous solution, type and amount of eluent, and the flow rates of sample and eluent solutions on the separation efficiency are investigated. The linear dependence of absorbance of lead on its concentration in the initial solution is in the range of 0.5-40.0 ng/mL with the detection limit of 0.13 ng/mL (3(Sb)/m, n = 10). The proposed method is applicable to the analysis of red lipstick, pine leaves, and water samples for their lead contents. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-Cycle, Push-Pull Fatigue Fracture Behavior of High-C, Si-Al-Rich Nanostructured Bainite Steel.

PubMed

Zhao, Jing; Ji, Honghong; Wang, Tiansheng

2017-12-29

The high-cycle, push-pull fatigue fracture behavior of high-C, Si-Al-rich nanostructured bainitic steel was studied through the measurement of fatigue limits, a morphology examination and phase composition analysis of the fatigue fracture surface, as well as fractography of the fatigue crack propagation. The results demonstrated that the push-pull fatigue limits at 10⁷ cycles were estimated as 710-889 MPa, for the samples isothermally transformed at the temperature range of 220-260 °C through data extrapolation, measured under the maximum cycle number of 10⁵. Both the interior inclusion and the sample surface constituted the fatigue crack origins. During the fatigue crack propagation, a high amount of secondary cracks were formed in almost parallel arrangements. The apparent plastic deformation occurred in the fracture surface layer, which induced approximately all retained austenite to transform into martensite.

High-Cycle, Push–Pull Fatigue Fracture Behavior of High-C, Si–Al-Rich Nanostructured Bainite Steel

PubMed Central

Zhao, Jing; Ji, Honghong

2017-01-01

The high-cycle, push–pull fatigue fracture behavior of high-C, Si–Al-rich nanostructured bainitic steel was studied through the measurement of fatigue limits, a morphology examination and phase composition analysis of the fatigue fracture surface, as well as fractography of the fatigue crack propagation. The results demonstrated that the push–pull fatigue limits at 107 cycles were estimated as 710–889 MPa, for the samples isothermally transformed at the temperature range of 220–260 °C through data extrapolation, measured under the maximum cycle number of 105. Both the interior inclusion and the sample surface constituted the fatigue crack origins. During the fatigue crack propagation, a high amount of secondary cracks were formed in almost parallel arrangements. The apparent plastic deformation occurred in the fracture surface layer, which induced approximately all retained austenite to transform into martensite. PMID:29286325

Comparison of supercritical fluid extraction and Soxhlet extraction for the determination of PCBs in seaweed samples.

PubMed

Punín Crespo, M O; Lage Yusty, M A

2005-06-01

The efficiency of supercritical fluid extraction for the determination of 12 polychlorinated biphenyls from algae samples is compared to Soxhlet extraction. Analytical detection limits for the individual congeners ranged from 0.62 microgl(-1) to 19 microgl(-1). Recovery was tested for both methods using standard addition procedure. At maximum spike level of concentration, the mean recoveries were not significantly different (P>0.05) of all PCBs studied, with the exception of PCBs 28, 52, 77 and 169. Method precision for Soxhlet extraction (< or =3.9%) was slightly better than for SFE (< or =9.2%). Although both methods yield comparable results, SFE offers the advantage of detecting all PCBs studied at lower concentrations, reducing extraction time, and reducing the amount of solvents needed. The optimized methods were applied to the analysis of three real seaweed samples, except for PCB101 the concentrations of all PCBs were low or below the detection limits. The levels of PCB101 found in sample 1 were 6.6+/-0.54 ng g(-1) d.w., in sample 2 the levels were 8.2+/-0.86 ng g(-1) d.w. and in sample 3 they were 7.7+/-0.08 ng g(-1) d.w.

Determination of heavy metal ions in vegetable samples using a magnetic metal-organic framework nanocomposite sorbent.

PubMed

Hassanpour, Akbar; Hosseinzadeh-Khanmiri, Rahim; Babazadeh, Mirzaagha; Abolhasani, Jafar; Ghorbani-Kalhor, Ebrahim

2015-01-01

This paper describes the synthesis and application of a novel magnetic metal-organic framework (MOF) [(Fe₃O₄-benzoyl isothiocyanate)/Cu₃(benzene-1,3,5-tricarboxylate)₂] to pre-concentrate trace amounts of Cd(II), Pb(II), Zn(II) and Cr(III) ions and their determination by flame atomic absorption spectrometry. A Box-Behnken design was used to find the parameters affecting the pre-concentration procedure through response surface methodology. Three factors including uptake time, amount of the magnetic sorbent and pH of the sample were selected as affecting factors in the sorption step, and four factors including type, volume and concentration of the eluent as well as the elution time were selected in the elution step for the optimisation study. The opted values were 30 mg, 10.1 min, 5.9, EDTA, 4.0 ml, 0.57 mol l(-1) EDTA solution and 13.0 min for the amount of the magnetic sorbent, uptake time, pH of the sample, type, volume, concentration of the eluent, and elution time, respectively. The limits of detection (LODs) were 0.12, 0.7, 0.16, and 0.4 ng ml(-1) for Cd(II), Pb(II), Zn(II) and Cr(III) ions, respectively. The relative standard deviations (RSDs) of the method were less than 7.2% for five separate batch experiments for the determination of 30 μg l(-1) of Cd(II), Pb(II), Zn(II) and Cr(III) ions. The sorption capacity of the [(Fe₃O₄-benzoyl isothiocyanate)/MOF] was 175 mg g(-1) for Cd(II), 168 mg g(-1) for Pb(II), 210 mg g(-1) for Zn(II) and 196 mg g(-1) for Cr(III). It was found that the magnetic MOF nanocomposite demonstrated a higher capacity compared with Fe₃O₄-benzoyl isothiocyanate. Finally, the magnetic MOF nanocomposite was successfully applied to the rapid extraction of trace amounts of the heavy metal ions from vegetable samples.

Penetrator role in Mars sample strategy

NASA Technical Reports Server (NTRS)

Boynton, William; Dwornik, Steve; Eckstrom, William; Roalstad, David A.

1988-01-01

The application of the penetrator to a Mars Return Sample Mission (MRSM) has direct advantages to meet science objectives and mission safety. Based on engineering data and work currently conducted at Ball Aerospace Systems Division, the concept of penetrators as scientific instruments is entirely practical. The primary utilization of a penetrator for MRSM would be to optimize the selection of the sample site location and to help in selection of the actual sample to be returned to Earth. It is recognized that the amount of sample to be returned is very limited, therefore the selection of the sample site is critical to the success of the mission. The following mission scenario is proposed. The site selection of a sample to be acquired will be performed by science working groups. A decision will be reached and a set of target priorities established based on data to give geochemical, geophysical and geological information. The first task of a penetrator will be to collect data at up to 4 to 6 possible landing sites. The penetrator can include geophysical, geochemical, geological and engineering instruments to confirm that scientific data requirements at that site will be met. This in situ near real-time data, collected prior to final targeting of the lander, will insure that the sample site is both scientifically valuable and also that it is reachable within limits of the capability of the lander.

Polymer monolithic capillary microextraction on-line coupled with inductively coupled plasma-mass spectrometry for the determination of trace Au and Pd in biological samples

NASA Astrophysics Data System (ADS)

Liu, Xiaolan; He, Man; Chen, Beibei; Hu, Bin

2014-11-01

A novel method based on on-line polymer monolithic capillary microextraction (CME)-inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of trace Au and Pd in biological samples. For this purpose, poly(glycidyl methacrylate-ethylene dimethacrylate) monolith was prepared and functionalized with mercapto groups. The prepared monolith exhibited good selectivity to Au and Pd, and good resistance to strong acid with a long life span. Factors affecting the extraction efficiency of CME, such as sample acidity, sample flow rate, eluent conditions and coexisting ion interference were investigated in detail. Under the optimal conditions, the limits of detection (LODs, 3σ) were 5.9 ng L- 1 for Au and 8.3 ng L- 1 for Pd, and the relative standard deviations (RSDs, c = 50 ng L-1, n = 7) were 6.5% for Au and 1.1% for Pd, respectively. The developed method was successfully applied to the determination of Au and Pd in human urine and serum samples with the recovery in the range of 84-118% for spiked samples. The developed on-line polymer monolithic CME-ICP-MS method has the advantages of rapidity, simplicity, low sample/reagent consumption, high sensitivity and is suitable for the determination of trace Au and Pd in biological samples with limited amount available and complex matrix.

Radioimmunoassays for the serum thymic factor (FTS)

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

Erickson, B.W.; Fok, K.F.; Incefy, G.S.

1987-01-06

This patent describes a radioimmunoassay of serum thymic factor (FTS) in a test sample, comprising: (a) contacting a first aliquot of the sample with anti-FTS antibody, with a known amount of FTS hormone standard and a known amount of radiolabeled FTS analogue; and (b) contacting a second aliquot of the sample with anti-FTS antibody and a known amount of radiolabeled FTS analogue; and (c) measuring the radioactivity of the antigen-antibody complex in each aliquot; and (d) calculating the amount of FTS in the test sample.

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

Li, Liang; Nachtergaele, Sigrid; Seddon, Annela M.

This paper utilizes cyclodextrin-based host-guest chemistry in a microfluidic device to modulate the crystallization of membrane proteins and the process of concentration of membrane protein samples. Methyl-{beta}-cyclodextrin (MBCD) can efficiently capture a wide variety of detergents commonly used for the stabilization of membrane proteins by sequestering detergent monomers. Reaction Center (RC) from Blastochloris viridis was used here as a model system. In the process of concentrating membrane protein samples, MBCD was shown to break up free detergent micelles and prevent them from being concentrated. The addition of an optimal amount of MBCD to the RC sample captured loosely bound detergentmore » from the protein-detergent complex and improved sample homogeneity, as characterized by dynamic light scattering. Using plug-based microfluidics, RC crystals were grown in the presence of MBCD, giving a different morphology and space group than crystals grown without MBCD. The crystal structure of RC crystallized in the presence of MBCD was consistent with the changes in packing and crystal contacts hypothesized for removal of loosely bound detergent. The incorporation of MBCD into a plug-based microfluidic crystallization method allows efficient use of limited membrane protein sample by reducing the amount of protein required and combining sparse matrix screening and optimization in one experiment. The use of MBCD for detergent capture can be expanded to develop cyclodextrin-derived molecules for fine-tuned detergent capture and thus modulate membrane protein crystallization in an even more controllable way.« less

Mesoporous Silica Nanoparticles as an Adsorbent for Preconcentration and Determination of Trace Amount of Nickel in Environmental Samples by Atom Trap Flame Atomic Absorption Spectrometry

NASA Astrophysics Data System (ADS)

Shirkhanloo, H.; Falahnejad, M.; Zavvar Mousavi, H.

2016-01-01

A rapid enrichment method based on solid-phase extraction (SPE) has been established for preconcentration and separation of trace Ni(II) ions in water samples prior to their determination by atom trap flame atomic absorption spectrometry. A column filled with bulky NH2-UVM7 was used as the novel adsorbent. Under optimal conditions, the linear range, limit of detection (LOD), and preconcentration factor (PF) were 3-92 μg/L, 0.8 μg/L, and 100, respectively. The validity of the method was checked by the standard reference material.

Soils, vegetation, and woody debris data from the 2001 Survey Line fire and a comparable unburned site, Tanana Flats region, Alaska

USGS Publications Warehouse

Manies, Kristen L.; Harden, Jennifer W.; Holingsworth, Teresa N.

2014-01-01

This report describes the collection and processing methodologies for samples obtained at two sites within Interior Alaska: (1) a location within the 2001 Survey Line burn, and (2) an unburned location, selected as a control. In 2002 and 2004 U.S. Geological Survey investigators measured soil properties including, but not limited to, bulk density, volumetric water content, carbon content, and nitrogen content from samples obtained from these sites. Stand properties, such as tree density, the amount of woody debris, and understory vegetation, were also measured and are presented in this report.

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

NASA Astrophysics Data System (ADS)

Palonen, V.

2015-12-01

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

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

PubMed

Palonen, V

2015-12-01

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

26 CFR 5.1502-45 - Limitation on losses to amount at risk.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 26 Internal Revenue 14 2010-04-01 2010-04-01 false Limitation on losses to amount at risk. 5.1502... Limitation on losses to amount at risk. (a) In general—(1) Scope. This section applies to a loss of any subsidiary if the common parent's stock meets the stock ownership requirement described in section 465(a)(1...

45 CFR 2530.50 - Is there a limit on the amount of transferred awards a designated individual may receive?

Code of Federal Regulations, 2013 CFR

2013-10-01

... 45 Public Welfare 4 2013-10-01 2013-10-01 false Is there a limit on the amount of transferred... to Public Welfare (Continued) CORPORATION FOR NATIONAL AND COMMUNITY SERVICE TRANSFER OF EDUCATION AWARDS § 2530.50 Is there a limit on the amount of transferred awards a designated individual may receive...

Designing single- and multiple-shell sampling schemes for diffusion MRI using spherical code.

PubMed

Cheng, Jian; Shen, Dinggang; Yap, Pew-Thian

2014-01-01

In diffusion MRI (dMRI), determining an appropriate sampling scheme is crucial for acquiring the maximal amount of information for data reconstruction and analysis using the minimal amount of time. For single-shell acquisition, uniform sampling without directional preference is usually favored. To achieve this, a commonly used approach is the Electrostatic Energy Minimization (EEM) method introduced in dMRI by Jones et al. However, the electrostatic energy formulation in EEM is not directly related to the goal of optimal sampling-scheme design, i.e., achieving large angular separation between sampling points. A mathematically more natural approach is to consider the Spherical Code (SC) formulation, which aims to achieve uniform sampling by maximizing the minimal angular difference between sampling points on the unit sphere. Although SC is well studied in the mathematical literature, its current formulation is limited to a single shell and is not applicable to multiple shells. Moreover, SC, or more precisely continuous SC (CSC), currently can only be applied on the continuous unit sphere and hence cannot be used in situations where one or several subsets of sampling points need to be determined from an existing sampling scheme. In this case, discrete SC (DSC) is required. In this paper, we propose novel DSC and CSC methods for designing uniform single-/multi-shell sampling schemes. The DSC and CSC formulations are solved respectively by Mixed Integer Linear Programming (MILP) and a gradient descent approach. A fast greedy incremental solution is also provided for both DSC and CSC. To our knowledge, this is the first work to use SC formulation for designing sampling schemes in dMRI. Experimental results indicate that our methods obtain larger angular separation and better rotational invariance than the generalized EEM (gEEM) method currently used in the Human Connectome Project (HCP).

Detection and quantification of reactive oxygen species (ROS) in indoor air.

PubMed

Montesinos, V Nahuel; Sleiman, Mohamad; Cohn, Sebastian; Litter, Marta I; Destaillats, Hugo

2015-06-01

Reactive oxygen species (ROS), such as free radicals and peroxides, are environmental trace pollutants potentially associated with asthma and airways inflammation. These compounds are often not detected in indoor air due to sampling and analytical limitations. This study developed and validated an experimental method to sample, identify and quantify ROS in indoor air using fluorescent probes. Tests were carried out simultaneously using three different probes: 2',7'-dichlorofluorescin (DCFH) to detect a broad range of ROS, Amplex ultra Red® (AuR) to detect peroxides, and terephthalic acid (TPA) to detect hydroxyl radicals (HO(•)). For each test, air samples were collected using two impingers in series kept in an ice bath, containing each 10 mL of 50 mM phosphate buffer at pH 7.2. In tests with TPA, that probe was also added to the buffer prior to sampling; in the other two tests, probes and additional reactants were added immediately after sampling. The concentration of fluorescent byproducts was determined fluorometrically. Calibration curves were developed by reacting DCFH and AuR with known amounts of H2O2, and using known amounts of 2-hydroxyterephthalic acid (HTPA) for TPA. Low detection limits (9-13 nM) and quantification limits (18-22 nM) were determined for all three probes, which presented a linear response in the range 10-500 nM for AuR and TPA, and 100-2000 nM for DCFH. High collection efficiency (CE) and recovery efficiency (RE) were observed for DCFH (CE=RE=100%) and AuR (CE=100%; RE=73%) by sampling from a laboratory-developed gas phase H2O2 generator. Interference of co-occurring ozone was evaluated and quantified for the three probes by sampling from the outlet of an ozone generator. The method was demonstrated by sampling air emitted by two portable air cleaners: a strong ozone generator (AC1) and a plasma generator (AC2). High ozone levels emitted by AC1 did not allow for simultaneous determination of ROS levels due to high background levels associated with ozone decomposition in the buffer. However, emitted ROS were quantified at the outlet of AC2 using two of the three probes. With AuR, the concentration of peroxides in air emitted by the air cleaner was 300 ppt of H2O2 equivalents. With TPA, the HO(•) concentration was 47 ppt. This method is best suited to quantify ROS in the presence of low ozone levels. Published by Elsevier B.V.

Methylated purines in urinary stones.

PubMed

Safranow, Krzysztof; Machoy, Zygmunt

2005-08-01

The aim of the study was to measure the content of methylated purines that appear as admixtures in uric acid stones. We analyzed urinary calculi from 48 residents of Western Pomerania who underwent surgery at the urology ward in Szczecin. Stone samples were dissolved in 0.1 mol/L NaOH. Extracts were diluted in 50 mmol/L KH(2)PO(4) and analyzed by reversed-phase HPLC with ultraviolet detection and use of a gradient of methanol concentration and pH. Uric acid was the main component of 9 stones. All 9 showed admixtures of 9 other purine derivatives: endogenous purine breakdown products (xanthine, hypoxanthine, and 2,8-dihydroxyadenine) and exogenous methyl derivatives of uric acid and xanthine (1-, 3-, and 7-methyluric acid; 1,3-dimethyluric acid; and 3- and 7-methylxanthine). Amounts of these purine derivatives ranged from the limit of detection to 12 mg/g of stone weight and showed a strong positive correlation (Spearman rank correlation coefficients, 0.63-0.94) with the uric acid content of the samples. The main methylated purine in the stones was 1-methyluric acid. Urinary purines at concentrations below their saturation limits may coprecipitate in samples supersaturated with uric acid and appear as admixtures in urinary stones. The amount of each purine depends on its average urinary excretion, similarity to the chemical structure of uric acid, and concentration of the latter in the stone. These findings suggest that purines in stones represent a substitutional solid solution with uric acid as solvent. Methylxanthines, which are ubiquitous components of the diet, drugs, and uric acid calculi, may be involved in the pathogenesis of urolithiasis.

Portable X-ray fluorescence for the detection of POP-BFRs in waste plastics.

PubMed

Sharkey, Martin; Abdallah, Mohamed Abou-Elwafa; Drage, Daniel S; Harrad, Stuart; Berresheim, Harald

2018-05-17

The purpose of this study was to establish the efficacy of portable X-ray fluorescence (XRF) instrumentation as a screening tool for a variety of end of life plastics which may contain excess amounts of brominated flame retardants (BFRs), in compliance with European Union (EU) and United Nations Environment Programme (UNEP) legislative limits (low POP concentration limits - LPCLs). 555 samples of waste plastics were collected from eight waste and recycling sites in Ireland, including waste electrical and electronic equipment (WEEE), textiles, polyurethane foams (PUFs), and expanded polystyrene foams. Samples were screened for bromine content, in situ using a Niton™ XL3T GOLDD XRF analyser, the results of which were statistically compared to mass spectrometry (MS)-based measurements of polybrominated diphenyl ethers (PBDEs), hexabromocyclododecane (HBCDD) and tetrabromobisphenol-A (TBBP-A) concentrations in the same samples. Regression between XRF and MS for WEEE samples shows that, despite an overall favourable trend, large deviations occur for a cluster of samples indicative of other bromine-based compounds in some samples; even compensating for false-positives due to background interference from electronic components, XRF tends to over-estimate MS-determined BFR concentrations in the 100 to 10,000 mg kg -1 range. Substantial deviations were additionally found between results for PUFs, textiles and polystyrene samples, with the XRF over-estimating BFR concentrations by a factor of up to 1.9; this is likely due to matrix effects influencing XRF measurements. However, expanded (EPS) and extruded polystyrene (XPS) yielded much more reliable estimations of BFR-content due to a dominance of HBCDD in these materials. XRF proved much more reliable as a "pass/fail" screening tool for LPCL compliance (including a prospective LPCL on Deca-BDE based on REACH). Using a conservative threshold of BFR content exceeding legislative limits (710 mg kg -1 bromine attributed to Penta-BDE), XRF mistakenly identifies only 6 % of samples (34/555) as exceeding legislative limits. Copyright © 2018 Elsevier B.V. All rights reserved.

Rapid and simultaneous detection of Salmonella spp., Escherichia coli O157, and Listeria monocytogenes by magnetic capture hybridization and multiplex real-time PCR.

PubMed

Carloni, Elisa; Rotundo, Luca; Brandi, Giorgio; Amagliani, Giulia

2018-05-25

The application of rapid, specific, and sensitive methods for pathogen detection and quantification is very advantageous in diagnosis of human pathogens in several applications, including food analysis. The aim of this study was the evaluation of a method for the multiplexed detection and quantification of three significant foodborne pathogenic species (Escherichia coli O157, Salmonella spp., and Listeria monocytogenes). The assay combines specific DNA extraction by multiplex magnetic capture hybridization (mMCH) with multiplex real-time PCR. The amplification assay showed linearity in the range 10 6 -10 genomic units (GU)/PCR for each co-amplified species. The sensitivity corresponded to 1 GU/PCR for E. coli O157 and L. monocytogenes, and 10 GU/PCR for Salmonella spp. The immobilization process and the hybrid capture of the MCH showed good efficiency and reproducibility for all targets, allowing the combination in equal amounts of the different nanoparticle types in mMCH. MCH and mMCH efficiencies were similar. The detection limit of the method was 10 CFU in samples with individual pathogens and 10 2  CFU in samples with combination of the three pathogens in unequal amounts (amount's differences of 2 or 3 log). In conclusion, this multiplex molecular platform can be applied to determine the presence of target species in food samples after culture enrichment. In this way, this method could be a time-saving and sensitive tool to be used in routine diagnosis.

Determination of residual nonsteroidal anti-inflammatory drugs in aqueous sample using magnetic nanoparticles modified with cetyltrimethylammonium bromide by high performance liquid chromatography.

PubMed

Khoeini Sharifabadi, Malihe; Saber-Tehrani, Mohammad; Waqif Husain, Syed; Mehdinia, Ali; Aberoomand-Azar, Parviz

2014-01-01

A simple and sensitive solid-phase extraction method for separation and preconcentration of trace amount of four nonsteroidal anti-inflammatory drugs (naproxen, indomethacin, diclofenac, and ibuprofen) using Fe3O4 magnetic nanoparticles modified with cetyltrimethylammonium bromide has been developed. For this purpose, the surface of MNPs was modified with cetyltrimethylammonium bromide (CTAB) as a cationic surfactant. Effects of different parameters influencing the extraction efficiency of drugs including the pH, amount of salt, shaking time, eluent type, the volume of solvent, amount of adsorbent, sample volume, and the time of desorption were investigated and optimized. Methanol has been used as desorption solvent and the extracts were analysed on a reversed-phase octadecyl silica column using 0.02 M phosphate-buffer (pH = 6.02) acetonitrile (65 : 35 v/v) as the mobile phase and the effluents were measured at 202 nm with ultraviolet detector. The relative standard deviation (RSD%) of the method was investigated at three concentrations (25, 50, and 200 ng/mL) and was in the range of 3.98-9.83% (n = 6) for 50 ng/mL. The calibration curves obtained for studied drugs show reasonable linearity (R (2) > 0.99) and the limit of detection (LODs) ranged between 2 and 7 ng/mL. Finally, the proposed method has been effectively employed in extraction and determination of the drugs in biological and environmental samples.

Fidelity and enhanced sensitivity of differential transcription profiles following linear amplification of nanogram amounts of endothelial mRNA

NASA Technical Reports Server (NTRS)

Polacek, Denise C.; Passerini, Anthony G.; Shi, Congzhu; Francesco, Nadeene M.; Manduchi, Elisabetta; Grant, Gregory R.; Powell, Steven; Bischof, Helen; Winkler, Hans; Stoeckert, Christian J Jr;

Combination of artificial neural network and genetic algorithm method for modeling of methylene blue adsorption onto wood sawdust from water samples.

PubMed

Khajeh, Mostafa; Sarafraz-Yazdi, Ali; Natavan, Zahra Bameri

2016-03-01

The aim of this research was to develop a low price and environmentally friendly adsorbent with abundant of source to remove methylene blue (MB) from water samples. Sawdust solid-phase extraction coupled with high-performance liquid chromatography was used for the extraction and determination of MB. In this study, an experimental data-based artificial neural network model is constructed to describe the performance of sawdust solid-phase extraction method for various operating conditions. The pH, time, amount of sawdust, and temperature were the input variables, while the percentage of extraction of MB was the output. The optimum operating condition was then determined by genetic algorithm method. The optimized conditions were obtained as follows: 11.5, 22.0 min, 0.3 g, and 26.0°C for pH of the solution, extraction time, amount of adsorbent, and temperature, respectively. Under these optimum conditions, the detection limit and relative standard deviation were 0.067 μg L(-1) and <2.4%, respectively. The Langmuir and Freundlich adsorption models were applied to describe the isotherm constant and for the removal and determination of MB from water samples. © The Author(s) 2013.

Father involvement moderates the effect of maternal depression during a child's infancy on child behavior problems in kindergarten.

PubMed

Mezulis, Amy H; Hyde, Janet Shibley; Clark, Roseanne

2004-12-01

This research investigated whether father involvement in infancy may reduce or exacerbate the well-established adverse effect of maternal depression during a child's infancy on behavior problems in childhood. In a community sample (N = 350), the authors found that fathers' self-reported parenting styles interacted with the amount of time fathers spent caring for their infants to moderate the longitudinal effect of maternal depression during the child's infancy on children's internalizing, but not externalizing, behaviors. Low to medium amounts of high-warmth father involvement and high amounts of medium- or high-control father involvement at this time were associated with lower child internalizing behaviors. Paternal depression during a child's infancy exacerbated the effect of maternal depression, but this moderating effect was limited to depressed fathers spending medium to high amounts of time caring for their infants. Results emphasize the moderating role fathers may play in reducing or exacerbating the adverse long-term effects of maternal depression during a child's infancy on later child behavior problems. ((c) 2004 APA, all rights reserved).

A Rapid and Accurate Extraction Procedure for Analysing Free Amino Acids in Meat Samples by GC-MS

PubMed Central

Barroso, Miguel A.; Ruiz, Jorge; Antequera, Teresa

2015-01-01

This study evaluated the use of a mixer mill as the homogenization tool for the extraction of free amino acids in meat samples, with the main goal of analyzing a large number of samples in the shortest time and minimizing sample amount and solvent volume. Ground samples (0.2 g) were mixed with 1.5 mL HCl 0.1 M and homogenized in the mixer mill. The final biphasic system was separated by centrifugation. The supernatant was deproteinized, derivatized and analyzed by gas chromatography. This procedure showed a high extracting ability, especially in samples with high free amino acid content (recovery = 88.73–104.94%). It also showed a low limit of detection and quantification (3.8 · 10−4–6.6 · 10−4  μg μL−1 and 1.3 · 10−3–2.2 · 10−2  μg μL−1, resp.) for most amino acids, an adequate precision (2.15–20.15% for run-to-run), and a linear response for all amino acids (R 2 = 0.741–0.998) in the range of 1–100 µg mL−1. Moreover, it takes less time and requires lower amount of sample and solvent than conventional techniques. Thus, this is a cost and time efficient tool for homogenizing in the extraction procedure of free amino acids from meat samples, being an adequate option for routine analysis. PMID:25873963

Neuropsychological impairments in panic disorder: a systematic review.

PubMed

O'Sullivan, Kate; Newman, Emily F

2014-01-01

There is a growing body of literature investigating the neuropsychological profile of panic disorder (PD), some of which suggests potential cognitive dysfunction. This paper systematically reviews the existing literature on neuropsychological performance in PD. PsycINFO, EMBASE, MEDLINE and PsycARTICLES databases were searched to identify articles reporting on neuropsychological function in PD published in English during the time period 1980 to March 2012. 14 studies were identified. There was limited support for impairment in short term memory among individuals with PD, although this was not found across all studies. Overall, the reviewed studies did not support the presence of impairment in other areas of cognitive functioning, including executive function, long term memory, visuospatial or perceptual abilities and working memory. Studies with samples of fewer than 15 participants per group were excluded from this review. A limited amount of research has been published on this topic and small sample sizes (under 25 per group) have been used by many studies. Therefore, the current review is based on a small number of studies with limited power. There is limited evidence of specific neuropsychological impairments in participants with PD. Impairments in short term memory warrant further investigation to establish their relevance to clinical practice. Larger sample sizes and appropriate statistical adjustment for multiple comparisons in future studies is highly recommended. Copyright © 2014 Elsevier B.V. All rights reserved.

Optimizing Sampling Efficiency for Biomass Estimation Across NEON Domains

NASA Astrophysics Data System (ADS)

Abercrombie, H. H.; Meier, C. L.; Spencer, J. J.

2013-12-01

Over the course of 30 years, the National Ecological Observatory Network (NEON) will measure plant biomass and productivity across the U.S. to enable an understanding of terrestrial carbon cycle responses to ecosystem change drivers. Over the next several years, prior to operational sampling at a site, NEON will complete construction and characterization phases during which a limited amount of sampling will be done at each site to inform sampling designs, and guide standardization of data collection across all sites. Sampling biomass in 60+ sites distributed among 20 different eco-climatic domains poses major logistical and budgetary challenges. Traditional biomass sampling methods such as clip harvesting and direct measurements of Leaf Area Index (LAI) involve collecting and processing plant samples, and are time and labor intensive. Possible alternatives include using indirect sampling methods for estimating LAI such as digital hemispherical photography (DHP) or using a LI-COR 2200 Plant Canopy Analyzer. These LAI estimations can then be used as a proxy for biomass. The biomass estimates calculated can then inform the clip harvest sampling design during NEON operations, optimizing both sample size and number so that standardized uncertainty limits can be achieved with a minimum amount of sampling effort. In 2011, LAI and clip harvest data were collected from co-located sampling points at the Central Plains Experimental Range located in northern Colorado, a short grass steppe ecosystem that is the NEON Domain 10 core site. LAI was measured with a LI-COR 2200 Plant Canopy Analyzer. The layout of the sampling design included four, 300 meter transects, with clip harvests plots spaced every 50m, and LAI sub-transects spaced every 10m. LAI was measured at four points along 6m sub-transects running perpendicular to the 300m transect. Clip harvest plots were co-located 4m from corresponding LAI transects, and had dimensions of 0.1m by 2m. We conducted regression analyses with LAI and clip harvest data to determine whether LAI can be used as a suitable proxy for aboveground standing biomass. We also compared optimal sample sizes derived from LAI data, and clip-harvest data from two different size clip harvest areas (0.1m by 1m vs. 0.1m by 2m). Sample sizes were calculated in order to estimate the mean to within a standardized level of uncertainty that will be used to guide sampling effort across all vegetation types (i.e. estimated within × 10% with 95% confidence). Finally, we employed a Semivariogram approach to determine optimal sample size and spacing.

Plutonium and uranium determination in environmental samples: combined solvent extraction-liquid scintillation method.

PubMed

McDowell, W J; Farrar, D T; Billings, M R

1974-12-01

A method for the determination of uranium and plutonium by a combined high-resolution liquid scintillation-solvent extraction method is presented. Assuming a sample count equal to background count to be the detection limit, the lower detection limit for these and other alpha-emitting nuclides is 1.0 dpm with a Pyrex sample tube, 0.3 dpm with a quartz sample tube using present detector shielding or 0.02 d.p.m. with pulse-shape discrimination. Alpha-counting efficiency is 100%. With the counting data presented as an alpha-energy spectrum, an energy resolution of 0.2-0.3 MeV peak half-width and an energy identification to +/-0.1 MeV are possible. Thus, within these limits, identification and quantitative determination of a specific alpha-emitter, independent of chemical separation, are possible. The separation procedure allows greater than 98% recovery of uranium and plutonium from solution containing large amounts of iron and other interfering substances. In most cases uranium, even when present in 10(8)-fold molar ratio, may be quantitatively separated from plutonium without loss of the plutonium. Potential applications of this general analytical concept to other alpha-counting problems are noted. Special problems associated with the determination of plutonium in soil and water samples are discussed. Results of tests to determine the pulse-height and energy-resolution characteristics of several scintillators are presented. Construction of the high-resolution liquid scintillation detector is described.

Application of 1013 ohm Faraday cup current amplifiers for boron isotopic analyses by solution mode and laser ablation multicollector inductively coupled plasma mass spectrometry.

PubMed

Lloyd, Nicholas S; Sadekov, Aleksey Yu; Misra, Sambuddha

2018-01-15

Boron isotope ratios (δ 11 B values) are used as a proxy for seawater paleo-pH, amongst several other applications. The analytical precision can be limited by the detection of low intensity ion beams from limited sample amounts. High-gain amplifiers offer improvements in signal/noise ratio and can be used to increase measurement precision and reduce sample amounts. 10 13 ohm amplifier technology has previously been applied to several radiogenic systems, but has thus far not been applied to non-traditional stable isotopes. Here we apply 10 13 ohm amplifier technology for the measurement of boron isotope ratios using solution mode MC-ICP-MS and laser ablation mode (LA-)MC-ICP-MS techniques. Precision is shown for reference materials as well as for low-volume foraminifera samples. The baseline uncertainty for a 0.1 pA 10 B + ion beam is reduced to <0.1 ‰ for a typical measurement period. The external precision is better than 0.2 ‰ (2SD) for δ 11 B measurements for solution samples containing as little as 0.8 ng total boron. For in situ microanalyses with LA-MC-ICP-MS, the external precision of 11 B/ 10 B from an in-house calcite standard was 1 ‰ (2SD) for individual spot analyses, and 0.3 ‰ for the mean of ≥10 replicate spot analyses. 10 13 ohm amplifier technology is demonstrated to offer advantages for the determination of δ 11 B values by both MC-ICP-MS and LA-MC-ICP-MS for small samples of biogenic carbonates, such as foraminifera shells. 10 13 ohm amplifier technology will also be of benefit to other non-traditional stable isotope measurements. Copyright © 2017 John Wiley & Sons, Ltd.

Paper-Based MicroRNA Expression Profiling from Plasma and Circulating Tumor Cells.

PubMed

Leong, Sai Mun; Tan, Karen Mei-Ling; Chua, Hui Wen; Huang, Mo-Chao; Cheong, Wai Chye; Li, Mo-Huang; Tucker, Steven; Koay, Evelyn Siew-Chuan

2017-03-01

Molecular characterization of circulating tumor cells (CTCs) holds great promise for monitoring metastatic progression and characterizing metastatic disease. However, leukocyte and red blood cell contamination of routinely isolated CTCs makes CTC-specific molecular characterization extremely challenging. Here we report the use of a paper-based medium for efficient extraction of microRNAs (miRNAs) from limited amounts of biological samples such as rare CTCs harvested from cancer patient blood. Specifically, we devised a workflow involving the use of Flinders Technology Associates (FTA) ® Elute Card with a digital PCR-inspired "partitioning" method to extract and purify miRNAs from plasma and CTCs. We demonstrated the sensitivity of this method to detect miRNA expression from as few as 3 cancer cells spiked into human blood. Using this method, background miRNA expression was excluded from contaminating blood cells, and CTC-specific miRNA expression profiles were derived from breast and colorectal cancer patients. Plasma separated out during purification of CTCs could likewise be processed using the same paper-based method for miRNA detection, thereby maximizing the amount of patient-specific information that can be derived from a single blood draw. Overall, this paper-based extraction method enables an efficient, cost-effective workflow for maximized recovery of small RNAs from limited biological samples for downstream molecular analyses. © 2016 American Association for Clinical Chemistry.

Development of a mercury detection kit based on melamine-functionalized gold nanoparticles.

PubMed

Liu, Guoyan; Ren, Huipeng; Guan, Yuyu; Dai, Ronghua; Chai, Chunyan

2015-01-01

A fast and simple mercury detection kit was developed based on melamine-functionalized gold nanoparticles (GNPs). The detection kit contained reagent 1 (GNPs), reagent 2 (melanine), a reaction cuvette with four separated cells, a colorimetric card and a plastic pipette. The GNPs were prepared by a citrate reduction of HAuCl4. A proper amount of melamine was applied to functionalize the GNPs. The complex reaction took place in the present of Hg(2+) in the test samples, leading to the combination of Hg(2+) with the C=N group of melamine located on the surface of the GNPs. This reaction resulted in damage to the stability of colloid gold, and the aggregation of GNPs occurred. Different color changes (from claret-red to lilac, purple and plum) were displayed with different concentrations of Hg(2+) in the test samples. It was very easy and convenient to determine the amount of mercury ion by the naked eye. The advantages of this methodology are listed as follows: a short detecting time (within 10 min), a high specificity (no significant interference was indicated upon adding a certain amount of Cu(2+), Pb(2+), Zn(2+), Mg(2+), Cd(2+) and Fe(2+)), high sensitivity with a detection limit of 0.01 mg L(-1) , easy operation and practical on-site use.

Intelligent Sampling of Hazardous Particle Populations in Resource-Constrained Environments

NASA Astrophysics Data System (ADS)

McCollough, J. P.; Quinn, J. M.; Starks, M. J.; Johnston, W. R.

2017-10-01

Sampling of anomaly-causing space environment drivers is necessary for both real-time operations and satellite design efforts, and optimizing measurement sampling helps minimize resource demands. Relating these measurements to spacecraft anomalies requires the ability to resolve spatial and temporal variability in the energetic charged particle hazard of interest. Here we describe a method for sampling particle fluxes informed by magnetospheric phenomenology so that, along a given trajectory, the variations from both temporal dynamics and spatial structure are adequately captured while minimizing oversampling. We describe the coordinates, sampling method, and specific regions and parameters employed. We compare resulting sampling cadences with data from spacecraft spanning the regions of interest during a geomagnetically active period, showing that the algorithm retains the gross features necessary to characterize environmental impacts on space systems in diverse orbital regimes while greatly reducing the amount of sampling required. This enables sufficient environmental specification within a resource-constrained context, such as limited telemetry bandwidth, processing requirements, and timeliness.

Fabrication and evaluation of magnetic activated carbon as adsorbent for ultrasonic assisted magnetic solid phase dispersive extraction of bisphenol A from milk prior to high performance liquid chromatographic analysis with ultraviolet detection.

PubMed

Filippou, Olga; Deliyanni, Eleni A; Samanidou, Victoria F

2017-01-06

In the present study, the impregnation of a micro - meso porous activated carbon with magnetite (Fe 3 O 4 ) was successfully achieved by sonication and the magnetic activated carbon prepared (Bmi) was evaluated as a new adsorbent for ultrasonic assisted magnetic solid phase dispersive extraction of Bisphenol A (BPA) from cow milk and human breast milk samples, prior to the determination by HPLC with UV detection. The prepared Bmi was characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). The effect of pH on adsorption, initial concentration, contact time and desorption were studied. The main experimental parameters influencing extraction efficiency of BPA, such as type and amount of the adsorbent, sample amount, type of desorption solvent, time of adsorption and desorption, type of precipitation solvent, were investigated and optimized. Under the optimal extraction conditions the absolute recovery of BPA was 81% and 95% in cow milk and human breast milk samples, respectively. Good linearity was observed in the investigated concentration range of 2.5μgkg -1 -5000μgkg -1 (R 2 =0.9997). Limit of detection (LOD) was 0.75μgL -1 , which is in accordance with the specific migration limit (SML) established by the European Union, and limit of quantification (LOQ) was 2.5μgL -1 . Within-day and between-day recoveries ranged from 91.4% to 98.6% and 89.1% to 99.4% respectively and the RSDs were less than 3.7%. Due to the excellent magnetic behavior of Bmi the proposed method was shown to be simple and rapid. Besides these, this method is sensitive, low cost, efficient and environmentally friendly. Copyright © 2016 Elsevier B.V. All rights reserved.

Rapid screening of heavy metals and trace elements in environmental samples using portable X-ray fluorescence spectrometer, A comparative study

PubMed Central

McComb, Jacqueline Q.; Rogers, Christian; Han, Fengxiang X.; Tchounwou, Paul B.

2014-01-01

With industrialization, great amounts of trace elements and heavy metals have been excavated and released on the surface of the earth and dissipated into the environments. Rapid screening technology for detecting major and trace elements as well as heavy metals in variety of environmental samples is most desired. The objectives of this study were to determine the detection limits, accuracy, repeatability and efficiency of a X-ray fluorescence spectrometer (Niton XRF analyzer) in comparison with the traditional analytical methods, inductively coupled plasma optical emission spectrometer (ICP-OES) and inductively coupled plasma optical emission spectrometer (ICP-MS) in screening of major and trace elements of environmental samples including estuary soils and sediments, contaminated soils, and biological samples. XRF is a fast and non-destructive method in measuring the total concentration of multi--elements simultaneously. Contrary to ICP-OES and ICP-MS, XRF analyzer is characterized by the limited preparation required for solid samples, non-destructive analysis, increased total speed and high throughout, the decreased production of hazardous waste and the low running costs as well as multi-elemental determination and portability in the fields. The current comparative study demonstrates that XRF is a good rapid non-destructive method for contaminated soils, sediments and biological samples containing higher concentrations of major and trace elements. Unfortunately, XRF does not have sensitive detection limits of most major and trace elements as ICP-OES or ICP-MS but it may serve as a rapid screening tool for locating hot spots of uncontaminated field soils and sediments. PMID:25861136

Leaching behaviour of bottom ash from RDF high-temperature gasification plants

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

Gori, M., E-mail: manuela.gori@dicea.unifi.it; Pifferi, L.; Sirini, P.

2011-07-15

This study investigated the physical properties, the chemical composition and the leaching behaviour of two bottom ash (BA) samples from two different refuse derived fuel high-temperature gasification plants, as a function of particle size. The X-ray diffraction patterns showed that the materials contained large amounts of glass. This aspect was also confirmed by the results of availability and ANC leaching tests. Chemical composition indicated that Fe, Mn, Cu and Cr were the most abundant metals, with a slight enrichment in the finest fractions. Suitability of samples for inert waste landfilling and reuse was evaluated through the leaching test EN 12457-2.more » In one sample the concentration of all metals was below the limit set by law, while limits were exceeded for Cu, Cr and Ni in the other sample, where the finest fraction showed to give the main contribution to leaching of Cu and Ni. Preliminary results of physical and geotechnical characterisation indicated the suitability of vitrified BA for reuse in the field of civil engineering. The possible application of a size separation pre-treatment in order to improve the chemical characteristics of the materials was also discussed.« less

Method validation using weighted linear regression models for quantification of UV filters in water samples.

PubMed

da Silva, Claudia Pereira; Emídio, Elissandro Soares; de Marchi, Mary Rosa Rodrigues

2015-01-01

This paper describes the validation of a method consisting of solid-phase extraction followed by gas chromatography-tandem mass spectrometry for the analysis of the ultraviolet (UV) filters benzophenone-3, ethylhexyl salicylate, ethylhexyl methoxycinnamate and octocrylene. The method validation criteria included evaluation of selectivity, analytical curve, trueness, precision, limits of detection and limits of quantification. The non-weighted linear regression model has traditionally been used for calibration, but it is not necessarily the optimal model in all cases. Because the assumption of homoscedasticity was not met for the analytical data in this work, a weighted least squares linear regression was used for the calibration method. The evaluated analytical parameters were satisfactory for the analytes and showed recoveries at four fortification levels between 62% and 107%, with relative standard deviations less than 14%. The detection limits ranged from 7.6 to 24.1 ng L(-1). The proposed method was used to determine the amount of UV filters in water samples from water treatment plants in Araraquara and Jau in São Paulo, Brazil. Copyright © 2014 Elsevier B.V. All rights reserved.

Extraction of trace amounts of mercury with sodium dodecyle sulphate-coated magnetite nanoparticles and its determination by flow injection inductively coupled plasma-optical emission spectrometry.

PubMed

Faraji, Mohammad; Yamini, Yadollah; Rezaee, Mohammad

2010-05-15

A new method for solid-phase extraction and preconcentration of trace amounts Hg(II) from environmental samples was developed by using sodium dodecyle sulphate-coated magnetite nanoparticles (SDS-coated Fe(3)O(4) NPs) as a new extractant. The procedure is based on the adsorption of the analyte, as mercury-Michler's thioketone [Hg(2)(TMK)(4)](2+) complex on the negatively charged surface of the SDS-coated Fe(3)O(4) NPs and then elution of the preconcentrated mercury from the surface of the SDS-coated Fe(3)O(4) NPs prior to its determination by flow injection inductively coupled plasma-optical emission spectrometry. The effects of pH, TMK concentration, SDS and Fe(3)O(4) NPs amounts, eluent type, sample volume and interfering ions on the recovery of the analyte were investigated. Under optimized conditions, the calibration curve was linear in the range of 0.2-100ngmL(-1) with r(2)=0.9994 (n=8). The limit of detection for Hg(II) determination was 0.04ngmL(-1). Also, relative standard deviation (R.S.D.) for the determination of 2 and 50ngmL(-1) of Hg(II) was 5.2 and 4.7% (n=6), respectively. Due to the quantitative extraction of Hg(II) from 1000mL of the sample solution an enhancement factor as large as 1230-fold can be obtained. The proposed method has been validated using a certified reference materials, and also the method has been applied successfully for the determination of Hg(II) in aqueous samples.

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

USGS Publications Warehouse

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

2004-01-01

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

42 CFR 410.155 - Outpatient mental health treatment limitation.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 42 Public Health 2 2010-10-01 2010-10-01 false Outpatient mental health treatment limitation. 410... § 410.155 Outpatient mental health treatment limitation. (a) Limitation. For services subject to the... Medicare payment amount and the patient liability amounts for outpatient mental health services subject to...

42 CFR 410.155 - Outpatient mental health treatment limitation.

Code of Federal Regulations, 2014 CFR

2014-10-01

... 42 Public Health 2 2014-10-01 2014-10-01 false Outpatient mental health treatment limitation. 410... § 410.155 Outpatient mental health treatment limitation. (a) Limitation. For services subject to the... Medicare payment amount and the patient liability amounts for outpatient mental health services subject to...

Development of a one-step immunochromatographic strip test for the detection of sennosides A and B.

PubMed

Putalun, Waraporn; Morinaga, Osamu; Tanaka, Hiroyuki; Shoyama, Yukihiro

2004-01-01

An immunochromatographic strip test was developed to detect sennoside A (1) and sennoside B (2) using anti-1 and anti-2 monoclonal antibodies. The qualitative assay was based on a competitive immunoassay in which the detector reagent consisted of colloidal gold particles coated with the respective sennoside antibodies. The capture reagents were 1- and 2-human serum albumin (HSA) conjugates immobilised on a nitrocellulose membrane on the test strip. The sample containing 1 and 2, together with detector reagent, passed over the zone where the capture reagents had been immobilised. The analytes in the sample competed for binding to the limited amount of antibodies in the detector reagent with the immobilised 1- and 2-HSA conjugates on the membrane and hence positive samples showed no colour in the capture spot zone. Detection limits for the strip test were 125 ng/mL for both sennosides. The assay system is useful as a rapid and simple screening method for the detection of 1 and 2 in plants, drugs and body fluids.

Selective precipitation of potassium in seawater samples for improving the sensitivity of plain γ-ray spectrometry

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

Ferrante, Marco, E-mail: marco.ferrante@lngs.infn.it; De Angelis, Francesco, E-mail: francesco.deangelis@univaq.it; Nisi, Stefano, E-mail: stefano.nisi@lngs.infn.it

2015-08-17

An analytical method is presented to reduce the amount of {sup 40}K in sea water samples, in order to lower its interference in γ-ray analysis below 1.4 MeV due to the Compton continuum. Sodium tetraphenylborate was used to successfully precipitate {sup 40}K in the samples. A custom procedure for precipitation of potassium was developed and it was evaluated for its selectivity, reproducibility and efficiency, using conventional analytical techniques such as atomic absorption spectrophotometry and inductively coupled plasma mass spectrometry (ICP-MS). This work has shown that the selective precipitation of potassium with sodium tetraphenylborate has led to a decrease of detectionmore » limit of radio nuclides such as {sup 238}U, {sup 226}Ra, {sup 228}Ra, {sup 137}Cs, {sup 134}Cs, {sup 133}I, {sup 134}I, {sup 60}Co in γ-analysis. In particular, the detection limit for nuclides with emissions in the energy window energy below 1400 keV is improved by almost one order of magnitude.« less

Magnetic porous carbon derived from a bimetallic metal-organic framework for magnetic solid-phase extraction of organochlorine pesticides from drinking and environmental water samples.

PubMed

Liu, Yaxi; Gao, Zongjun; Wu, Ri; Wang, Zhenhua; Chen, Xiangfeng; Chan, T-W Dominic

2017-01-06

In this work, magnetic porous carbon material derived from a bimetallic metal-organic framework was explored as an adsorbent for magnetic solid-phase extraction of organochlorine pesticides (OCPs). The synthesized porous carbon possessed a high specific surface area and magnetization saturation. The OCPs in the samples were quantified using gas chromatography coupled with a triple quadrupole mass spectrometer. The experimental parameters, including the desorption solvent and conditions, amount of adsorbent, extraction time, extraction temperature, and ionic strength of the solution, were optimized. Under optimal conditions, the developed method displayed good linearity (r>0.99) within the concentration range of 2-500ngL -1 . Low limits of detection (0.39-0.70ngL -1 , signal-to-noise ratio=3:1) and limits of quantification (1.45-2.0ngL -1 , signal-to-noise ratio=10:1) as well as good precision (relative standard deviation<10%) were also obtained. The developed method was applied in the analysis of OCPs in drinking and environmental water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Quantification of the xenoestrogens 4-tert.-octylphenol and bisphenol A in water and in fish tissue based on microwave assisted extraction, solid-phase extraction and liquid chromatography-mass spectrometry.

PubMed

Pedersen, S N; Lindholst, C

1999-12-09

Extraction methods were developed for quantification of the xenoestrogens 4-tert.-octylphenol (tOP) and bisphenol A (BPA) in water and in liver and muscle tissue from the rainbow trout (Oncorhynchus mykiss). The extraction of tOP and BPA from tissue samples was carried out using microwave-assisted solvent extraction (MASE) followed by solid-phase extraction (SPE). Water samples were extracted using only SPE. For the quantification of tOP and BPA, liquid chromatography mass spectrometry (LC-MS) equipped with an atmospheric pressure chemical ionisation interface (APCI) was applied. The combined methods for tissue extraction allow the use of small sample amounts of liver or muscle (typically 1 g), low volumes of solvent (20 ml), and short extraction times (25 min). Limits of quantification of tOP in tissue samples were found to be approximately 10 ng/g in muscle and 50 ng/g in liver (both based on 1 g of fresh tissue). The corresponding values for BPA were approximately 50 ng/g in both muscle and liver tissue. In water, the limit of quantification for tOP and BPA was approximately 0.1 microg/l (based on 100 ml sample size).

[Trace analysis of aristolochic acid A].

PubMed

Liu, Yalin; Gao, Huimin; Wang, Zhimin; Zhang, Qiwei

2010-12-01

A HPLC method for limit detection of aristolochic acid A in the Chinese herbs containing aristolochic acid or suspected-containing aristolochic acid and their preparations was established. The samples were analyzed on an Alltima C18 column eluted with methanol-water-acetic acid (68:32:1.5) as the mobile phase. Flow rate was at 1.0 mL x min(-1) and the detection wavelength was at 390 nm. The calibration curve was linear over the range from 0.016 to 0.51 g (r = 0.9993) and LOD was 4 ng. The average recovery was 101.2% with RSD of 2.01%. The procedures of sample preparation were systematically investigated. The contents of aristolochic acid A in Radix et Rhizoma Asari bought from market or drugstore were fluctuated from 3.1 to 26.6 microg x g(-1) and 3 of 11 samples accorded with the quality requirement of current Chinese Pharmacopoeia. Among 15 batches samples of Chinese medicaments, only one sample was found to contain aristolochic acid A. The present investigation shows that the method is sensitive and repeatable and it could be used for the limit detection of aristolochic acid A in the Chinese herbal medicines containing trace amount of aristolochic acid A or suspected-containing aristolochic acid A and their preparations.

Lowering the quantification limit of the QubitTM RNA HS assay using RNA spike-in.

PubMed

Li, Xin; Ben-Dov, Iddo Z; Mauro, Maurizio; Williams, Zev

2015-05-06

RNA quantification is often a prerequisite for most RNA analyses such as RNA sequencing. However, the relatively low sensitivity and large sample consumption of traditional RNA quantification methods such as UV spectrophotometry and even the much more sensitive fluorescence-based RNA quantification assays, such as the Qubit™ RNA HS Assay, are often inadequate for measuring minute levels of RNA isolated from limited cell and tissue samples and biofluids. Thus, there is a pressing need for a more sensitive method to reliably and robustly detect trace levels of RNA without interference from DNA. To improve the quantification limit of the Qubit™ RNA HS Assay, we spiked-in a known quantity of RNA to achieve the minimum reading required by the assay. Samples containing trace amounts of RNA were then added to the spike-in and measured as a reading increase over RNA spike-in baseline. We determined the accuracy and precision of reading increases between 1 and 20 pg/μL as well as RNA-specificity in this range, and compared to those of RiboGreen(®), another sensitive fluorescence-based RNA quantification assay. We then applied Qubit™ Assay with RNA spike-in to quantify plasma RNA samples. RNA spike-in improved the quantification limit of the Qubit™ RNA HS Assay 5-fold, from 25 pg/μL down to 5 pg/μL while maintaining high specificity to RNA. This enabled quantification of RNA with original concentration as low as 55.6 pg/μL compared to 250 pg/μL for the standard assay and decreased sample consumption from 5 to 1 ng. Plasma RNA samples that were not measurable by the Qubit™ RNA HS Assay were measurable by our modified method. The Qubit™ RNA HS Assay with RNA spike-in is able to quantify RNA with high specificity at 5-fold lower concentration and uses 5-fold less sample quantity than the standard Qubit™ Assay.

Food safety aspects of primary environmental contaminants in the edible tissues of roe deer (Capreolus capreolus).

PubMed

Lehel, József; Zwillinger, Dóra; Bartha, András; Lányi, Katalin; Laczay, Péter

2017-11-01

The muscle, liver, kidney and fat samples of 20 roe deer of both sexes originating from a hunting area in central Hungary were investigated for the presence of heavy metals such as As, Cd, Hg and Pb, and their contents were evaluated for possible health risk to consumers. Both As and Hg were found at a level below the limit of detection (< 0.5 mg/kg wet weight) in all samples. The median of the measured Cd concentrations was significantly higher in both the kidney and the liver (p = 0.0011) of bucks than of does. In bucks, Cd levels exceeded the respective maximum limits laid down in the European legislation in four kidney and three muscle samples, whereas in does, the measured concentrations were below the respective limits in all samples. The detected amounts of Pb exceeded the maximum limits in the kidney of one buck and eight does, in the liver of two bucks and six does, in the muscle of six bucks and nine does, whereas in all fat tissues of both bucks and does. The concentration of Pb (p = 0.02) was significantly greater in the kidney of does compared to roebucks. Based on data obtained from the present study, the consumption of organs and tissues of the investigated roe deer could be objectionable from food-toxicological point of view and may pose risk to the high consumers of wild game due to their cadmium and lead contents.

The limit of detection for explosives in spectroscopic differential reflectometry

NASA Astrophysics Data System (ADS)

Dubroca, Thierry; Vishwanathan, Karthik; Hummel, Rolf E.

2011-05-01

In the wake of recent terrorist attacks, such as the 2008 Mumbai hotel explosion or the December 25th 2009 "underwear bomber", our group has developed a technique (US patent #7368292) to apply differential reflection spectroscopy to detect traces of explosives. Briefly, light (200-500 nm) is shone on a surface such as a piece of luggage at an airport. Upon reflection, the light is collected with a spectrometer combined with a CCD camera. A computer processes the data and produces in turn a differential reflection spectrum involving two adjacent areas of the surface. This differential technique is highly sensitive and provides spectroscopic data of explosives. As an example, 2,4,6, trinitrotoluene (TNT) displays strong and distinct features in differential reflectograms near 420 nm. Similar, but distinctly different features are observed for other explosives. One of the most important criteria for explosive detection techniques is the limit of detection. This limit is defined as the amount of explosive material necessary to produce a signal to noise ratio of three. We present here, a method to evaluate the limit of detection of our technique. Finally, we present our sample preparation method and experimental set-up specifically developed to measure the limit of detection for our technology. This results in a limit ranging from 100 nano-grams to 50 micro-grams depending on the method and the set-up parameters used, such as the detector-sample distance.

Towards a minimally invasive sampling tool for high resolution tissue analytical mapping

NASA Astrophysics Data System (ADS)

Gottardi, R.

2015-09-01

Multiple spatial mapping techniques of biological tissues have been proposed over the years, but all present limitations either in terms of resolution, analytical capacity or invasiveness. Ren et al (2015 Nanotechnology 26 284001) propose in their most recent work the use of a picosecond infrared laser (PIRL) under conditions of ultrafast desorption by impulsive vibrational excitation (DIVE) to extract small amounts of cellular and molecular components, conserving their viability, structure and activity. The PIRL DIVE technique would then work as a nanobiopsy with minimal damage to the surrounding tissues, which could potentially be applied for high resolution local structural characterization of tissues in health and disease with the spatial limit determined by the laser focus.

Correlation analysis between sulphate content and leaching of sulphates in recycled aggregates from construction and demolition wastes.

PubMed

Barbudo, Auxi; Galvín, Adela P; Agrela, Francisco; Ayuso, Jesús; Jiménez, Jose Ramón

2012-06-01

In some recycled aggregates applications, such as component of new concrete or roads, the total content of soluble sulphates should be measured and controlled. Restrictions are usually motivated by the resistance or stability of the new structure, and in most cases, structural concerns can be remedied by the use of techniques such as sulphur-resistant cements. However, environmental risk assessment from recycling and reuse construction products is often forgotten. The purpose of this study is to analyse the content of soluble sulphate on eleven recycled aggregates and six samples prepared in laboratory by the addition of different gypsum percentages. As points of reference, two natural aggregates were tested. An analysis of the content of the leachable amount of heavy metals regulated by European regulation was included. As a result, the correlation between solubility and leachability data allow suggest a limiting gypsum amount of 4.4% on recycled aggregates. This limit satisfies EU Landfill Directive criteria, which is currently used as reference by public Spanish Government for recycled aggregates in construction works. Copyright © 2012 Elsevier Ltd. All rights reserved.

26 CFR 1.179-2 - Limitations on amount subject to section 179 election.

Code of Federal Regulations, 2010 CFR

2010-04-01

... trade or business and interest from working capital of the trade or business. Taxable income derived... aggregate amount of partnership items, deductions and losses are treated as negative income. Any limitation... aggregate amount of S corporation items, deductions and losses are treated as negative income. Any...

42 CFR 423.336 - Risk-sharing arrangements.

Code of Federal Regulations, 2010 CFR

2010-10-01

... range as follows: (A) First threshold lower limit. The first threshold lower limit of the corridor is equal to— (1) The target amount for the plan; minus (2) An amount equal to the first threshold risk.... (B) Second threshold lower limit. The second threshold lower limit of the corridor is equal to— (1...

Microvolume Protein Concentration Determination using the NanoDrop 2000c Spectrophotometer

PubMed Central

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

2009-01-01

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

Process control of apple winemaking by low-resolution gas-phase Fourier-transform infrared spectroscopy.

PubMed

Ahro, M; Hakala, M; Kauppinen, J; Kallio, H

2001-10-01

Four apple wine fermentation processes have been observed by means of direct-inlet gas-phase FTIR spectroscopy. The apple juice concentrates were each fermented by two species of Saccharomyces cerevisiae starters, and the experiment was repeated. The development of the concentrations of 1-propanol, 4-methylpyridine, acetaldehyde, acetic acid, and ethyl acetate was monitored. Two different sampling methods were used--static headspace and direct injection of the must. The performance of the FTIR method is limited by the high ethanol concentration. It can be mathematically proven that the amount of sample can be selected so that any distortion due to ethanol is minimized. Headspace GC-MS was used for preliminary compound identification.

Headspace Solid Phase Micro Extraction Gas Chromatographic Determination of Fenthion in Human Serum

PubMed Central

Kasiotis, Konstantinos M.; Souki, Helen; Tsakirakis, Angelos N.; Carageorgiou, Haris; Theotokatos, Spiridon A.; Haroutounian, Serkos A.; Machera, Kyriaki

2008-01-01

A simple and effective analytical procedure was developed for the determination of fenthion residues in human serum samples. The sample treatment was performed using the headspace solid-phase micro extraction with polyacrylate fiber, which has the advantage to require low amount of serum (1 mL) without tedious pre-treatment. The quantification of fenthion was carried out by gas chromatography-mass spectrometry and the recoveries ranged from 79 to 104% at two spiking levels for 6 replicates. Detection and quantification limits were calculated as 1.51 and 4.54 ng/mL of serum respectively. Two fenthion metabolites fenoxon and fenthion–sulfoxide were also identified. PMID:19325792

Analytical determination of selenium in medical samples, staple food and dietary supplements by means of total reflection X-ray fluorescence spectroscopy

NASA Astrophysics Data System (ADS)

Stosnach, Hagen

2010-09-01

Selenium is essential for many aspects of human health and, thus, the object of intensive medical research. This demands the use of analytical techniques capable of analysing selenium at low concentrations with high accuracy in widespread matrices and sometimes smallest sample amounts. In connection with the increasing importance of selenium, there is a need for rapid and simple on-site (or near-to-site) selenium analysis in food basics like wheat at processing and production sites, as well as for the analysis of this element in dietary supplements. Common analytical techniques like electrothermal atomic absorption spectroscopy (ETAAS) and inductively-coupled plasma mass spectrometry (ICP-MS) are capable of analysing selenium in medical samples with detection limits in the range from 0.02 to 0.7 μg/l. Since in many cases less complicated and expensive analytical techniques are required, TXRF has been tested regarding its suitability for selenium analysis in different medical, food basics and dietary supplement samples applying most simple sample preparation techniques. The reported results indicate that the accurate analysis of selenium in all sample types is possible. The detection limits of TXRF are in the range from 7 to 12 μg/l for medical samples and 0.1 to 0.2 mg/kg for food basics and dietary supplements. Although this sensitivity is low compared to established techniques, it is sufficient for the physiological concentrations of selenium in the investigated samples.

Efficient Sample Tracking With OpenLabFramework

PubMed Central

List, Markus; Schmidt, Steffen; Trojnar, Jakub; Thomas, Jochen; Thomassen, Mads; Kruse, Torben A.; Tan, Qihua; Baumbach, Jan; Mollenhauer, Jan

2014-01-01

The advance of new technologies in biomedical research has led to a dramatic growth in experimental throughput. Projects therefore steadily grow in size and involve a larger number of researchers. Spreadsheets traditionally used are thus no longer suitable for keeping track of the vast amounts of samples created and need to be replaced with state-of-the-art laboratory information management systems. Such systems have been developed in large numbers, but they are often limited to specific research domains and types of data. One domain so far neglected is the management of libraries of vector clones and genetically engineered cell lines. OpenLabFramework is a newly developed web-application for sample tracking, particularly laid out to fill this gap, but with an open architecture allowing it to be extended for other biological materials and functional data. Its sample tracking mechanism is fully customizable and aids productivity further through support for mobile devices and barcoded labels. PMID:24589879

Fatty acid profile of edible oils and fats consumed in India.

PubMed

Dorni, Charles; Sharma, Paras; Saikia, Gunendra; Longvah, T

2018-01-01

A total 320 samples of edible oils and fats (Oils-236; Vanaspati- 45; Ghee-39) were sampled from 107 sampling sites in India and were evaluated for their fatty acid profile. This is the first comprehensive report on fatty acids profile of fats & oil commonly consumed in India. Every variety of edible oil showed its own unique fatty acid profile with significant variation within each individual fatty acid. Pure safflower oil exhibited the highest total TPUFA (76.78%) while the highest TSFA was noticed for coconut oil (90.84%). High level of erucic acid in the range of 48.5 to 54.2% was observed in mustard oil.. Groundnut and rice bran oils showed TPUFA/TSFA ratio closer to WHO recommended value. Several vanaspati samples exhibited trans fatty acid beyond the permitted limit while trace amount of the same was also detected in ghee. Copyright © 2017. Published by Elsevier Ltd.

Screening and confirmatory methods for the analysis of macrocyclic lactone mycotoxins by CE with amperometric detection.

PubMed

Arribas, Alberto Sánchez; Bermejo, Esperanza; Zapardiel, Antonio; Téllez, Helena; Rodríguez-Flores, Juana; Zougagh, Mohammed; Ríos, Angel; Chicharro, Manuel

2009-02-01

A simple analytical scheme for the screening and quantification of zearalenone and its metabolites, alpha-zearalenol and beta-zearalenol, is reported. Extracts from maize flour samples were collected by supercritical fluid extraction and afterwards, they were analyzed by CE with amperometric detection. This scheme allowed a rapid and reliable identification of contaminated flour samples according to the reference value established for zearalenone by directive 2005/38/EC (200 microg/kg). The sample screening method was carried out by CZE using 25 mM borate separation buffer at pH 9.2 and 25.0 kV as separation voltage, monitoring the amperometric signal at +700 mV with a carbon paste electrode. In this way, total amount of mycotoxins was determined and samples were processed in 4 min with a detection limit of 12 microg/L, enough to discriminate between positive (more than 200 microg/L total mycotoxins) and negative samples (less than 200 microg/L total mycotoxins). Positive samples were then subjected to CZE separation and quantification of each analyte was done with 50 mM borate running buffer modified with 30% methanol at pH 9.7 and 17.5 kV as separation voltage. Under these conditions, separation was achieved in 15 min with detection limits from 20 to 35 microg/L for each analyte.

The relationship between observational scale and explained variance in benthic communities

PubMed Central

Flood, Roger D.; Frisk, Michael G.; Garza, Corey D.; Lopez, Glenn R.; Maher, Nicole P.

2018-01-01

This study addresses the impact of spatial scale on explaining variance in benthic communities. In particular, the analysis estimated the fraction of community variation that occurred at a spatial scale smaller than the sampling interval (i.e., the geographic distance between samples). This estimate is important because it sets a limit on the amount of community variation that can be explained based on the spatial configuration of a study area and sampling design. Six benthic data sets were examined that consisted of faunal abundances, common environmental variables (water depth, grain size, and surficial percent cover), and sonar backscatter treated as a habitat proxy (categorical acoustic provinces). Redundancy analysis was coupled with spatial variograms generated by multiscale ordination to quantify the explained and residual variance at different spatial scales and within and between acoustic provinces. The amount of community variation below the sampling interval of the surveys (< 100 m) was estimated to be 36–59% of the total. Once adjusted for this small-scale variation, > 71% of the remaining variance was explained by the environmental and province variables. Furthermore, these variables effectively explained the spatial structure present in the infaunal community. Overall, no scale problems remained to compromise inferences, and unexplained infaunal community variation had no apparent spatial structure within the observational scale of the surveys (> 100 m), although small-scale gradients (< 100 m) below the observational scale may be present. PMID:29324746

Determination of ultratrace elements in natural waters by solid-phase extraction and atomic spectrometry methods.

PubMed

Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Frache, Roberto

2003-01-01

A study was carried out on the preconcentration of ultratrace amounts of cadmium, lead, manganese, copper and iron from high-salinity aqueous samples and determination by atomic spectrometry methods. Sample volume, amount of resin, loading flow rate, and elution volume were optimized in order to obtain the simultaneous preconcentration of all the analytes. Quantitative recoveries were obtained by using 200 mg of iminodiacetic resin with a loading flow rate of 2 mL min(-1), elution volume of 3 mL and sample volume of 50-450 mL. Only copper in seawater samples was not completely retained by the resin (60-70% recovery), due to unfavorable competition of iminodiacetic-active groups with organically bound metal.To quantify the metals in the eluates, two atomic spectrometry techniques were compared: electrothermal atomization atomic absorption spectrometry (ETAAS) and inductively coupled plasma-optical emission spectrometry (ICP-OES) with simultaneous CCD detection system. Both techniques are suitable for sample analysis with detection limits of 1.0, 4.7, 3.3, 6.8, and 53 ng L(-1) using ETAAS and 12, 122, 3.4, 17, and 21 ng L(-1) using ICP-OES for Cd, Pb, Mn, Cu, and Fe, respectively. Relative standard deviations of the procedures ranged from 1.7 to 14% at the sub-microg L(-1) concentration level. The accuracy of both methods was verified by analyzing various certified reference materials (river water, estuarine water, coastal and off-shore seawater).

A statistical approach to determine fluxapyroxad and its three metabolites in soils, sediment and sludge based on a combination of chemometric tools and a modified quick, easy, cheap, effective, rugged and safe method.

PubMed

Li, Shasha; Liu, Xingang; Zhu, Yulong; Dong, Fengshou; Xu, Jun; Li, Minmin; Zheng, Yongquan

2014-09-05

An effective method for the quantification of fluxapyroxad and its three metabolites in soils, sediment and sludge was developed using ultrahigh performance chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). Both the extraction and clean-up steps of the QuEChERS procedure were optimised using a chemometric tool, which was expected to facilitate the rapid analysis with minimal procedures. Several operating parameters (MeCN/acetic acid ratio in the extraction solution (i.e., acetic acid percentage), water volume, extraction time, PSA amount, C18 amount, and GCB amount) were investigated using a Plackett-Burman (P-B) screening design. Afterward, the significant factors (acetic acid percentage, water volume, and PSA amount) obtained were optimised using central composite design (CCD) combined with the desirability function (DF) to determine the optimum experimental conditions. The optimised procedure provides high-level linearity for all studied compounds with correlation coefficients ranging between 0.9972 and 0.9999. The detection limits were in the range of 0.1 to 1.0μg/kg and the limits of quantitation (LOQs) were between 0.5 and 3.4μg/kg with relative standard deviations (RSD) between 2.3% and 9.6% (n=6). Therefore, the developed protocol can serve as a simple and sensitive tool for monitoring fluxapyroxad and its three metabolites in soil, sediment and sludge samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Nitric oxide measurements at a nonurban eastern United States site - Wallops instrument results from July 1983 GTE/CITE mission

NASA Technical Reports Server (NTRS)

Torres, A. L.

1985-01-01

The NASA Goddard Space Flight Center/Wallops Flight Facility nitric oxide detector used in the July 1983 GTE/CITE 1 instrument intercomparison is a chemiluminescence system which, at that time, had a detection limit of about 2 pptv (S/N = 1) for 60-s integrations. A substantial amount of NO concentration data was taken with this system at Wallops Island, VA, a site that should be typical of numerous nonurban coastal areas of the eastern United States and for which little other data are available. Midday concentrations under conditions of northwest winds averaged about 200 pptv, a value low enough to imply lower NO(x) amounts than are generally thought to exist in the eastern United States. During a 2-day period when the sampled air had spent 1-2 days over the Atlantic Ocean, average NO concentrations of 70 and 33 ptv were observed. Measurements at night indicated an average NO concentration of 16 pptv under wind conditions making contamination of the sampled air by local anthropogenic sources unlikely.

Modified surface based on magnetic nanocomposite of dithiooxamide/Fe3O4 as a sorbent for preconcentration and determination of trace amounts of copper

NASA Astrophysics Data System (ADS)

Mirabi, Ali; Shokuhi Rad, Ali; Khodadad, Hadiseh

2015-09-01

Magnetic nanocomposites surface (MNCS) which has anionic surfactant sodium dodecyl sulfate (SDS) coating and has undergone dithiooxamide treatment as the sorbent could be an easy and useful method to extract and make a pre-concentrated in detecting the copper ions before they are determined via the flame atomic absorption spectrometry (FAAS). The influences of the experimental parameters such as the pH of the sample, the type and concentration of the eluent, dithiooxamide concentration and volume, amount of sorbent and the interactions of ions with respect to the copper ion detection have been studied. The calibration graph was linear in the range of 2-600 ng ml-1 with detection limit of 0.2 ng ml-1. Relative standard deviation (RSD) for 6 replicate measurements was 1.8%. This method of detection has been applied to the determination of Cu ions at levels in real samples such as wheat flour, tomatoes, potatoes, red beans, oat, tap water, river water and sea water with satisfactory results.

Robotic liquid handling and automation in epigenetics.

PubMed

Gaisford, Wendy

2012-10-01

Automated liquid-handling robots and high-throughput screening (HTS) are widely used in the pharmaceutical industry for the screening of large compound libraries, small molecules for activity against disease-relevant target pathways, or proteins. HTS robots capable of low-volume dispensing reduce assay setup times and provide highly accurate and reproducible dispensing, minimizing variation between sample replicates and eliminating the potential for manual error. Low-volume automated nanoliter dispensers ensure accuracy of pipetting within volume ranges that are difficult to achieve manually. In addition, they have the ability to potentially expand the range of screening conditions from often limited amounts of valuable sample, as well as reduce the usage of expensive reagents. The ability to accurately dispense lower volumes provides the potential to achieve a greater amount of information than could be otherwise achieved using manual dispensing technology. With the emergence of the field of epigenetics, an increasing number of drug discovery companies are beginning to screen compound libraries against a range of epigenetic targets. This review discusses the potential for the use of low-volume liquid handling robots, for molecular biological applications such as quantitative PCR and epigenetics.

Electron spin resonance spectroscopy for immunoassay using iron oxide nanoparticles as probe.

PubMed

Jiang, Jia; Tian, Sizhu; Wang, Kun; Wang, Yang; Zang, Shuang; Yu, Aimin; Zhang, Ziwei

2018-02-01

With the help of iron oxide nanoparticles, electron spin resonance spectroscopy (ESR) was applied to immunoassay. Iron oxide nanoparticles were used as the ESR probe in order to achieve an amplification of the signal resulting from the large amount of Fe 3+ ion enclosed in each nanoparticle. Rabbit IgG was used as antigen to test this method. Polyclonal antibody of rabbit IgG was used as antibody to detect the antigen. Iron oxide nanoparticle with a diameter of either 10 or 30 nm was labeled to the antibody, and Fe 3+ in the nanoparticle was probed for ESR signal. The sepharose beads were used as solid phase to which rabbit IgG was conjugated. The nanoparticle-labeled antibody was first added in the sample containing antigen, and the antigen-conjugated sepharose beads were then added into the sample. The nanoparticle-labeled antibody bound to the antigen on sepharose beads was separated from the sample by centrifugation and measured. We found that the detection ranges of the antigen obtained with nanoparticles of different sizes were different because the amount of antibody on nanoparticles of 10 nm was about one order of magnitude higher than that on nanoparticles of 30 nm. When 10 nm nanoparticle was used as probe, the upper limit of detection was 40.00 μg mL -1 , and the analytical sensitivity was 1.81 μg mL -1 . When 30 nm nanoparticle was used, the upper limit of detection was 3.00 μg mL -1 , and the sensitivity was 0.014 and 0.13 μg mL -1 depending on the ratio of nanoparticle to antibody. Graphical abstract Schematic diagram of procedure and ESR spectra.

Whole Genome Amplification and Reduced-Representation Genome Sequencing of Schistosoma japonicum Miracidia.

PubMed

Shortt, Jonathan A; Card, Daren C; Schield, Drew R; Liu, Yang; Zhong, Bo; Castoe, Todd A; Carlton, Elizabeth J; Pollock, David D

2017-01-01

In areas where schistosomiasis control programs have been implemented, morbidity and prevalence have been greatly reduced. However, to sustain these reductions and move towards interruption of transmission, new tools for disease surveillance are needed. Genomic methods have the potential to help trace the sources of new infections, and allow us to monitor drug resistance. Large-scale genotyping efforts for schistosome species have been hindered by cost, limited numbers of established target loci, and the small amount of DNA obtained from miracidia, the life stage most readily acquired from humans. Here, we present a method using next generation sequencing to provide high-resolution genomic data from S. japonicum for population-based studies. We applied whole genome amplification followed by double digest restriction site associated DNA sequencing (ddRADseq) to individual S. japonicum miracidia preserved on Whatman FTA cards. We found that we could effectively and consistently survey hundreds of thousands of variants from 10,000 to 30,000 loci from archived miracidia as old as six years. An analysis of variation from eight miracidia obtained from three hosts in two villages in Sichuan showed clear population structuring by village and host even within this limited sample. This high-resolution sequencing approach yields three orders of magnitude more information than microsatellite genotyping methods that have been employed over the last decade, creating the potential to answer detailed questions about the sources of human infections and to monitor drug resistance. Costs per sample range from $50-$200, depending on the amount of sequence information desired, and we expect these costs can be reduced further given continued reductions in sequencing costs, improvement of protocols, and parallelization. This approach provides new promise for using modern genome-scale sampling to S. japonicum surveillance, and could be applied to other schistosome species and other parasitic helminthes.

Predicting Classifier Performance with Limited Training Data: Applications to Computer-Aided Diagnosis in Breast and Prostate Cancer

PubMed Central

Basavanhally, Ajay; Viswanath, Satish; Madabhushi, Anant

2015-01-01

Clinical trials increasingly employ medical imaging data in conjunction with supervised classifiers, where the latter require large amounts of training data to accurately model the system. Yet, a classifier selected at the start of the trial based on smaller and more accessible datasets may yield inaccurate and unstable classification performance. In this paper, we aim to address two common concerns in classifier selection for clinical trials: (1) predicting expected classifier performance for large datasets based on error rates calculated from smaller datasets and (2) the selection of appropriate classifiers based on expected performance for larger datasets. We present a framework for comparative evaluation of classifiers using only limited amounts of training data by using random repeated sampling (RRS) in conjunction with a cross-validation sampling strategy. Extrapolated error rates are subsequently validated via comparison with leave-one-out cross-validation performed on a larger dataset. The ability to predict error rates as dataset size increases is demonstrated on both synthetic data as well as three different computational imaging tasks: detecting cancerous image regions in prostate histopathology, differentiating high and low grade cancer in breast histopathology, and detecting cancerous metavoxels in prostate magnetic resonance spectroscopy. For each task, the relationships between 3 distinct classifiers (k-nearest neighbor, naive Bayes, Support Vector Machine) are explored. Further quantitative evaluation in terms of interquartile range (IQR) suggests that our approach consistently yields error rates with lower variability (mean IQRs of 0.0070, 0.0127, and 0.0140) than a traditional RRS approach (mean IQRs of 0.0297, 0.0779, and 0.305) that does not employ cross-validation sampling for all three datasets. PMID:25993029

Mixed hemimicelles solid-phase extraction based on ionic liquid-coated Fe3O4/SiO2 nanoparticles for the determination of flavonoids in bio-matrix samples coupled with high performance liquid chromatography.

PubMed

He, Huan; Yuan, Danhua; Gao, Zhanqi; Xiao, Deli; He, Hua; Dai, Hao; Peng, Jun; Li, Nan

2014-01-10

A novel magnetic solid-phase extraction (MSPE) method based on mixed hemimicelles of room temperature ionic liquids (RTILs) coated Fe3O4/SiO2 nanoparticles (NPs) was developed for simultaneous extraction of trace amounts of flavonoids in bio-matrix samples. A comparative study on the use of RTILs (C16mimBr) and CTAB-coated Fe3O4/SiO2 NPs as sorbents was presented. Owing to bigger adsorption amounts for analytes, RTILs-coated Fe3O4/SiO2 NPs was selected as MSPE materials and three analytes luteolin, quercetin and kaempferol can be quantitatively extracted and simultaneously determined coupled with high performance liquid chromatography (HPLC) in urine samples. No interferences were caused by proteins or endogenous compounds. Good linearity (R(2)>0.9993) for all calibration curves was obtained, and the limits of detection (LOD) for luteolin, quercetin and kaempferol were 0.10 ng/mL, 0.50 ng/mL and 0.20 ng/mL in urine samples, respectively. Satisfactory recoveries (93.5-97.6%, 90.1-95.4% and 93.3-96.6% for luteolin, quercetin and kaempferol) in biological matrices were achieved. It was notable that while using a small amount of Fe3O4/SiO2 NPs (4.0 mg) and C16mimBr (1.0 mg), satisfactory preconcentration factors and extraction recoveries for the three flavonoids were obtained. To the best of our knowledge, this is the first time a mixed hemimicelles MSPE method based on RTILs and Fe3O4/SiO2 NPs magnetic separation has ever been used for pretreatment of complex biological samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Resistivity and Induced Polarization Imaging at a Hydrocarbon Contaminated Site in Brazil

NASA Astrophysics Data System (ADS)

Ustra, A.; Elis, V.; Hiodo, F.; Bondioli, A.; Miura, G.

2012-12-01

An area contaminated by accidental BTEX spills was investigated with resistivity and induced polarization methods. The main objective in this study was to relate the geophysical signature of the area with zones that were possibly undergoing microbial degradation of the contaminants. The spills took place over a decade ago; however, the exact location of these spills is unknown, as well as the amount of contaminant that was released into the subsurface. DC-resistivity identified a high contrast between the background (rho up to 2000 ohm.m) and a relatively conductive zone (rho < 100 ohm.m), where high chargeabilities were also measured (m > 30 mV/V). Normalized chargeability is enhanced in this anomaly zone (mn > 0.1). Soil samples collected in the area were submitted to direct bacterial count, clay content estimation, X-ray diffraction and SEM analysis. The electrical properties of each samples was also measured. The samples collected from the "background" (high resistivity zone) presented total bacterial amounts much smaller (dozens of colony forming units) than the samples from the conductive zone (millions of colony forming units). This observation could lead us to interpret that the zone of higher bacteria amount is undergoing biodegradation that would explain the increased conductivity at that portion of the subsurface. However, the geophysical properties observed at this zone could also be related to the clay content distribution throughout the surveyed area (concentrations up to 30%). Moreover, despite the fact that more microbes were found in the area, SEM images did not find any biodegradation typical feature of the grains, which are for example, mineral corrosion and dissolution or even biomineralization. This study is still undergoing and we are searching for more evidence of biodegradation in the samples. This study shows the limitation of the use of geophysical methods to access contaminant presence and/or biodegradation zones when the exact location of the contamination is unknown.

Internal acid buffering in San Joaquin Valley fog drops and its influence on aerosol processing

NASA Astrophysics Data System (ADS)

Collett, Jeffrey L.; Hoag, Katherine J.; Rao, Xin; Pandis, Spyros N.

Although several chemical pathways exist for S(IV) oxidation in fogs and clouds, many are self-limiting: as sulfuric acid is produced and the drop pH declines, the rates of these pathways also decline. Some of the acid that is produced can be buffered by uptake of gaseous ammonia. Additional internal buffering can result from protonation of weak and strong bases present in solution. Acid titrations of high pH fog samples (median pH=6.49) collected in California's San Joaquin Valley reveal the presence of considerable internal acid buffering. In samples collected at a rural location, the observed internal buffering could be nearly accounted for based on concentrations of ammonia and bicarbonate present in solution. In samples collected in the cities of Fresno and Bakersfield, however, significant additional, unexplained buffering was present over a pH range extending from approximately four to seven. The additional buffering was found to be associated with dissolved compounds in the fogwater. It could not be accounted for by measured concentrations of low molecular weight ( C1- C3) carboxylic acids, S(IV), phosphate, or nitrophenols. The amount of unexplained buffering in individual fog samples was found to correlate strongly with the sum of sample acetate and formate concentrations, suggesting that unmeasured organic species may be important contributors. Simulation of a Bakersfield fog episode with and without the additional, unexplained buffering revealed a significant impact on the fog chemistry. When the additional buffering was included, the simulated fog pH remained 0.3-0.7 pH units higher and the amount of sulfate present after the fog evaporated was increased by 50%. Including the additional buffering in the model simulation did not affect fogwater nitrate concentrations and was found to slightly decrease ammonium concentrations. The magnitude of the buffering effect on aqueous sulfate production is sensitive to the amount of ozone present to oxidize S(IV) in these high pH fogs.

Estimation of the limit of detection using information theory measures.

PubMed

Fonollosa, Jordi; Vergara, Alexander; Huerta, Ramón; Marco, Santiago

2014-01-31

Definitions of the limit of detection (LOD) based on the probability of false positive and/or false negative errors have been proposed over the past years. Although such definitions are straightforward and valid for any kind of analytical system, proposed methodologies to estimate the LOD are usually simplified to signals with Gaussian noise. Additionally, there is a general misconception that two systems with the same LOD provide the same amount of information on the source regardless of the prior probability of presenting a blank/analyte sample. Based upon an analogy between an analytical system and a binary communication channel, in this paper we show that the amount of information that can be extracted from an analytical system depends on the probability of presenting the two different possible states. We propose a new definition of LOD utilizing information theory tools that deals with noise of any kind and allows the introduction of prior knowledge easily. Unlike most traditional LOD estimation approaches, the proposed definition is based on the amount of information that the chemical instrumentation system provides on the chemical information source. Our findings indicate that the benchmark of analytical systems based on the ability to provide information about the presence/absence of the analyte (our proposed approach) is a more general and proper framework, while converging to the usual values when dealing with Gaussian noise. Copyright © 2013 Elsevier B.V. All rights reserved.

Synthesis and characterization of pore size-tunable magnetic mesoporous silica nanoparticles.

PubMed

Zhang, Jixi; Li, Xu; Rosenholm, Jessica M; Gu, Hong-chen

2011-09-01

Magnetic mesoporous silica nanoparticles (M-MSNs) are emerging as one of the most appealing candidates for theranostic carriers. Herein, a simple synthesis method of M-MSNs with a single Fe(3)O(4) nanocrystal core and a mesoporous shell with radially aligned pores was elaborated using tetraethyl orthosilicate (TEOS) as silica source, cationic surfactant CTAB as template, and 1,3,5-triisopropylbenzene (TMB)/decane as pore swelling agents. Due to the special localization of TMB during the synthesis process, the pore size was increased with added TMB amount within a limited range, while further employment of TMB lead to severe particle coalescence and not well-developed pore structure. On the other hand, when a proper amount of decane was jointly incorporated with limited amounts of TMB, effective pore expansion of M-MSNs similar to that of analogous mesoporous silica nanoparticles was realized. The resultant M-MSN materials possessed smaller particle size (about 40-70 nm in diameter), tunable pore sizes (3.8-6.1 nm), high surface areas (700-1100 m(2)/g), and large pore volumes (0.44-1.54 cm(3)/g). We also demonstrate their high potential in conventional DNA loading. Maximum loading capacity of salmon sperm DNA (375 mg/g) was obtained by the use of the M-MSN sample with the largest pore size of 6.1 nm. Copyright © 2011 Elsevier Inc. All rights reserved.

Optimization of the solvent-based dissolution method to sample volatile organic compound vapors for compound-specific isotope analysis.

PubMed

Bouchard, Daniel; Wanner, Philipp; Luo, Hong; McLoughlin, Patrick W; Henderson, James K; Pirkle, Robert J; Hunkeler, Daniel

2017-10-20

The methodology of the solvent-based dissolution method used to sample gas phase volatile organic compounds (VOC) for compound-specific isotope analysis (CSIA) was optimized to lower the method detection limits for TCE and benzene. The sampling methodology previously evaluated by [1] consists in pulling the air through a solvent to dissolve and accumulate the gaseous VOC. After the sampling process, the solvent can then be treated similarly as groundwater samples to perform routine CSIA by diluting an aliquot of the solvent into water to reach the required concentration of the targeted contaminant. Among solvents tested, tetraethylene glycol dimethyl ether (TGDE) showed the best aptitude for the method. TGDE has a great affinity with TCE and benzene, hence efficiently dissolving the compounds during their transition through the solvent. The method detection limit for TCE (5±1μg/m 3 ) and benzene (1.7±0.5μg/m 3 ) is lower when using TGDE compared to methanol, which was previously used (385μg/m 3 for TCE and 130μg/m 3 for benzene) [2]. The method detection limit refers to the minimal gas phase concentration in ambient air required to load sufficient VOC mass into TGDE to perform δ 13 C analysis. Due to a different analytical procedure, the method detection limit associated with δ 37 Cl analysis was found to be 156±6μg/m 3 for TCE. Furthermore, the experimental results validated the relationship between the gas phase TCE and the progressive accumulation of dissolved TCE in the solvent during the sampling process. Accordingly, based on the air-solvent partitioning coefficient, the sampling methodology (e.g. sampling rate, sampling duration, amount of solvent) and the final TCE concentration in the solvent, the concentration of TCE in the gas phase prevailing during the sampling event can be determined. Moreover, the possibility to analyse for TCE concentration in the solvent after sampling (or other targeted VOCs) allows the field deployment of the sampling method without the need to determine the initial gas phase TCE concentration. The simplified field deployment approach of the solvent-based dissolution method combined with the conventional analytical procedure used for groundwater samples substantially facilitates the application of CSIA to gas phase studies. Copyright © 2017 Elsevier B.V. All rights reserved.

Application of NaClO-treated multiwalled carbon nanotubes as solid phase extraction sorbents for preconcentration of trace 2,4-dichlorophenoxyacetic acid in aqueous samples.

PubMed

Lu, Ping; Deng, Dayi; Ni, Xiaodan

2012-09-01

Multiwalled carbon nanotubes functionalized by oxidation of original multiwalled carbon nanotubes with NaClO were prepared and their application as solid phase extraction sorbent for 2,4-dichlorophenoxyacetic acid (2,4-D) was investigated systemically, and a new method was developed for the determination of trace 2,4-D in water samples based on extraction and preconcentration of 2,4-D with solid phase extraction columns packed with NaClO-treated multiwalled carbon nanotubes prior to its determination by HPLC. The optimum experimental parameters for preconcentration of 2,4-D, including the column activating conditions, the amount of the sorbent, pH of the sample, elution composition, and elution volume, were investigated. The results indicated 2,4-D could be quantitatively retained by 100 mg NaClO-treated multiwalled carbon nanotubes at pH 5, and then eluted completely with 10 mL 3:1 (v/v) methanol-ammonium acetate solution (0.3 mol/L). The detection limit of this method for 2,4-D was 0.15 μg/L, and the relative standard deviation was 2.3% for fortified tap water samples and 2.5% for fortified riverine water sample at the 10 μg/L level. The method was validated using fortified tap water and riverine water samples with known amount of 2,4-D at the 0.4, 10, and 30 μg/L levels, respectively. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A portable molecular-sieve-based CO{sub 2} sampling system for radiocarbon measurements

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

Palonen, V., E-mail: vesa.palonen@helsinki.fi

We have developed a field-capable sampling system for the collection of CO{sub 2} samples for radiocarbon-concentration measurements. Most target systems in environmental research are limited in volume and CO{sub 2} concentration, making conventional flask sampling hard or impossible for radiocarbon studies. The present system captures the CO{sub 2} selectively to cartridges containing 13X molecular sieve material. The sampling does not introduce significant under-pressures or significant losses of moisture to the target system, making it suitable for most environmental targets. The system also incorporates a significantly larger sieve container for the removal of CO{sub 2} from chambers prior to the CO{submore » 2} build-up phase and sampling. In addition, both the CO{sub 2} and H{sub 2}O content of the sample gas are measured continuously. This enables in situ estimation of the amount of collected CO{sub 2} and the determination of CO{sub 2} flux to a chamber. The portable sampling system is described in detail and tests for the reliability of the method are presented.« less

[Simultaneous determination of the migrations of bisphenol A and phenol in polycarbonate bottles based on subcritical water extraction and high performance liquid chromatography].

PubMed

Bai, Weiwei; Liu, Shuhui; Cao, Jiangping; Fan, Yingying; Xie, Qilong

2013-03-01

A new method was established for the simultaneous determination of the migration amounts of bisphenol A (BPA) and phenol from polycarbonate (PC) bottles based on subcritical water extraction (SWE) and high performance liquid chromatography. The optimum extraction conditions included an extraction temperature of 120 degree C, a pressure of 6.89 MPa (1000 psi), a static extraction time of 1 h and one cycle. Under the conditions, the migration amounts of the BPA ranged from 6.81 to 1116 micro g/g in 11 samples. Phenol was not detectable in 5 samples, and in other ones the migration amounts of phenol varied in the range of 3.25 -6. 08 micro g/g. The traditional soaking extraction experiments showed that PC was subjected to weak hydrolysis after long-time leaching. The BPA and phenol were separated in 8 min. Good linearities were obtained in the range of 0. 05 - 20 mg/L for BPA and 0.02 - 20 mg/L for phenol ( r > 0.999 7). The limits of detection were 7.6 micro g/L for BPA and 2.0 micro g/L for phenol. Intra-day and inter-day repeatabilities (expressed as RSD) were less than 5.21% and 11.63%, respectively. Compared with traditional water soaking extraction, the extraction efficiencies increased 49 - 106 times using this developed SWE method. The procedure is simple, rapid and environment friendly, and can be utilized to determine the migration amounts of BPA and phenol in PC bottles.

Utility of ultrasound assisted-cloud point extraction and spectophotometry as a preconcentration and determination tool for the sensitive quantification of mercury species in fish samples

NASA Astrophysics Data System (ADS)

Altunay, Nail

2018-01-01

The current study reports, for the first time, the development of a new analytical method employing ultrasound assisted-cloud point extraction (UA-CPE) for the extraction of CH3Hg+ and Hg2 + species from fish samples. Detection and quantification of mercury species were performed at 550 nm by spectrophotometry. The analytical variables affecting complex formation and extraction efficiency were extensively evaluated and optimized by univariate method. Due to behave 14-fold more sensitive and selective of thiophene 2,5-dicarboxylic acid (H2TDC) to Hg2 + ions than CH3Hg+ in presence of mixed surfactant, Tween 20 and SDS at pH 5.0, the amounts of free Hg2 + and total Hg were spectrophotometrically established at 550 nm by monitoring Hg2 + in the pretreated- and extracted-fish samples in ultrasonic bath to speed up extraction using diluted acid mixture (1:1:1, v/v, 4 mol L- 1 HNO3, 4 mol L- 1 HCl, and 0.5 mol L- 1 H2O2), before and after pre-oxidation with permanganate in acidic media. The amount of CH3Hg+ was calculated from difference between total Hg and Hg2 + amounts. The UA-CPE method showed to be suitable for the extraction and determination of mercury species in certified reference materials. The results were in a good agreement (with Student's t-test at 95% confidence limit) with the certified values, and the relative standard deviation was lower than 3.2%. The limits of detection have been 0.27 and 1.20 μg L- 1, for Hg2 + from aqueous calibration solutions and matrix-matched calibration solutions spiked before digestion, respectively, while it is 2.43 μg L- 1 for CH3Hg+ from matrix-matched calibration solutions. A significant matrix effect was not observed from comparison of slopes of both calibration curves, so as to represent the sample matrix. The method was applied to fish samples for speciation analysis of Hg2 + and CH3Hg+. In terms of speciation, while total Hg is detected in range of 2.42-32.08 μg kg- 1, the distribution of mercury in fish were in range of 0.7-11.06 μg kg- 1 for CH3Hg+ and in range of 1.72-24.56 μg kg- 1 for Hg2 +.

Drop-on-demand sample introduction system coupled with the flowing atmospheric-pressure afterglow for direct molecular analysis of complex liquid micro-volume samples

PubMed Central

Schaper, J. Niklas; Pfeuffer, Kevin P.; Shelley, Jacob T.; Bings, Nicolas H.

2012-01-01

One of the fastest developing fields in analytical spectrochemistry in recent years is ambient desorption/ionization mass spectrometry (ADI-MS). This burgeoning interest has been due to the demonstrated advantages of the method: simple mass spectra, little or no sample preparation, and applicability to samples in the solid, liquid, or gaseous state. One such ADI-MS source, the flowing atmospheric-pressure afterglow (FAPA), is capable of direct analysis of solids just by aiming the source at the solid surface and sampling the produced ions into a mass spectrometer. However, direct introduction of significant volumes of liquid samples into this source has not been possible, as solvent loads can quench the afterglow and, thus, the formation of reagent ions. As a result, the analysis of liquid samples is preferably carried out by analyzing dried residues or by desorbing small amounts of liquid samples directly from the liquid surface. In the former case, reproducibility of sample introduction is crucial if quantitative results are desired. In the present study, introduction of liquid samples as very small droplets helps overcome the issues of sample positioning and reduced levels of solvent intake. A recently developed “drop-on-demand” (DOD) aerosol generator is capable of reproducibly producing very small volumes of liquid (~17 pL). In this paper, the coupling of FAPA-MS and DOD is reported and applications are suggested. Analytes representing different classes of substances were tested and limits of detections were determined. Matrix tolerance was investigated for drugs of abuse and their metabolites by analyzing raw urine samples and quantification without the use of internal standards. Limits of detection below 2 µg/mL, without sample pretreatment, were obtained. PMID:23025277

Drop-on-demand sample introduction system coupled with the flowing atmospheric-pressure afterglow for direct molecular analysis of complex liquid microvolume samples.

PubMed

Schaper, J Niklas; Pfeuffer, Kevin P; Shelley, Jacob T; Bings, Nicolas H; Hieftje, Gary M

2012-11-06

One of the fastest developing fields in analytical spectrochemistry in recent years is ambient desorption/ionization mass spectrometry (ADI-MS). This burgeoning interest has been due to the demonstrated advantages of the method: simple mass spectra, little or no sample preparation, and applicability to samples in the solid, liquid, or gaseous state. One such ADI-MS source, the flowing atmospheric-pressure afterglow (FAPA), is capable of direct analysis of solids just by aiming the source at the solid surface and sampling the produced ions into a mass spectrometer. However, direct introduction of significant volumes of liquid samples into this source has not been possible, as solvent loads can quench the afterglow and, thus, the formation of reagent ions. As a result, the analysis of liquid samples is preferably carried out by analyzing dried residues or by desorbing small amounts of liquid samples directly from the liquid surface. In the former case, reproducibility of sample introduction is crucial if quantitative results are desired. In the present study, introduction of liquid samples as very small droplets helps overcome the issues of sample positioning and reduced levels of solvent intake. A recently developed "drop-on-demand" (DOD) aerosol generator is capable of reproducibly producing very small volumes of liquid (∼17 pL). In this paper, the coupling of FAPA-MS and DOD is reported and applications are suggested. Analytes representing different classes of substances were tested and limits of detections were determined. Matrix tolerance was investigated for drugs of abuse and their metabolites by analyzing raw urine samples and quantification without the use of internal standards. Limits of detection below 2 μg/mL, without sample pretreatment, were obtained.

Modified T-history method for measuring thermophysical properties of phase change materials at high temperature

NASA Astrophysics Data System (ADS)

Omaraa, Ehsan; Saman, Wasim; Bruno, Frank; Liu, Ming

2017-06-01

Latent heat storage using phase change materials (PCMs) can be used to store large amounts of energy in a narrow temperature difference during phase transition. The thermophysical properties of PCMs such as latent heat, specific heat and melting and solidification temperature need to be defined at high precision for the design and estimating the cost of latent heat storage systems. The existing laboratory standard methods, such as differential thermal analysis (DTA) and differential scanning calorimetry (DSC), use a small sample size (1-10 mg) to measure thermophysical properties, which makes these methods suitable for homogeneous elements. In addition, this small amount of sample has different thermophysical properties when compared with the bulk sample and may have limitations for evaluating the properties of mixtures. To avoid the drawbacks in existing methods, the temperature - history (T-history) method can be used with bulk quantities of PCM salt mixtures to characterize PCMs. This paper presents a modified T-history setup, which was designed and built at the University of South Australia to measure the melting point, heat of fusion, specific heat, degree of supercooling and phase separation of salt mixtures for a temperature range between 200 °C and 400 °C. Sodium Nitrate (NaNO3) was used to verify the accuracy of the new setup.

Digital microfluidics platform for interfacing solid-liquid extraction column with portable capillary electropherograph for analysis of soil amino acids.

PubMed

Gorbatsova, Jelena; Jaanus, Martin; Vaher, Merike; Kaljurand, Mihkel

2016-02-01

In this work, the concept of a field-portable analyzer is proposed that operates with milliliter amounts of solvents and samples. The need to develop such an analyzer is not only driven by specific extraterrestrial analysis but also, for example, by forensics applications where the amount of liquid that can be taken to the field is severely limited. The prototype of the proposed analyzer consists of a solid-liquid extractor, the output of which is connected to the micropump, which delivers droplets of extracts to digital microfluidic platform (DMFP). In this way, world-to-chip interfacing is established. Further, the sample droplets are transported to CE capillary inlet port, separated and detected via a contactless conductivity detector. Working buffers and other solvents needed to perform CE analysis are also delivered as droplets to the DMFP and transported through the CE capillary. The performance of the analyzer is demonstrated by analysis of amino acids in sand matrices. The recovery of the spiked amino acids from the inert sand sample was from 34 to 51% with analysis LOD from 0.2 to 0.6 ppm and migration time RSD from 0.2 to 6.0%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

HPLC study of migration of terephthalic acid and isophthalic acid from PET bottles into edible oils.

PubMed

Khaneghah, Amin Mousavi; Limbo, Sara; Shoeibi, Shahram; Mazinani, Somayeh

2014-08-01

Polyethylene terephthalate (PET) containers for food oil packaging were evaluated with a newly established determination method for terephthalic acid (TPA) and isophthalic acid (IPA). The analysis of monomers, TPA and IPA that migrate from PET bottles into oils was performed using high-pressure liquid chromatography with a diode array detector. Three types of commercial oils (sunflower oil, canola oil and blended oil which included sunflower oil, soy bean oil and cottonseed oil) were bottled in PET containers. These samples were incubated for 10 days at 49 °C as accelerated test condition. The means of recovery for this method varied from 70% to 72% and from 101% to 111% for TPA and IPA, respectively. The results showed that the amounts of specific migration of TPA and IPA into the samples conform to European Union legislation that identifies specific migration limits. More important, the results highlighted a different behavior of migration as a function of the fatty acid profile. Previous investigations have been performed with food simulants such as HB307 or 20% ethanol but our study used real food samples and determined trace amounts of the migrated compounds. Further investigation will be needed to better explain the influence of fatty acid conformation on migration of PET monomers. © 2013 Society of Chemical Industry.

Influence of increasing amount of recycled concrete powder on mechanical properties of cement paste

NASA Astrophysics Data System (ADS)

Topič, Jaroslav; Prošek, Zdeněk; Plachý, Tomáš

2017-09-01

This paper deals with using fine recycled concrete powder in cement composites as micro-filler and partial cement replacement. Binder properties of recycled concrete powder are given by exposed non-hydrated cement grains, which can hydrate again and in small amount replace cement or improve some mechanical properties. Concrete powder used in the experiments was obtained from old railway sleepers. Infrastructure offer more sources of old concrete and they can be recycled directly on building site and used again. Experimental part of this paper focuses on influence of increasing amount of concrete powder on mechanical properties of cement paste. Bulk density, shrinkage, dynamic Young’s modulus, compression and flexural strength are observed during research. This will help to determine limiting amount of concrete powder when decrease of mechanical properties outweighs the benefits of cement replacement. The shrinkage, dynamic Young’s modulus and flexural strength of samples with 20 to 30 wt. % of concrete powder are comparable with reference cement paste or even better. Negative effect of concrete powder mainly influenced the compression strength. Only a 10 % cement replacement reduced compression strength by about 25 % and further decrease was almost linear.

Exploring the relationship between child physical abuse and adult dating violence using a causal inference approach in an emerging adult population in South Korea.

PubMed

Jennings, Wesley G; Park, MiRang; Richards, Tara N; Tomsich, Elizabeth; Gover, Angela; Powers, Ráchael A

2014-12-01

Child maltreatment is one of the most commonly examined risk factors for violence in dating relationships. Often referred to as the intergenerational transmission of violence or cycle of violence, a fair amount of research suggests that experiencing abuse during childhood significantly increases the likelihood of involvement in violent relationships later, but these conclusions are primarily based on correlational research designs. Furthermore, the majority of research linking childhood maltreatment and dating violence has focused on samples of young people from the United States. Considering these limitations, the current study uses a rigorous, propensity score matching approach to estimate the causal effect of experiencing child physical abuse on adult dating violence among a large sample of South Korean emerging adults. Results indicate that the link between child physical abuse and adult dating violence is spurious rather than causal. Study limitations and implications are discussed. Copyright © 2014 Elsevier Ltd. All rights reserved.

Autism and urinary exogenous neuropeptides: development of an on-line SPE-HPLC-tandem mass spectrometry method to test the opioid excess theory.

PubMed

Dettmer, K; Hanna, D; Whetstone, P; Hansen, R; Hammock, B D

2007-08-01

Autism is a complex neurodevelopmental disorder with unknown etiology. One hypothesis regarding etiology in autism is the "opioid peptide excess" theory that postulates that excessive amounts of exogenous opioid-like peptides derived from dietary proteins are detectable in urine and that these compounds may be pathophysiologically important in autism. A selective LC-MS/MS method was developed to analyze gliadinomorphin, beta-casomorphin, deltorphin 1, and deltorphin 2 in urine. The method is based on on-line SPE extraction of the neuropeptides from urine, column switching, and subsequent HPLC analysis. A limit of detection of 0.25 ng/mL was achieved for all analytes. Analyte recovery rates from urine ranged between 78% and 94%, with relative standard deviations of 0.2-6.8%. The method was used to screen 69 urine samples from children with and without autism spectrum disorders for the occurrence of neuropeptides. The target neuropeptides were not detected above the detection limit in either sample set.

Limitation in the detection of Listeria monocytogenes in food in the presence of competing Listeria innocua.

PubMed

Oravcová, K; Trncíková, T; Kuchta, T; Kaclíková, E

2008-02-01

Detectability of Listeria monocytogenes at 10(0) CFU per food sample in the presence of Listeria innocua using standard microbiological detection was evaluated and compared with the real-time PCR-based method. Enrichment in half-Fraser broth followed by subculture in Fraser broth according to EN ISO 11290-1 was used. False-negative detection of 10(0) CFU L. monocytogenes was obtained in the presence of 10(1) CFU L. innocua per sample using the standard detection method in contrast to more than 10(5) CFU L. innocua per sample using real-time PCR. Identification of L. monocytogenes on the chromogenic medium by the standard procedure was impossible if L. innocua was able to overgrow L. monocytogenes by more than three orders of magnitude after the enrichment in model samples. These results were confirmed using naturally contaminated food samples. Standard microbiological method was insufficient for the reliable detection of 10(0) CFU L. monocytogenes in the presence of more than 10(0) CFU of L. innocua per sample. On the other hand, if the growth of L. monocytogenes was sufficient to reach the concentration equal to the detection limit of PCR, the amount of the other microflora present in the food sample including L. innocua was not relevant for success of the PCR detection of L. monocytogenes. After the enrichment, the PCR detection is more convenient than the standard one as PCR detection is not compromised by other present microflora.

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

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

In-line micro-matrix solid-phase dispersion extraction for simultaneous separation and extraction of Sudan dyes in different spices.

PubMed

Rajabi, Maryam; Sabzalian, Sedigheh; Barfi, Behruz; Arghavani-Beydokhti, Somayeh; Asghari, Alireza

2015-12-18

A novel, simple, fast, and miniaturized method, termed in-line micro-matrix solid-phase dispersion (in-line MMSPD), coupled with high performance liquid chromatography (HPLC) was developed for the simultaneous extraction and determination of Sudan dyes (i.e. Sudan I-IV, Sudan orange G, Sudan black B, and Sudan red G) with the aid of an experimental design strategy. In this method, a matrix solid-phase dispersion (MSPD) column including a suitable mixture of polar sorbents was inserted in the mobile phase pathway, and while the interfering compounds were retained, the analytes were eluted and entered into the analytical column. In this way, the extraction, elution, and separation of the analytes were performed sequentially. Under the optimal experimental conditions (including the amount of sample, 0.0426g; amount of dispersant phase, 0.0216g of florisil, 0.0227g of silica, 0.0141g of alumina; and blending time, 112s), the limits of detection (LODs), limits of quantification, linear dynamic ranges, and recoveries were obtained to be 0.3-15.3μgkg(-1), 1-50μgkg(-1), 50-28,000μgkg(-1), and 94.5-99.1%, respectively. The results obtained showed that determination of the selected Sudan dyes in food samples using an enough sensitive and a simple analytically validated method like in-line MMSPD may offer a suitable screening method, which could be useful for food analysis and adulteration. Copyright © 2015 Elsevier B.V. All rights reserved.

Comparison of Laboratory-Developed and Commercial Monoclonal Antibody-Based Sandwich Enzyme-Linked Immunosorbent Assays for Almond (Prunus dulcis) Detection and Quantification.

PubMed

Liu, Changqi; Chhabra, Guneet S; Zhao, Jing; Zaffran, Valerie D; Gupta, Sahil; Roux, Kenneth H; Gradziel, Thomas M; Sathe, Shridhar K

2017-10-01

A commercially available monoclonal antibody (mAb)-based direct sandwich enzyme-linked immunosorbent assay (ELISA) kit (BioFront Technologies, Tallahassee, Fla., U.S.A.) was compared with an in-house developed mAb 4C10-based ELISA for almond detection. The assays were comparable in sensitivity (limit of detection < 1 ppm full fat almond, limit of quantification < 5 ppm full fat almond), specificity (no cross-reactivity with 156 tested foods at a concentration of 100000 ppm whole sample), and reproducibility (intra- and interassay variability < 15% CV). The target antigens were stable and detectable in whole almond seeds subjected to autoclaving, blanching, frying, microwaving, and dry roasting. The almond recovery ranges for spiked food matrices were 84.3% to 124.6% for 4C10 ELISA and 81.2% to 127.4% for MonoTrace ELISA. The almond recovery ranges for commercial and laboratory prepared foods with declared/known almond amount were 30.9% to 161.2% for 4C10 ELISA and 38.1% to 207.6% for MonoTrace ELISA. Neither assay registered any false-positive or negative results among the tested commercial and laboratory prepared samples. Ability to detect and quantify trace amounts of almonds is important for improving safety of almond sensitive consumers. Two monoclonal antibody-based ELISAs were compared for almond detection. The information is useful to food industry, regulatory agencies, scientific community, and almond consumers. © 2017 Institute of Food Technologists®.

[Application of Stir Bar Sorptive Extraction and Gas Chromatograph Mass Spectrometer to the Phthalic Acid Esters Analysis in Seawater].

PubMed

Gao, Chen-chen; Li, Feng-min; Lu, Lun; Sun, Yue

2015-10-01

For the determination of trace amounts of phthalic acid esters (PAEs) in complex seawater matrix, a stir bar sorptive extraction gas chromatography mass spectrometry (SBSE-GC-MS) method was established. Dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), butyl benzyl phthalate (BBP), dibutyl phthalate (2-ethylhexyl) phthalate (DEHP) and dioctyl phthalate (DOP) were selected as study objects. The effects of extraction time, amount of methanol, amount of sodium chloride, desorption time and desorption solvent were optimized. The method of SBSE-GC-MS was validated through recoveries and relative standard deviation. The optimal extraction time was 2 h. The optimal methanol content was 10%. The optimal sodium chloride content was 5% . The optimal desorption time was 50 min. The optimal desorption solvent was the mixture of methanol to acetonitrile (4:1, volume: volume). The linear relationship between the peak area and the concentration of PAEs was relevant. The correlation coefficients were greater than 0.997. The detection limits were between 0.25 and 174.42 ng x L(-1). The recoveries of different concentrations were between 56.97% and 124.22% . The relative standard deviations were between 0.41% and 14.39%. On the basis of the method, several estuaries water sample of Jiaozhou Bay were detected. DEP was detected in all samples, and the concentration of BBP, DEHP and DOP were much higher than the rest.

Ultra-micro analysis of liquids and suspensions based on laser-induced plasma emissions

NASA Astrophysics Data System (ADS)

Cheung, N. H.; Ng, C. W.; Ho, W. F.; Yeung, E. S.

1998-05-01

Spectrochemical analysis of liquids and suspensions using laser-induced plasma emissions was investigated. Nd:YAG pulsed-laser (532-nm) ablation of aqueous samples produced plasmas that were hot (few eV) and extensively ionized, with electron density in the 10 18 cm -3 range. Analyte line signals were initially masked by intense plasma continuum emissions, and would only emerge briefly above the background when the plume temperature dropped below 1 eV during the course of its very rapid cooling. In contrast, 193-nm laser ablation at similar fluence generated plasmas of much lower (<1 eV) temperature but comparable electron density. The plasma continuum emissions were relatively weak and the signal-to-background ratio was a thousand times better. This `cold' plasma was ideal for sampling trace amounts of biologically important elements such as sodium and potassium. By ablating hydrodynamically focused jets in a sheath-flow, and with acoustic normalization for improved precision, the single-shot detection limits of sodium and potassium were 8 and 50 fg, respectively. Using the sheath-flow arrangement, the amounts of sodium and potassium inside single human red blood cells were simultaneously determined for the first time. The intracellular contents for a given blood donor were found to vary significantly, with only very weak correlation between the amounts of sodium and potassium in individual cells.

Changes in Rice Pesticide Use and Surface Water Concentrations in the Sacramento River Watershed, California

USGS Publications Warehouse

Orlando, James L.; Kuivila, Kathryn

2004-01-01

Pesticides applied to rice fields in California are transported into the Sacramento River watershed by the release of rice field water. Despite monitoring and mitigation programs, concentrations of two rice pesticides, molinate and thiobencarb, continue to exceed the surface-water concentration performance goals established by the Central Valley Regional Water Quality Control Board. There have been major changes in pesticide use over the past decade, and the total amount of pesticides applied remains high. Molinate use has declined by nearly half, while thiobencarb use has more than doubled; carbofuran has been eliminated and partially replaced by the pyrethroid pesticide lambda-cyhalothrin. A study was conducted in 2002 and 2003 by the U.S. Geological Survey to determine if the changes in pesticide use on rice resulted in corresponding changes in pesticide concentrations in surface waters. During the rice growing season (May-July), water samples, collected weekly at three sites in 2002 and two sites in 2003, were analyzed for pesticides using both solid-phase and liquid-liquid extraction in combination with gas chromatography/mass spectrometry. Analytes included lambda-cyhalothrin, molinate, thiobencarb, and two degradation products of molinate: 2-keto-molinate and 4-keto-molinate. Molinate, thiobencarb, and 4-keto-molinate were detected in all samples, 2-keto-molinate was detected in less than half of the samples, and lambda-cyhalothrin was not detected in any samples. At two of the sites sampled in 2002 (Colusa Basin Drain 1 and Sacramento Slough), concentrations of molinate were similar, but thiobencarb concentrations differed by a factor of five. Although concentrations cannot be estimated directly from application amounts in different watersheds, the ratio of molinate to thiobencarb concentrations can be compared with the ratio of molinate to thiobencarb use in the basins. The higher concentration ratio in the Sacramento Slough Basin, compared with the ratio in the basin area feeding the Colusa Basin Drain 1, is consistent with the higher use ratio, suggesting that differences in application amounts can explain the observed concentration differences. The samples from the downstream site (Tower) sampled in 2002 had the lowest concentrations of pesticides. Performance goals were exceeded for either molinate or thiobencarb in six samples from the upstream sites, but not in any samples from the downstream Tower site. In 2003, concentrations at upstream sites were much lower than the previous year with only one sample containing thiobencarb at a concentration above the performance goal. Lower concentrations could be partially due to delays in rice planting and pesticide application owing to spring rainstorms. Historical data is available on peak concentrations of molinate and thiobencarb measured at Colusa Basin Drain 5 (one of our sites in 2003) since 1981. Implementing holding times for pesticide-treated rice field water in the early 1980s succeeded in decreasing concentrations in surface waters. Detailed pesticide use data is available since 1991 and changing use patterns for molinate and thiobencarb can explain some, but not all, of the trends in peak pesticide concentrations. A stronger relationship is seen between the lengths of time that performance goals were exceeded and the amount of a pesticide applied within a basin. Different extraction and analytical techniques were used to improve the recovery and lower the method detection limit for lambda-cyhalothrin. Recoveries of lambda-cyhalothrin from solid-phase extraction cartridges typically vary, so subsamples were processed by liquid-liquid extraction. The advantage of using a larger sample volume (3 L instead of 1 L) to lower detection limits was offset by poor recovery during the cleanup step using an activated carbon column. Results suggest that as the concentrations of dissolved organic carbon in the sample increase, the recovery g

Determination of 4-nonylphenol and 4-octylphenol in human blood samples by high-performance liquid chromatography with multi-electrode electrochemical coulometric-array detection.

PubMed

Inoue, K; Yoshimura, Y; Makino, T; Nakazawa, H

2000-11-01

Alkylphenols can affect human health because they disrupt the endocrine system. In this study, an analytical method for determining trace amounts of 4-nonylphenol (NP) and 4-octylphenol (OP) in human blood samples was developed. Reversed-phase HPLC with multi-electrode electrochemical coulometric-array detection was used for the determination of NP and OP in plasma and serum samples prepared with a solid-phase extraction method. The separation was achieved using an isocratic mobile phase of 0.7% phosphoric acid-acetonitrile with a C18 reversed phase column. The detection limits of NP and OP were 1.0 and 0.5 ng ml-1, respectively. The recoveries of NP and OP added to human plasma samples were above 70.0% with a relative standard deviation of less than 15.5%. The method was found to be applicable to the determination of NP and OP in various human blood samples such as serum and plasma.

Evaluation of heavy metals and polycyclic aromatic hydrocarbons in honeys from different origins.

PubMed

Corredera, Lourdes; Bayarri, Susana; Pérez-Arquillué, Consuelo; Lázaro, Regina; Molino, Francisco; Herrera, Antonio

2014-03-01

A survey of honey samples from different geographical and botanical origins, including some samples collected from a fire-affected area in Spain, was conducted to assess their content of heavy metals and polycyclic aromatic hydrocarbons (PAHs). The levels of the determined toxic elements (Pb, Cd, As, and Sn) were low and were in the range of those reported by other studies. In our work the total amount of heavy metals and Pb was higher in dark honeys than in pale honeys. In the collected samples, no detectable levels of the 15 PAHs studied were found. The obtained data served to assess the levels of heavy metals and PAHs in honey samples from different geographical and environmental origins and to contribute to the scarce data about pollutant content of this matrix. In light of these results, the analyzed samples do not pose any serious concern to human health, and the data obtained in this study could serve to contribute to the establishment of specific maximum limits for honey.

Instrumental neutron activation analysis for studying size-fractionated aerosols

NASA Astrophysics Data System (ADS)

Salma, Imre; Zemplén-Papp, Éva

1999-10-01

Instrumental neutron activation analysis (INAA) was utilized for studying aerosol samples collected into a coarse and a fine size fraction on Nuclepore polycarbonate membrane filters. As a result of the panoramic INAA, 49 elements were determined in an amount of about 200-400 μg of particulate matter by two irradiations and four γ-spectrometric measurements. The analytical calculations were performed by the absolute ( k0) standardization method. The calibration procedures, application protocol and the data evaluation process are described and discussed. They make it possible now to analyse a considerable number of samples, with assuring the quality of the results. As a means of demonstrating the system's analytical capabilities, the concentration ranges, median or mean atmospheric concentrations and detection limits are presented for an extensive series of aerosol samples collected within the framework of an urban air pollution study in Budapest. For most elements, the precision of the analysis was found to be beyond the uncertainty represented by the sampling techniques and sample variability.

Minimal-assumption inference from population-genomic data

NASA Astrophysics Data System (ADS)

Weissman, Daniel; Hallatschek, Oskar

Samples of multiple complete genome sequences contain vast amounts of information about the evolutionary history of populations, much of it in the associations among polymorphisms at different loci. Current methods that take advantage of this linkage information rely on models of recombination and coalescence, limiting the sample sizes and populations that they can analyze. We introduce a method, Minimal-Assumption Genomic Inference of Coalescence (MAGIC), that reconstructs key features of the evolutionary history, including the distribution of coalescence times, by integrating information across genomic length scales without using an explicit model of recombination, demography or selection. Using simulated data, we show that MAGIC's performance is comparable to PSMC' on single diploid samples generated with standard coalescent and recombination models. More importantly, MAGIC can also analyze arbitrarily large samples and is robust to changes in the coalescent and recombination processes. Using MAGIC, we show that the inferred coalescence time histories of samples of multiple human genomes exhibit inconsistencies with a description in terms of an effective population size based on single-genome data.

[Confirmation of West Nile virus seroreactivity in central nervous system infections of unknown etiology from Ankara Province, Central Anatolia, Turkey].

PubMed

Ergünay, Koray; Özkul, Aykut

2011-04-01

West Nile virus (WNV) infections may trigger febrile conditions and/or neuroinvasive disease in a portion of the exposed individuals. Serosurveillance data from various regions of Turkey indicate WNV activity. The aim of this study was to confirm the antibody specificity of the serum samples via virus neutralization assay, previously reported to be reactive for WNV IgM. The samples originated from two individuals with the preliminary diagnosis of aseptic meningitis/encephalitis of unknown etiology in 2009 and had been classified as probable WNV infections. Cerebrospinal fluid and sera samples of these patients had been evaluated as negative for WNV RNA and IgG antibodies. Only one serum sample could be included in the neutralization assay due to the limited amounts in the current investigation. The sample was observed as positive in dilutions of 1/20 and 1/40, thus confirming the diagnosis of WNV-related central nervous system infection in a 62 year-old female patient from Ankara, Central Anatolia, Turkey.

Preservation of Liquid Biological Samples

NASA Technical Reports Server (NTRS)

Putcha, Lakshmi (Inventor); Nimmagudda, Ramalingeshwara R. (Inventor)

2000-01-01

The present invention provides a method of preserving a liquid biological sample, comprising the step of: contacting said liquid biological sample with a preservative comprising, sodium benzoate in an amount of at least about 0.15% of the sample (weight/volume) and citric acid in an amount of at least about 0.025% of the sample (weight/volume).

Effects of sample injection amount and time-of-flight mass spectrometric detection dynamic range on metabolome analysis by high-performance chemical isotope labeling LC-MS.

PubMed

Zhou, Ruokun; Li, Liang

2015-04-06

The effect of sample injection amount on metabolome analysis in a chemical isotope labeling (CIL) liquid chromatography-mass spectrometry (LC-MS) platform was investigated. The performance of time-of-flight (TOF) mass spectrometers with and without a high-dynamic-range (HD) detection system was compared in the analysis of (12)C2/(13)C2-dansyl labeled human urine samples. An average of 1635 ± 21 (n = 3) peak pairs or putative metabolites was detected using the HD-TOF-MS, compared to 1429 ± 37 peak pairs from a conventional or non-HD TOF-MS. In both instruments, signal saturation was observed. However, in the HD-TOF-MS, signal saturation was mainly caused by the ionization process, while in the non-HD TOF-MS, it was caused by the detection process. To extend the MS detection range in the non-HD TOF-MS, an automated switching from using (12)C to (13)C-natural abundance peaks for peak ratio calculation when the (12)C peaks are saturated has been implemented in IsoMS, a software tool for processing CIL LC-MS data. This work illustrates that injecting an optimal sample amount is important to maximize the metabolome coverage while avoiding the sample carryover problem often associated with over-injection. A TOF mass spectrometer with an enhanced detection dynamic range can also significantly increase the number of peak pairs detected. In chemical isotope labeling (CIL) LC-MS, relative metabolite quantification is done by measuring the peak ratio of a (13)C2-/(12)C2-labeled peak pair for a given metabolite present in two comparative samples. The dynamic range of peak ratio measurement does not need to be very large, as only subtle changes of metabolite concentrations are encountered in most metabolomic studies where relative metabolome quantification of different groups of samples is performed. However, the absolute concentrations of different metabolites can be very different, requiring a technique to provide a wide detection dynamic range to allow the detection of as many peak pairs as possible. In this work, we demonstrated that controlling the sample injection amount into LC-MS was critical to achieve the optimal detectability while avoiding sample carry-over problem. In addition, the use of a high-dynamic-range TOF system increased the number of peak pairs detected, compared to a conventional TOF system. We also investigated the ionization and detection saturation factors limiting the dynamic range of detection. This article is part of a Special Issue entitled: Protein dynamics in health and disease. Guest Editors: Pierre Thibault and Anne-Claude Gingras. Copyright © 2014 Elsevier B.V. All rights reserved.

Amino acid precursors in lunar fines - Limits to the contribution of jet exhaust

NASA Technical Reports Server (NTRS)

Fox, S. W.; Harada, K.; Hare, P. E.

1976-01-01

A sample of lunar fines collected at a maximum distance, 6.5 km, from the descent engine on Apollo 17 has been analyzed for total amino acids obtainable by hydrolysis of aqueous extracts. The minimum amounts of amino acids, calculated for a disk of 6 km radius are 10,000 to 100,000 times those which could be contributed by the lunar module jet exhaust, on the basis of conservatively limiting assumptions. The amino acids thus obtained are not explainable as due to chemical or biological contamination; their source is accordingly inferred as lunar. Under the conditions of hydrolysis of lunar extracts, cyanide is found to be converted, almost exclusively to glycine, to an extent of 0.0001.

Studies of Be migration in the JET tokamak using AMS with 10Be marker

NASA Astrophysics Data System (ADS)

Bykov, I.; Bergsåker, H.; Possnert, G.; Zhou, Y.; Heinola, K.; Pettersson, J.; Conroy, S.; Likonen, J.; Petersson, P.; Widdowson, A.

2016-03-01

The JET tokamak is operated with beryllium limiter tiles in the main chamber and tungsten coated carbon fiber composite tiles and solid W tiles in the divertor. One important issue is how wall materials are migrating during plasma operation. To study beryllium redistribution in the main chamber and in the divertor, a 10Be enriched limiter tile was installed prior to plasma operations in 2011-2012. Methods to take surface samples have been developed, an abrasive method for bulk Be tiles in the main chamber, which permits reuse of the tiles, and leaching with hot HCl to remove all Be deposited at W coated surfaces in the divertor. Quantitative analysis of the total amount of Be in cm2 sized samples was made with inductively coupled plasma atomic emission spectroscopy (ICP-AES). The 10Be/9Be ratio in the samples was measured with accelerator mass spectrometry (AMS). The experimental setup and methods are described in detail, including sample preparation, measures to eliminate contributions in AMS from the 10B isobar, possible activation due to plasma generated neutrons and effects of diffusive isotope mixing. For the first time marker concentrations are measured in the divertor deposits. They are in the range 0.4-1.2% of the source concentration, with moderate poloidal variation.

Label-free virus detection using silicon photonic microring resonators

PubMed Central

McClellan, Melinda S.; Domier, Leslie L; Bailey, Ryan C.

2013-01-01

Viruses represent a continual threat to humans through a number of mechanisms, which include disease, bioterrorism, and destruction of both plant and animal food resources. Many contemporary techniques used for the detection of viruses and viral infections suffer from limitations such as the need for extensive sample preparation or the lengthy window between infection and measurable immune response, for serological methods. In order to develop a method that is fast, cost-effective, and features reduced sample preparation compared to many other virus detection methods, we report the application of silicon photonic microring resonators for the direct, label-free detection of intact viruses in both purified samples as well as in a complex, real-world analytical matrix. As a model system, we demonstrate the quantitative detection of Bean pod mottle virus, a pathogen of great agricultural importance, with a limit of detection of 10 ng/mL. By simply grinding a small amount of leaf sample in buffer with a mortar and pestle, infected leaves can be identified over a healthy control with a total analysis time of less than 45 min. Given the inherent scalability and multiplexing capability of the semiconductor-based technology, we feel that silicon photonic microring resonators are well-positioned as a promising analytical tool for a number of viral detection applications. PMID:22138465

Digital droplet multiple displacement amplification (ddMDA) for whole genome sequencing of limited DNA samples

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

Rhee, Minsoung; Light, Yooli K.; Meagher, Robert J.

Here, multiple displacement amplification (MDA) is a widely used technique for amplification of DNA from samples containing limited amounts of DNA (e.g., uncultivable microbes or clinical samples) before whole genome sequencing. Despite its advantages of high yield and fidelity, it suffers from high amplification bias and non-specific amplification when amplifying sub-nanogram of template DNA. Here, we present a microfluidic digital droplet MDA (ddMDA) technique where partitioning of the template DNA into thousands of sub-nanoliter droplets, each containing a small number of DNA fragments, greatly reduces the competition among DNA fragments for primers and polymerase thereby greatly reducing amplification bias. Consequently,more » the ddMDA approach enabled a more uniform coverage of amplification over the entire length of the genome, with significantly lower bias and non-specific amplification than conventional MDA. For a sample containing 0.1 pg/μL of E. coli DNA (equivalent of ~3/1000 of an E. coli genome per droplet), ddMDA achieves a 65-fold increase in coverage in de novo assembly, and more than 20-fold increase in specificity (percentage of reads mapping to E. coli) compared to the conventional tube MDA. ddMDA offers a powerful method useful for many applications including medical diagnostics, forensics, and environmental microbiology.« less

Digital droplet multiple displacement amplification (ddMDA) for whole genome sequencing of limited DNA samples

DOE PAGES

Rhee, Minsoung; Light, Yooli K.; Meagher, Robert J.; ...

2016-05-04

Here, multiple displacement amplification (MDA) is a widely used technique for amplification of DNA from samples containing limited amounts of DNA (e.g., uncultivable microbes or clinical samples) before whole genome sequencing. Despite its advantages of high yield and fidelity, it suffers from high amplification bias and non-specific amplification when amplifying sub-nanogram of template DNA. Here, we present a microfluidic digital droplet MDA (ddMDA) technique where partitioning of the template DNA into thousands of sub-nanoliter droplets, each containing a small number of DNA fragments, greatly reduces the competition among DNA fragments for primers and polymerase thereby greatly reducing amplification bias. Consequently,more » the ddMDA approach enabled a more uniform coverage of amplification over the entire length of the genome, with significantly lower bias and non-specific amplification than conventional MDA. For a sample containing 0.1 pg/μL of E. coli DNA (equivalent of ~3/1000 of an E. coli genome per droplet), ddMDA achieves a 65-fold increase in coverage in de novo assembly, and more than 20-fold increase in specificity (percentage of reads mapping to E. coli) compared to the conventional tube MDA. ddMDA offers a powerful method useful for many applications including medical diagnostics, forensics, and environmental microbiology.« less

Determination of dissolved aluminum in water samples

USGS Publications Warehouse

Afifi, A.A.

1983-01-01

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

Extraction of 3,4,4'-Trichlorocarbanilide from Rat Fecal Samples for Determination by High Pressure Liquid Chromatography-Tandem Mass Spectrometry.

PubMed

Kennedy, Rebekah C; Fling, Russell R; Terry, Paul D; Menn, Fu-Min; Chen, Jiangang; Borman, Christopher J

2015-07-15

Triclocarban (3,4,4'-Trichlorocarbanilide; TCC) in the environment has been well documented. Methods have been developed to monitor TCC levels from various matrices including water, sediment, biosolids, plants, blood and urine; however, no method has been developed to document the concentration of TCC in fecal content after oral exposure in animal studies. In the present study, we developed and validated a method that uses liquid extraction coupled with HPLC-MS/MS determination to measure TCC in feces. The limit of detection and limit of quantitation in control rats without TCC exposure was 69.0 ng/g and 92.9 ng/g of feces, respectively. The base levels of TCC in feces were lower than LOD. At 12 days of treatment, the fecal TCC concentration increased to 2220 µg/g among 0.2% w/w exposed animals. The concentration in fecal samples decreased over the washout period in 0.2% w/w treated animals to 0.399 µ/g feces after exposure was removed for 28 days. This method required a small amount of sample (0.1 g) with simple sample preparation. Given its sensitivity and efficiency, this method may be useful for monitoring TCC exposure in toxicological studies of animals.

Solid sampling determination of total fluorine in baby food samples by high-resolution continuum source graphite furnace molecular absorption spectrometry.

PubMed

Ozbek, Nil; Akman, Suleyman

2016-11-15

This study describes the applicability of solid sampling technique for the determination of fluorine in various baby foods via molecular absorption of calcium monofluoride generated in a graphite furnace of high-resolution continuum source atomic absorption spectrometry. Fluorine was determined at CaF wavelength, 606.440nm in a graphite tube applying a pyrolysis temperature of 1000°C and a molecule forming temperature of 2200°C. The limit of detection and characteristic mass of the method were 0.20ng and 0.17ng of fluorine, respectively. The fluorine concentrations determined in standard reference sample (bush branches and leaves) were in good agreement with the certified values. By applying the optimized parameters, the concentration of fluorine in various baby foods were determined. The fluorine concentrations were ranged from

Comparing Cumberland With Other Samples Analyzed by Curiosity

NASA Image and Video Library

2014-12-16

This graphic offers comparisons between the amount of an organic chemical named chlorobenzene detected in the Cumberland rock sample and amounts of it in samples from three other Martian surface targets analyzed by NASA Curiosity Mars rover.

Graphite furnace atomic absorption spectrometric detection of vanadium in water and food samples after solid phase extraction on multiwalled carbon nanotubes.

PubMed

Wadhwa, Sham Kumar; Tuzen, Mustafa; Gul Kazi, Tasneem; Soylak, Mustafa

2013-11-15

Vanadium(V) ions as 8-hydroxyquinoline chelates were loaded on multiwalled carbon nanotubes (MWNTs) in a mini chromatographic column. Vanadium was determined by graphite furnace atomic absorption spectrometry (GFAAS). Various analytical parameters including pH of the working solutions, amounts of 8-hydroxyquinoline, eluent type, sample volume, and flow rates were investigated. The effects of matrix ions and some transition metals were also studied. The column can be reused 250 times without any loss in its sorption properties. The preconcentration factor was found as 100. Detection limit (3 s) and limit of quantification (10 s) for the vanadium in the optimal conditions were observed to be 0.012 µg L(-1) and 0.040 μg L(-1), respectively. The capacity of adsorption was 9.6 mg g(-1). Relative standard deviation (RSD) was found to be 5%. The validation of the method was confirmed by using NIST SRM 1515 Apple leaves, NIST SRM 1570a Spinach leaves and GBW 07605 Tea certified reference materials. The procedure was applied to the determination of vanadium in tap water and bottled drinking water samples. The procedure was also successfully applied to microwave digested food samples including black tea, coffee, tomato, cabbage, zucchini, apple and chicken samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Liquid chromatographic determination of microcystins in water samples following pre-column excimer fluorescence derivatization with 4-(1-pyrene)butanoic acid hydrazide.

PubMed

Hayama, Tadashi; Katoh, Kenji; Aoki, Takayoshi; Itoyama, Miki; Todoroki, Kenichiro; Yoshida, Hideyuki; Yamaguchi, Masatoshi; Nohta, Hitoshi

2012-11-28

A method to measure the concentrations of microcystins (MCs) in water samples has been developed by incorporating pre-column fluorescence derivatization and liquid chromatography (LC). A solid-phase extraction for pretreatment was used to extract the MCs in water samples. The MCs were derivatized with excimer-forming 4-(1-pyrene)butanoic acid hydrazide (PBH). The MCs could then be detected by fluorescence after separation with a pentafluorophenyl (PFP)-modified superficially porous (core shell) particle LC column. The derivatization reactions of MCs with PBH proceeded easily in the presence of 4,6-dimethoxy-1,3,5-triazin-2-yl-4-methylmorpholinium (DMT-MM) as a condensation reagent, and the resulting derivatives could be easily separated on the PFP column. The derivatives were selectively detected at excimer fluorescence wavelengths (440-540 nm). The instrument detection limit and the instrument quantification limit of the MCs standards were 0.4-1.2 μg L(-1) and 1.4-3.9 μg L(-1), respectively. The method was validated at 0.1 and 1.0 μg L(-1) levels in tap and pond water samples, and the recovery of MCs was between 67 and 101% with a relative standard deviation of 11%. The proposed method can be used to quantify trace amounts of MCs in water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Quality of ground water in Clark County, Washington, 1988

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

Turney, G.L.

1990-01-01

Water samples were collected from 76 wells throughout Clark County, in southwest Washington, during April and May 1988, and were analyzed from concentrations of major ions, silica, nitrate, phosphorus, aluminum, manganese, radon, and bacteria. Samples from 20 wells were analyzed for concentrations of trace elements and organic compounds, including most of those on the US Environmental Protection Agency (USEPA) priority pollutant list. Dissolved solids concentrations range from 12 to 245 mg/L, with a median concentration of 132 mg/L. The major dissolved constituents are calcium, bicarbonate, and silica, and, in some samples, sodium. Nitrate concentrations exceeded 1.0 mg/L throughout the Vancouvermore » urban area, and were as large as 6.7 mg/L. Comparison with limited historical data indicates that nitrate concentrations were somewhat correlated, possibly indicating similar sources. Volatile organic compound, including tetrachloroethane and 1,1,1-trichloroethane, were detected in samples from three wells in the Vancouver area. Trace amounts of volatile organic compounds were reported in samples from several other wells, but at concentrations too close to analytical detection limits to ascertain that they were in the groundwater. Trace elements and radiochemical constituents were present at small levels indicating natural sources for these constituents. Only pH, turbidity, iron, manganese, and total coliform bacteria had values that did not meet USEPA Drinking Water Standards.« less

Microfluidic paper-based analytical device for particulate metals.

PubMed

Mentele, Mallory M; Cunningham, Josephine; Koehler, Kirsten; Volckens, John; Henry, Charles S

2012-05-15

A microfluidic paper-based analytical device (μPAD) fabricated by wax printing was designed to assess occupational exposure to metal-containing aerosols. This method employs rapid digestion of particulate metals using microliters of acid added directly to a punch taken from an air sampling filter. Punches were then placed on a μPAD, and digested metals were transported to detection reservoirs upon addition of water. These reservoirs contained reagents for colorimetric detection of Fe, Cu, and Ni. Dried buffer components were used to set the optimal pH in each detection reservoir, while precomplexation agents were deposited in the channels between the sample and detection zones to minimize interferences from competing metals. Metal concentrations were quantified from color intensity images using a scanner in conjunction with image processing software. Reproducible, log-linear calibration curves were generated for each metal, with method detection limits ranging from 1.0 to 1.5 μg for each metal (i.e., total mass present on the μPAD). Finally, a standard incineration ash sample was aerosolized, collected on filters, and analyzed for the three metals of interest. Analysis of this collected aerosol sample using a μPAD showed good correlation with known amounts of the metals present in the sample. This technology can provide rapid assessment of particulate metal concentrations at or below current regulatory limits and at dramatically reduced cost.

Patulin in apple-based foods: occurrence and safety evaluation.

PubMed

Beretta, B; Gaiaschi, A; Galli, C L; Restani, P

2000-05-01

Patulin is a mycotoxin produced by certain species of Penicillium and Aspergillus, often detectable in mouldy fruits and their derivatives. On the basis of a PMTDI of 0.4 microgram/kg bw, limit values of 50 micrograms/kg or 50 micrograms/l of patulin have been set in fruit derivatives. To estimate the quantity of patulin that can be taken in with the diet, we analysed by HPLC samples of apples and apple derivatives which are most likely to be contaminated with patulin. In apple juices and in homogenized baby-foods, the mycotoxin concentration was always below the established limits, while in some samples of juice with pulp the mycotoxin content exceeded the safe levels. In rotten apples, not only was the amount of patulin extraordinarily high in the rotten area, but the mycotoxin had also spread to the part unaffected by mould. The data presented in this study indicate that the intake of patulin with apple derivatives is usually below the tolerable level of 0.4 microgram/kg bw/day, but since the patulin content in apples can vary considerably, the quality of fruits used in the production of apple derivatives should be strictly controlled in order not to exceed the safe limits.

Contributions a la caracterisation et a l'amelioration de l'usinabilite de pieces d'acier elaborees par metallurgie des poudres

NASA Astrophysics Data System (ADS)

Boilard, Patrick

Even though powder metallurgy (P/M) is a near net shape process, a large number of parts still require one or more machining operations during the course of their elaboration and/or their finishing. The main objectives of the work presented in this thesis are centered on the elaboration of blends with enhanced machinability, as well as helping with the definition and in the characterization of the machinability of P/M parts. Enhancing machinability can be done in various ways, through the use of machinability additives and by decreasing the amount of porosity of the parts. These different ways of enhancing machinability have been investigated thoroughly, by systematically planning and preparing series of samples in order to obtain valid and repeatable results leading to meaningful conclusions relevant to the P/M domain. Results obtained during the course of the work are divided into three main chapters: (1) the effect of machining parameters on machinability, (2) the effect of additives on machinability, and (3) the development and the characterization of high density parts obtained by liquid phase sintering. Regarding the effect of machining parameters on machinability, studies were performed on parameters such as rotating speed, feed, tool position and diameter of the tool. Optimal cutting parameters are found for drilling operations performed on a standard FC-0208 blend, for different machinability criteria. Moreover, study of material removal rates shows the sensitivity of the machinability criteria for different machining parameters and indicates that thrust force is more regular than tool wear and slope of the drillability curve in the characterization of machinability. The chapter discussing the effect of various additives on machinability reveals many interesting results. First, work carried out on MoS2 additions reveals the dissociation of this additive and the creation of metallic sulphides (namely CuxS sulphides) when copper is present. Results also show that it is possible to reduce the amount of MoS2 in the blend so as to lower the dimensional change and the cost (blend Mo8A), while enhancing machinability and keeping hardness values within the same range (70 HRB). Second, adding enstatite (MgO·SiO2) permits the observation of the mechanisms occurring with the use of this additive. It is found that the stability of enstatite limits the diffusion of graphite during sintering, leading to the presence of free graphite in the pores, thus enhancing machinability. Furthermore, a lower amount of graphite in the matrix leads to a lower hardness, which is also beneficial to machinability. It is also found that the presence of copper enhances the diffusion of graphite, through the formation of a liquid phase during sintering. With the objective of improving machinability by reaching higher densities, blends were developed for densification through liquid phase sintering. High density samples are obtained (>7.5 g/cm3) for blends prepared with Fe-C-P constituents, namely with 0.5%P and 2.4%C. By systematically studying the effect of different parameters, the importance of the chemical composition (mainly the carbon content) and the importance of the sintering cycle (particularly the cooling rate) are demonstrated. Moreover, various heat treatments studied illustrate the different microstructures achievable for this system, showing various amounts of cementite, pearlite and free graphite. Although the machinability is limited for samples containing large amounts of cementite, it can be greatly improved with very slow cooling, leading to graphitization of the carbon in presence of phosphorus. Adequate control of the sintering cycle on samples made from FGS1625 powder leads to the obtention of high density (≥7.0 g/cm 3) microstructures containing various amounts of pearlite, ferrite and free graphite. Obtaining ferritic microstructures with free graphite designed for very high machinability (tool wear <1.0%) or fine pearlitic microstructures with excellent mechanical properties (transverse rupture strength >1600 MPa) is therefore possible. These results show that improvement of machinability through higher densities is limited by microstructure. Indeed, for the studied samples, microstructure is dominant in the determination of machinability, far more important than density, judging by the influence of cementite or of the volume fraction of free graphite on machinability for example. (Abstract shortened by UMI.)

20 CFR 663.420 - Can the duration and amount of ITA's be limited?

Code of Federal Regulations, 2011 CFR

2011-04-01

... limited? 663.420 Section 663.420 Employees' Benefits EMPLOYMENT AND TRAINING ADMINISTRATION, DEPARTMENT OF LABOR ADULT AND DISLOCATED WORKER ACTIVITIES UNDER TITLE I OF THE WORKFORCE INVESTMENT ACT Individual Training Accounts § 663.420 Can the duration and amount of ITA's be limited? (a) Yes, the State or Local...

24 CFR 203.18c - One-time or up-front mortgage insurance premium excluded from limitations on maximum mortgage...

Code of Federal Regulations, 2010 CFR

2010-04-01

... insurance premium excluded from limitations on maximum mortgage amounts. 203.18c Section 203.18c Housing and...-front mortgage insurance premium excluded from limitations on maximum mortgage amounts. After... LOAN INSURANCE PROGRAMS UNDER NATIONAL HOUSING ACT AND OTHER AUTHORITIES SINGLE FAMILY MORTGAGE...

24 CFR 203.18c - One-time or up-front mortgage insurance premium excluded from limitations on maximum mortgage...

Code of Federal Regulations, 2011 CFR

2011-04-01

... insurance premium excluded from limitations on maximum mortgage amounts. 203.18c Section 203.18c Housing and...-front mortgage insurance premium excluded from limitations on maximum mortgage amounts. After... LOAN INSURANCE PROGRAMS UNDER NATIONAL HOUSING ACT AND OTHER AUTHORITIES SINGLE FAMILY MORTGAGE...

Direct determination of lead in biological samples by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) after furnace-fusion in the sample cuvette-tungsten boat furnace.

PubMed

Okamoto, Y

2000-06-01

The newly conceived electrothermal vaporization (ETV) system using a tungsten boat furnace (TBF) sample cuvette was designed for the direct analysis of solid samples with detection by inductively coupled plasma mass spectrometry (ICP-MS). Into this small sample cuvette, a solid mixture of the biological samples and diammonium hydrogenphosphate powder as a fusion flux was placed and situated on a TBF. Tetramethylammonium hydroxide solution was added to the mixture. After the on-furnace digestion had been completed, the analyte in the cuvette was vaporized and introduced into the ICP mass spectrometer. The solid samples were analyzed by using a calibration curve prepared from the aqueous standard solutions. The detection limit was estimated to be 5.1 pg of lead, which corresponds to 10.2 ng g(-1) of lead in solid samples when a prepared sample amount of 1.0 mg was applied. The relative standard deviation for 8 replicate measurements obtained with 100 pg of lead was calculated to be 6.5%. The analytical results for various biological samples are described.

Pesticide concentrations in snail kite eggs and nestlings in Florida

USGS Publications Warehouse

Sykes, P.W.

1985-01-01

From 1970-1977, unhatched snail kite eggs and young that were found dead at nests in Florida were analyzed by gas chromatography for residues of organochlorine pollutants. The 1970 and 1974 material showed measurable amounts of p,p'-DDE, p,p'-DDD, p,p'-DDT, and dieldrin. Dieldrin and polychlorinated biphenyl (PCB) residues were less than 0.1 ppm in the eggs and were detected in only one sample of muscle tissue at 0.11 ppm. Concentrations in ppm wet weight of p,p'-DDE, p,p' DDD, p,p'-DDT, dieldrin, and PCB for two samples of muscle and three of brain tissue (all 1977 material) were not detected at the limit of quantification (0.05 ppm).

Sensitive and affordable diagnostic assay for the quantitative detection of anaplastic lymphoma kinase (ALK) alterations in patients with non-small cell lung cancer.

PubMed

Dama, Elisa; Tillhon, Micol; Bertalot, Giovanni; de Santis, Francesca; Troglio, Flavia; Pessina, Simona; Passaro, Antonio; Pece, Salvatore; de Marinis, Filippo; Dell'Orto, Patrizia; Viale, Giuseppe; Spaggiari, Lorenzo; Di Fiore, Pier Paolo; Bianchi, Fabrizio; Barberis, Massimo; Vecchi, Manuela

2016-06-14

Accurate detection of altered anaplastic lymphoma kinase (ALK) expression is critical for the selection of lung cancer patients eligible for ALK-targeted therapies. To overcome intrinsic limitations and discrepancies of currently available companion diagnostics for ALK, we developed a simple, affordable and objective PCR-based predictive model for the quantitative measurement of any ALK fusion as well as wild-type ALK upregulation. This method, optimized for low-quantity/-quality RNA from FFPE samples, combines cDNA pre-amplification with ad hoc generated calibration curves. All the models we derived yielded concordant predictions when applied to a cohort of 51 lung tumors, and correctly identified all 17 ALK FISH-positive and 33 of the 34 ALK FISH-negative samples. The one discrepant case was confirmed as positive by IHC, thus raising the accuracy of our test to 100%. Importantly, our method was accurate when using low amounts of input RNA (10 ng), also in FFPE samples with limited tumor cellularity (5-10%) and in FFPE cytology specimens. Thus, our test is an easily implementable diagnostic tool for the rapid, efficacious and cost-effective screening of ALK status in patients with lung cancer.

Determination of thiopental in urine sample with high-performance liquid chromatography using iodine-azide reaction as a postcolumn detection system.

PubMed

Zakrzewski, Robert; Ciesielski, Witold

2005-09-25

The reaction between iodine and azide ions induced by thiopental was utilized as a postcolumn reaction for chromatographic determination of thiopental. The method is based on the separation of thiopental on an Nova-Pak CN HP column with an acetonitrile-aqueous solution of sodium azide as a mobile phase, followed by spectrophotometric measurement of the residual iodine (lambda=350 nm) from the postcolumn iodine-azide reaction induced by thiopental after mixing an iodine solution containing iodide ions with the column effluent containing azide ions and thiopental. Chromatograms obtained for thiopental showed negative peaks as a result of the decrease in background absorbance. The detection limit (defined as S/N=3) was 20 nM (0.4 pmol injected amount) for thiopental. Calibration graphs, plotted as peak area versus concentrations, were linear from 40 nM. The elaborated method was applied to determine thiopental in urine samples. The detection limit (defined as S/N=3) was 0.025 nmol/ml urine. Calibration graphs, plotted as peak area versus concentrations, were linear from 0.05 nmol/ml urine. Authentic urine samples were analyzed, thiopental was determined at nmol/ml urine level.

Determination of mutagenic amines in water and food samples by high pressure liquid chromatography with amperometric detection using a multiwall carbon nanotubes-glassy carbon electrode.

PubMed

Bueno, Ana María; Marín, Miguel Ángel; Contento, Ana María; Ríos, Ángel

2016-02-01

A chromatographic method, using amperometric detection, for the sensitive determination of six representative mutagenic amines was developed. A glassy carbon electrode (GCE), modified with multiwall carbon nanotubes (GCE-CNTs), was prepared and its response compared to a conventional glassy carbon electrode. The chromatographic method (HPLC-GCE-CNTs) allowed the separation and the determination of heterocyclic aromatic amines (HAAs) classified as mutagenic amines by the International Agency for Research of Cancer. The new electrode was systematically studied in terms of stability, sensitivity, and reproducibility. Statistical analysis of the obtained data demonstrated that the modified electrode provided better sensitivity than the conventional unmodified ones. Detection limits were in the 3.0 and 7.5 ng/mL range, whereas quantification limits ranged between 9.5 and 25.0 ng/mL were obtained. The applicability of the method was demonstrated by the determination of the amines in several types of samples (water and food samples). Recoveries indicate very good agreement between amounts added and those found for all HAAs (recoveries in the 92% and 105% range). Copyright © 2015 Elsevier Ltd. All rights reserved.

Application of relativistic electrons for the quantitative analysis of trace elements

NASA Astrophysics Data System (ADS)

Hoffmann, D. H. H.; Brendel, C.; Genz, H.; Löw, W.; Richter, A.

1984-04-01

Particle induced X-ray emission methods (PIXE) have been extended to relativistic electrons to induce X-ray emission (REIXE) for quantitative trace-element analysis. The electron beam (20 ≤ E0≤ 70 MeV) was supplied by the Darmstadt electron linear accelerator DALINAC. Systematic measurements of absolute K-, L- and M-shell ionization cross sections revealed a scaling behaviour of inner-shell ionization cross sections from which X-ray production cross sections can be deduced for any element of interest for a quantitative sample investigation. Using a multielemental mineral monazite sample from Malaysia the sensitivity of REIXE is compared to well established methods of trace-element analysis like proton- and X-ray-induced X-ray fluorescence analysis. The achievable detection limit for very heavy elements amounts to about 100 ppm for the REIXE method. As an example of an application the investigation of a sample prepared from manganese nodules — picked up from the Pacific deep sea — is discussed, which showed the expected high mineral content of Fe, Ni, Cu and Ti, although the search for aliquots of Pt did not show any measurable content within an upper limit of 250 ppm.

A nonlethal sampling method to obtain, generate and assemble whole blood transcriptomes from small, wild mammals.

PubMed

Huang, Zixia; Gallot, Aurore; Lao, Nga T; Puechmaille, Sébastien J; Foley, Nicole M; Jebb, David; Bekaert, Michaël; Teeling, Emma C

2016-01-01

The acquisition of tissue samples from wild populations is a constant challenge in conservation biology, especially for endangered species and protected species where nonlethal sampling is the only option. Whole blood has been suggested as a nonlethal sample type that contains a high percentage of bodywide and genomewide transcripts and therefore can be used to assess the transcriptional status of an individual, and to infer a high percentage of the genome. However, only limited quantities of blood can be nonlethally sampled from small species and it is not known if enough genetic material is contained in only a few drops of blood, which represents the upper limit of sample collection for some small species. In this study, we developed a nonlethal sampling method, the laboratory protocols and a bioinformatic pipeline to sequence and assemble the whole blood transcriptome, using Illumina RNA-Seq, from wild greater mouse-eared bats (Myotis myotis). For optimal results, both ribosomal and globin RNAs must be removed before library construction. Treatment of DNase is recommended but not required enabling the use of smaller amounts of starting RNA. A large proportion of protein-coding genes (61%) in the genome were expressed in the blood transcriptome, comparable to brain (65%), kidney (63%) and liver (58%) transcriptomes, and up to 99% of the mitogenome (excluding D-loop) was recovered in the RNA-Seq data. In conclusion, this nonlethal blood sampling method provides an opportunity for a genomewide transcriptomic study of small, endangered or critically protected species, without sacrificing any individuals. © 2015 John Wiley & Sons Ltd.

Pesticide residues analysis in water samples of Nagarpur and Saturia Upazila, Bangladesh

NASA Astrophysics Data System (ADS)

Hasanuzzaman, M.; Rahman, M. A.; Islam, M. S.; Salam, M. A.; Nabi, M. R.

2018-03-01

Pesticides used to protect the crops from pest attack in the agricultural fields pose harmful effect to the non-target organisms such as human and many other aquatic and terrestrial organisms either directly or indirectly through food chain. The present study was conducted to monitor a total of seven pesticide residues under organochlorine, organophosphorus and carbamate pesticides in three different sources of pond water, paddy field water and tube-well water from Nagarpur Upazila and paddy field water in the company of Dhaleshwari and Gazikhali river water from Saturia Upazila, Bangladesh. A total of 40 water samples were analyzed using high-performance liquid chromatography equipped with ultraviolet detector. Among the organophosphorus pesticides, diazinon was detected in eight water samples at a concentration ranging from 4.11 to 257.91 μg/l whereas, malathion was detected only in one water sample at a concentration of 84.64 μg/l and chlorpyrifos pesticide was also detected only in one water sample and the concentration was 37.3 μg/l. Trace amount of carbaryl was identified but it was below the detection limit. None of the tested water samples was found to be contaminated with DDT or its metabolites (DDE and DDD). The water samples contaminated with the suspected pesticides were above the acceptable limit except for the fish pond samples of Sahabatpur and Dubaria union. To control the misuse of pesticides and to reduce the possible health risk, appropriate control systems of pests such as integrated pest management system should be implemented immediately by the authorities of the country.

Contribution of acidic components to the total acid number (TAN) of bio-oil

DOE PAGES

Park, Lydia K-E.; Liu, Jiaojun; Yiacoumi, Sotira; ...

2017-03-28

Bio-oil or pyrolysis oil — a product of thermochemical decomposition of biomass under oxygen-limited conditions — holds great potential to be a substitute for nonrenewable fossil fuels. But, its high acidity, which is primarily due to the degradation of hemicelluloses, limits its applications. For the evaluation of bio-oil production and treatment, it is essential to accurately measure the acidity of bio-oil. The total acid number (TAN), which is defined as the amount of potassium hydroxide needed to titrate one gram of a sample and has been established as an ASTM method to measure the acidity of petroleum products, has beenmore » employed to investigate the acidity of bio-oil. The TAN values of different concentrations of bio-oil components such as standard solutions of acetic acid, propionic acid, vanillic acid, hydroxybenzoic acid, syringic acid, hydroxymethylfurfural, and phenol were analyzed according to the ASTM D664 standard method. Our method showed the same linear relationship between the TAN values and the molar concentrations of acetic, propionic, and hydroxybenzoic acids. A different linear relationship was found for vanillic acid, due to the presence of multiple functional groups that can contribute to the TAN value. Furthermore, the influence of the titration solvent on the TAN values has been determined by comparing the TAN values and titration curves obtained from the standard method with results from the TAN analysis in aqueous environment and with equilibrium modeling results. Aqueous bio-oil samples with a known amount of acetic acid added were also analyzed. The additional acetic acid in bio-oil samples caused a proportional increase in the TAN values. These results of this research indicate that the TAN value of a sample with acids acting as monoprotic acids in the titration solvent can be converted to the molar concentration of total acids. For a sample containing acids that act as diprotic and polyprotic acids, however, its TAN value cannot be simply converted to the molar concentration of total acids because these acids have a stronger contribution to the TAN values than the contribution of monoprotic acids.« less

Contribution of acidic components to the total acid number (TAN) of bio-oil

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

Park, Lydia K-E.; Liu, Jiaojun; Yiacoumi, Sotira

Bio-oil or pyrolysis oil — a product of thermochemical decomposition of biomass under oxygen-limited conditions — holds great potential to be a substitute for nonrenewable fossil fuels. But, its high acidity, which is primarily due to the degradation of hemicelluloses, limits its applications. For the evaluation of bio-oil production and treatment, it is essential to accurately measure the acidity of bio-oil. The total acid number (TAN), which is defined as the amount of potassium hydroxide needed to titrate one gram of a sample and has been established as an ASTM method to measure the acidity of petroleum products, has beenmore » employed to investigate the acidity of bio-oil. The TAN values of different concentrations of bio-oil components such as standard solutions of acetic acid, propionic acid, vanillic acid, hydroxybenzoic acid, syringic acid, hydroxymethylfurfural, and phenol were analyzed according to the ASTM D664 standard method. Our method showed the same linear relationship between the TAN values and the molar concentrations of acetic, propionic, and hydroxybenzoic acids. A different linear relationship was found for vanillic acid, due to the presence of multiple functional groups that can contribute to the TAN value. Furthermore, the influence of the titration solvent on the TAN values has been determined by comparing the TAN values and titration curves obtained from the standard method with results from the TAN analysis in aqueous environment and with equilibrium modeling results. Aqueous bio-oil samples with a known amount of acetic acid added were also analyzed. The additional acetic acid in bio-oil samples caused a proportional increase in the TAN values. These results of this research indicate that the TAN value of a sample with acids acting as monoprotic acids in the titration solvent can be converted to the molar concentration of total acids. For a sample containing acids that act as diprotic and polyprotic acids, however, its TAN value cannot be simply converted to the molar concentration of total acids because these acids have a stronger contribution to the TAN values than the contribution of monoprotic acids.« less

Determination of palladium and platinum by atomic absorption

USGS Publications Warehouse

Schnepfe, M.M.; Grimaldi, F.S.

1969-01-01

Palladium and platinum are determined by atomic absorption after fire-assay concentration into a gold bead. The limit of determination is ~0??06 ppm in a 20-g sample. Serious depressive interelement interferences are removed by buffering the solutions with a mixture of cadmium and copper sulphates with cadmium and copper concentrations each at 0??5%. Substantial amounts of Ag, Al, Au, Bi, Ca, Co, Cr, Fe, Hg, K, La, Mg, Mn, Mo, Na, Ni, Pb, Te, Ti, V, Y, Zn, and the platinum metals do not interfere in the atomic-absorption determination. ?? 1969.

Validation of the analysis of respirable crystalline silica (quartz) in foams used with CIP 10-R samplers.

PubMed

Eypert-Blaison, Céline; Moulut, Jean-Claude; Lecaque, Thierry; Marc, Florian; Kauffer, Edmond

2011-05-01

Sampling the respirable fraction to measure exposure to crystalline silica is most often carried out using cyclones. However, low flow rates (<4 l min(-1)) and continuing improvement in workplace hygiene means less and less material is sampled for analysis, resulting in increased analytical uncertainty. Use of the CIP 10-R sampler, working at a flow rate of 10 l min(-1), is one attempt to solve current analytical difficulties. To check the ability of the analysis of quartz sampled on foams, known amounts of quartz associated with a matrix have been injected into foams. The results obtained show that the proposed protocol, with prior acid attack and ashing of the foams, satisfies the recommendations of EN 482 Standard [CEN. (2006) Workplace atmospheres-general requirements for the performance of procedures for the measurements of chemical agents. Brussels, Belgium: EN 482 Comité Européen de normalization (CEN).], namely an expanded uncertainty of <50% for quartz weights between 0.1 and 0.5 times the 8-h exposure limit value and <30% for quartz weights between 0.5 and 2 times the 8-h exposure limit value, assuming an exposure limit value equal to 0.1 mg m(-3). Results obtained show that the 101 reflection line allows a quartz quantity of the order of 25 μg to be satisfactorily measured, which corresponds to a 10th of the exposure limit value, assuming an exposure limit value of 0.05 mg m(-3). In this case, the 100 and 112 reflection lines with expanded uncertainties of ~50% would also probably lead to satisfactory quantification. Particular recommendations are also proposed for the preparation of calibration curves to improve the method.

Implementing an Accurate and Rapid Sparse Sampling Approach for Low-Dose Atomic Resolution STEM Imaging

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

Kovarik, Libor; Stevens, Andrew J.; Liyu, Andrey V.

Aberration correction for scanning transmission electron microscopes (STEM) has dramatically increased spatial image resolution for beam-stable materials, but it is the sample stability rather than the microscope that often limits the practical resolution of STEM images. To extract physical information from images of beam sensitive materials it is becoming clear that there is a critical dose/dose-rate below which the images can be interpreted as representative of the pristine material, while above it the observation is dominated by beam effects. Here we describe an experimental approach for sparse sampling in the STEM and in-painting image reconstruction in order to reduce themore » electron dose/dose-rate to the sample during imaging. By characterizing the induction limited rise-time and hysteresis in scan coils, we show that sparse line-hopping approach to scan randomization can be implemented that optimizes both the speed of the scan and the amount of the sample that needs to be illuminated by the beam. The dose and acquisition time for the sparse sampling is shown to be effectively decreased by factor of 5x relative to conventional acquisition, permitting imaging of beam sensitive materials to be obtained without changing the microscope operating parameters. As a result, the use of sparse line-hopping scan to acquire STEM images is demonstrated with atomic resolution aberration corrected Z-contrast images of CaCO 3, a material that is traditionally difficult to image by TEM/STEM because of dose issues.« less

Implementing an Accurate and Rapid Sparse Sampling Approach for Low-Dose Atomic Resolution STEM Imaging

DOE PAGES

Kovarik, Libor; Stevens, Andrew J.; Liyu, Andrey V.; ...

2016-10-17

Aberration correction for scanning transmission electron microscopes (STEM) has dramatically increased spatial image resolution for beam-stable materials, but it is the sample stability rather than the microscope that often limits the practical resolution of STEM images. To extract physical information from images of beam sensitive materials it is becoming clear that there is a critical dose/dose-rate below which the images can be interpreted as representative of the pristine material, while above it the observation is dominated by beam effects. Here we describe an experimental approach for sparse sampling in the STEM and in-painting image reconstruction in order to reduce themore » electron dose/dose-rate to the sample during imaging. By characterizing the induction limited rise-time and hysteresis in scan coils, we show that sparse line-hopping approach to scan randomization can be implemented that optimizes both the speed of the scan and the amount of the sample that needs to be illuminated by the beam. The dose and acquisition time for the sparse sampling is shown to be effectively decreased by factor of 5x relative to conventional acquisition, permitting imaging of beam sensitive materials to be obtained without changing the microscope operating parameters. The use of sparse line-hopping scan to acquire STEM images is demonstrated with atomic resolution aberration corrected Z-contrast images of CaCO3, a material that is traditionally difficult to image by TEM/STEM because of dose issues.« less

Performance of a novel high throughput method for the determination of VX in drinking water samples.

PubMed

Knaack, Jennifer S; Zhou, Yingtao; Magnuson, Matthew; Silvestri, Erin; Johnson, Rudolph C

2013-03-05

VX (O-ethyl-S-(2-diisopropylaminoethyl) methylphosphonothioate) is a highly toxic organophosphorus nerve agent, and even low levels of contamination in water can be harmful. Measurement of low concentrations of VX in aqueous matrixes is possible using an immunomagnetic scavenging technique and detection using liquid chromatography/tandem-mass spectrometry. Performance of the method was characterized in high-performance liquid chromatography (HPLC)-grade water preserved with sodium omadine, an antimicrobial agent, and sodium thiosulfate, a dechlorinating agent, over eight analytical batches with quality control samples analyzed over 10 days. The minimum reportable level was 25 ng/L with a linear dynamic range up to 4.0 μg/L. The mean accuracies for two quality control samples containing VX at concentrations of 0.250 and 2.00 μg/L were 102 ± 3% and 103 ± 6%, respectively. The stability of VX was determined in five tap water samples representing a range of water quality parameters and disinfection practices over a 91 day period. In preserved tap water samples, VX recovery was between 81 and 92% of the fortified amount, 2.0 μg/L, when analyzed immediately after preparation. Recovery of VX decreased to between 31 and 45% of the fortified amount after 91 days, indicating hydrolysis of VX. However, the preservatives minimized the hydrolysis rate to close to the theoretical limit. The ability to detect low concentrations of VX in preserved tap water 91 days after spiking suggests applicability of this method for determining water contamination with VX and utility during environmental remediation.

Determination and assessment of total mercury levels in local, frozen and canned fish in Lebanon.

PubMed

Obeid, Pierre J; El-Khoury, Bilal; Burger, Joanne; Aouad, Samer; Younis, Mira; Aoun, Amal; El-Nakat, John Hanna

2011-01-01

Fish is an important constituent of the Lebanese diet. However, very little attention in our area is given to bring awareness regarding the effect of the toxicity of mercury (Hg) mainly through fish consumption. This study aimed to report analytical data on total mercury levels in several fish species for the first time in thirty years and to also made individuals aware of the presence and danger from exposure to mercury through fish consumption. Fish samples were selected from local Lebanese markets and fisheries and included 94 samples of which were fresh, frozen, processed, and canned fish. All values were reported as microgram of mercury per gram of fish based on wet weight. The level of mercury ranged from 0.0190 to 0.5700 microg/g in fresh samples, 0.0059 to 0.0665 microg/g in frozen samples, and 0.0305 to 0.1190 microg/g in canned samples. The data clearly showed that higher levels of mercury were detected in local fresh fish as opposed to other types thus placing consumers at higher risk from mercury exposure. Moreover, the data revealed that Mallifa (yellowstripe barracuda/Sphyraena chrysotaenia), Sargous (white seabream/Diplodus sargus), Ghobbos (bogue/Boops boops), and shrimp (Penaeus sp.) were among the types containing the highest amounts of mercury. On the other hand, processed fish such as fish fillet, fish burger, small shrimp and crab are found to contain lower levels of mercury and are associated with lower exposure risks to mercury. Lebanese population should therefore, be aware to consume limited amounts of fresh local fish to minimize exposure to mercury.

Calcium Alginate-Caged Multiwalled Carbon Nanotubes Dispersive Microsolid Phase Extraction Combined With Gas Chromatography-Flame Ionization Detection for the Determination of Polycyclic Aromatic Hydrocarbons in Water Samples.

PubMed

Abboud, Ayad Sami; Sanagi, Mohd Marsin; Ibrahim, Wan Aini Wan; Keyon, Aemi S Abdul; Aboul-Enein, Hassan Y

2018-02-01

In this study, caged calcium alginate-caged multiwalled carbon nanotubes dispersive microsolid phase extraction was described for the first time for the extraction of polycyclic aromatic hydrocarbons (PAHs) from water samples prior to gas chromatographic analysis. Fluorene, phenanthrene and fluoranthene were selected as model compounds. The caged calcium alginate-caged multiwalled carbon nanotubes was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy and thermal gravimetry analyses. The effective parameters namely desorption solvent, solvent volume, extraction time, desorption time, the mass of adsorbent and sample volume were optimized. Under the optimum extraction conditions, the developed method showed good linearity in the range of 0.5-50 ng mL-1 (R2 ≥ 0.996), low limits of detection and quantification (0.42-0.22 ng mL-1) (0.73-1.38 ng mL-1) respectively, good relative recoveries (71.2-104.2%) and reproducibility (RSD 1.8-12.4%, n = 3) for the studied PAHs in water sample. With high enrichment factor (1,000), short extraction time (<30 min), low amounts of adsorbent (100 mg) and low amounts of solvent (0.1 mol) have proven that the microsolid phase extraction method based on calcium alginate-caged multiwalled carbon nanotubes are environmentally friendly and convenient extraction method to use as an alternative adsorbent in the simultaneous preconcentration of PAHs from environmental water samples. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Extraction and labeling methods for microarrays using small amounts of plant tissue.

PubMed

Stimpson, Alexander J; Pereira, Rhea S; Kiss, John Z; Correll, Melanie J

2009-03-01

Procedures were developed to maximize the yield of high-quality RNA from small amounts of plant biomass for microarrays. Two disruption techniques (bead milling and pestle and mortar) were compared for the yield and the quality of RNA extracted from 1-week-old Arabidopsis thaliana seedlings (approximately 0.5-30 mg total biomass). The pestle and mortar method of extraction showed enhanced RNA quality at the smaller biomass samples compared with the bead milling technique, although the quality in the bead milling could be improved with additional cooling steps. The RNA extracted from the pestle and mortar technique was further tested to determine if the small quantity of RNA (500 ng-7 microg) was appropriate for microarray analyses. A new method of low-quantity RNA labeling for microarrays (NuGEN Technologies, Inc.) was used on five 7-day-old seedlings (approximately 2.5 mg fresh weight total) of Arabidopsis that were grown in the dark and exposed to 1 h of red light or continued dark. Microarray analyses were performed on a small plant sample (five seedlings; approximately 2.5 mg) using these methods and compared with extractions performed with larger biomass samples (approximately 500 roots). Many well-known light-regulated genes between the small plant samples and the larger biomass samples overlapped in expression changes, and the relative expression levels of selected genes were confirmed with quantitative real-time polymerase chain reaction, suggesting that these methods can be used for plant experiments where the biomass is extremely limited (i.e. spaceflight studies).

Chemistry Testing on Plasma Versus Serum Samples in Dialysis Patients: Clinical and Quality Improvement Implications.

PubMed

Carey, Roger Neill; Jani, Chinu; Johnson, Curtis; Pearce, Jim; Hui-Ng, Patricia; Lacson, Eduardo

2016-09-07

Plasma samples collected in tubes containing separator gels have replaced serum samples for most chemistry tests in many hospital and commercial laboratories. Use of plasma samples for blood tests in the dialysis population eliminates delays in sample processing while waiting for clotting to complete, laboratory technical issues associated with fibrin formation, repeat sample collection, and patient care issues caused by delay of results because of incompletely clotted specimens. Additionally, a larger volume of plasma is produced than serum for the same amount of blood collected. Plasma samples are also acceptable for most chemical tests involved in the care of patients with ESRD. This information becomes very important when United States regulatory requirements for ESRD inadvertently limit the type of sample that can be used for government reporting, quality assessment, and value-based payment initiatives. In this narrative, we summarize the renal community experience and how the subsequent resolution of the acceptability of phosphorus levels measured from serum and plasma samples may have significant implications in the country's continued development of a value-based Medicare ESRD Quality Incentive Program. Copyright © 2016 by the American Society of Nephrology.

Shell-vial culture, coupled with real-time PCR, applied to Rickettsia conorii and Rickettsia massiliae-Bar29 detection, improving the diagnosis of the Mediterranean spotted fever.

PubMed

Segura, Ferran; Pons, Immaculada; Sanfeliu, Isabel; Nogueras, María-Mercedes

2016-04-01

Rickettsia conorii and Rickettsia massiliae-Bar29 are related to Mediterranean spotted fever (MSF). They are intracellular microorganisms. The Shell-vial culture assay (SV) improved Rickettsia culture but it still has some limitations: blood usually contains low amount of microorganisms and the samples that contain the highest amount of them are non-sterile. The objectives of this study were to optimize SV culture conditions and monitoring methods and to establish antibiotic concentrations useful for non-sterile samples. 12 SVs were inoculated with each microorganism, incubated at different temperatures and monitored by classical methods and real-time PCR. R. conorii was detected by all methods at all temperatures since 7th day of incubation. R. massiliae-Bar29 was firstly observed at 28°C. Real-time PCR allowed to detected it 2-7 days earlier (depend on temperature) than classical methods. Antibiotics concentration needed for the isolation of these Rickettsia species from non-sterile samples was determined inoculating SV with R. conorii, R. massiliae-Bar29, biopsy or tick, incubating them with different dilutions of antibiotics and monitoring them weekly. To sum up, if a MSF diagnosis is suspected, SV should be incubated at both 28°C and 32°C for 1-3 weeks and monitored by a sensitive real-time PCR. If the sample is non-sterile the panel of antibiotics tested can be added. Copyright © 2016 Elsevier GmbH. All rights reserved.

Gene expression from plants grown on the International Space Station

NASA Astrophysics Data System (ADS)

Stimpson, Alexander; Pereira, Rhea; Kiss, John Z.; Correll, Melanie

Three experiments were performed on the International Space Station (ISS) in 2006 as part of the TROPI experiments. These experiments were performed to study graviTROPIsm and photoTROPIsm responses of Arabidopsis in microgravity (µg). Seedlings were grown with a variety of light and gravitational treatments for approximately five days. The frozen samples were returned to Earth during three space shuttle missions in 2007 and stored at -80° C. Due to the limited amount of plant biomass returned, new protocols were developed to minimize the amount of material needed for RNA extraction as a preparation for microarray analysis. Using these new protocols, RNA was extracted from several sets of seedlings grown in red light followed by blue light with one sample from 1.0g treatment and the other at µg. Using a 2-fold change criterion, microarray (Affymetrix, GeneChip) results showed that 613 genes were upregulated in the µg sample while 757 genes were downregulated. Upregulated genes in response to µg included transcription factors from the WRKY (15 genes), MYB (3) and ZF (8) families as well as those that are involved in auxin responses (10). Downregulated genes also included transcription factors such as MYB (5) and Zinc finger (10) but interestingly only two WRKY family genes were down-regulated during the µg treatment. Studies are underway to compare these results with other samples to identify the genes involved in the gravity and light signal transduction pathways (this project is Supported By: NASA NCC2-1200).

Ultratrace determination of arsenic in water samples by electrothermal atomic absorption spectrometry after pre-concentration with Mg-Al-Fe ternary layered double hydroxide nano-sorbent.

PubMed

Abdolmohammad-Zadeh, Hossein; Jouyban, Abolghasem; Amini, Roghayeh

2013-11-15

A selective solid phase extraction method, based on nano-structured Mg-Al-Fe(NO3(-)) ternary layered double hydroxide as a sorbent, is developed for the pre-concentration of ultra-trace levels of arsenic (As) prior to determination by electrothermal atomic absorption spectrometry. It is found that both As(III) and As(V) could be quantitatively retained on the sorbent within a wide pH range of 4-12. Accordingly, the presented method is applied to determination of total inorganic As in aqueous solutions. Maximum analytical signal of As is achieved when the pyrolysis and atomization temperatures are close to 900 °C and 2300 °C, respectively. Several variables affecting the extraction efficiency including pH, sample flow rate, amount of nano-sorbent, elution conditions and sample volume are optimized. Under the optimized conditions, the limit of detection (3Sb/m) and the relative standard deviation are 4.6 pg mL(-1) and 3.9%, respectively. The calibration graph is linear in the range of 15.0-650 pg mL(-1) with a correlation coefficient of 0.9979, sorption capacity and pre-concentration factor are 8.68 mg g(-1) and 300, respectively. The developed method is validated by the analysis of a standard reference material (SRM 1643e) and is successfully applied to the determination of ultra-trace amounts of As in different water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Trace analysis of energetic materials via direct analyte-probed nanoextraction coupled to direct analysis in real time mass spectrometry.

PubMed

Clemons, Kristina; Dake, Jeffrey; Sisco, Edward; Verbeck, Guido F

2013-09-10

Direct analysis in real time mass spectrometry (DART-MS) has proven to be a useful forensic tool for the trace analysis of energetic materials. While other techniques for detecting trace amounts of explosives involve extraction, derivatization, solvent exchange, or sample clean-up, DART-MS requires none of these. Typical DART-MS analyses directly from a solid sample or from a swab have been quite successful; however, these methods may not always be an optimal sampling technique in a forensic setting. For example, if the sample were only located in an area which included a latent fingerprint of interest, direct DART-MS analysis or the use of a swab would almost certainly destroy the print. To avoid ruining such potentially invaluable evidence, another method has been developed which will leave the fingerprint virtually untouched. Direct analyte-probed nanoextraction coupled to nanospray ionization-mass spectrometry (DAPNe-NSI-MS) has demonstrated excellent sensitivity and repeatability in forensic analyses of trace amounts of illicit drugs from various types of surfaces. This technique employs a nanomanipulator in conjunction with bright-field microscopy to extract single particles from a surface of interest and has provided a limit of detection of 300 attograms for caffeine. Combining DAPNe with DART-MS provides another level of flexibility in forensic analysis, and has proven to be a sufficient detection method for trinitrotoluene (TNT), RDX, and 1-methylaminoanthraquinone (MAAQ). Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

Estimating dermal transfer from PCB-contaminated porous surfaces.

PubMed

Slayton, T M; Valberg, P A; Wait, A D

1998-06-01

Health risks posed by dermal contact with PCB-contaminated porous surfaces have not been directly demonstrated and are difficult to estimate indirectly. Surface contamination by organic compounds is commonly assessed by collecting wipe samples with hexane as the solvent. However, for porous surfaces, hexane wipe characterization is of limited direct use when estimating potential human exposure. Particularly for porous surfaces, the relationship between the amount of organic material collected by hexane and the amount actually picked up by, for example, a person's hand touch is unknown. To better mimic PCB pickup by casual hand contact with contaminated concrete surfaces, we used alternate solvents and wipe application methods that more closely mimic casual dermal contact. Our sampling results were compared to PCB pickup using hexane-wetted wipes and the standard rubbing protocol. Dry and oil-wetted samples, applied without rubbing, picked up less than 1% of the PCBs picked up by the standard hexane procedure; with rubbing, they picked up about 2%. Without rubbing, saline-wetted wipes picked up 2.5%; with rubbing, they picked up about 12%. While the nature of dermal contact with a contaminated surface cannot be perfectly reproduced with a wipe sample, our results with alternate wiping solvents and rubbing methods more closely mimic hand contact than the standard hexane wipe protocol. The relative pickup estimates presented in this paper can be used in conjunction with site-specific PCB hexane wipe results to estimate dermal pickup rates at sites with PCB-contaminated concrete.

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

PubMed

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

2016-09-23

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

Characteristics and composition of watermelon, pumpkin, and paprika seed oils and flours.

PubMed

El-Adawy, T A; Taha, K M

2001-03-01

The nutritional quality and functional properties of paprika seed flour and seed kernel flours of pumpkin and watermelon were studied, as were the characteristics and structure of their seed oils. Paprika seed and seed kernels of pumpkin and watermelon were rich in oil and protein. All flour samples contained considerable amounts of P, K, Mg, Mn, and Ca. Paprika seed flour was superior to watermelon and pumpkin seed kernel flours in content of lysine and total essential amino acids. Oil samples had high amounts of unsaturated fatty acids with linoleic and oleic acids as the major acids. All oil samples fractionated into seven classes including triglycerides as a major lipid class. Data obtained for the oils' characteristics compare well with those of other edible oils. Antinutritional compounds such as stachyose, raffinose, verbascose, trypsin inhibitor, phytic acid, and tannins were detected in all flours. Pumpkin seed kernel flour had higher values of chemical score, essential amino acid index, and in vitro protein digestibility than the other flours examined. The first limiting amino acid was lysine for both watermelon and pumpkin seed kernel flours, but it was leucine in paprika seed flour. Protein solubility index, water and fat absorption capacities, emulsification properties, and foam stability were excellent in watermelon and pumpkin seed kernel flours and fairly good in paprika seed flour. Flour samples could be potentially added to food systems such as bakery products and ground meat formulations not only as a nutrient supplement but also as a functional agent in these formulations.

The facile flow-injection spectrophotometric detection of gold(III) in water and pharmaceutical samples using 3,5-dimethoxy-4-hydroxy-2-aminoacetophenone isonicotinoyl hydrazone (3,5-DMHAAINH).

PubMed

Babu, S Hari; Suvardhan, K; Kumar, K Suresh; Reddy, K M; Rekha, D; Chiranjeevi, P

2005-04-11

A simple, sensitive and rapid flow-injection spectrophotometric method was developed for the determination of trace amounts of Au(III) in aqueous dimethylformamide (DMF). The method is based on formation of Au(III)-(3,5-DMHAAINH)3 complex. The optimum conditions for the chromogenic reaction of Au(III) with 3,5-DMHAAINH is studied and the colored (reddish brown) complex is selectively monitored at lambda(max) 490 nm at pH 6.0. The reaction and flow conditions of the full experimental design were optimized. The detection limit (2 s) of 0.1 microg l-1 Au(III) was obtained at a sampling rate of 15 samples h-1. Beer's law is obeyed over the range of 0.30-4.00 microg ml-1. The molar absorptivity and Sandell's sensitivity were 3.450x10(4) M and 0.0050 microg ml-1, respectively. Job's method of continuous variation and stability constants corresponding to these maxima was determined and found to be 9.3x10(15) (1:3, M:R) (M, metal; R, reagent). The detailed study of various interferences confirmed the high selectivity of the developed method. The method was successfully applied for the determination of trace amount of Au(III) in water and pharmaceutical samples. The results obtained were in agreement with the reported methods at the 95% confidence level.

A Dramatic Classroom Demonstration of Limiting Reagent Using the Vinegar and Sodium Hydrogen Carbonate Reaction

ERIC Educational Resources Information Center

Artdej, Romklao; Thongpanchang, Tienthong

2008-01-01

This demonstration is designed to illustrate the concept of limiting reagent in a spectacular way. Via a series of experiments where the amount of vinegar is fixed and the amount of NaHCO[subscript 3] is gradually increased, the volume of CO[subscript 2] generated from the reaction varies corresponding to the amount of NaHCO[subscript 3] until it…

Evaluation of metal ion release from Ti6Al4V and Co-Cr-Mo casting alloys: in vivo and in vitro study.

PubMed

El Sawy, Amal A; Shaarawy, Mohammed A

2014-02-01

The aim of this study was to evaluate the amount of ions released from Ti6Al4V and Co-Cr-Mo alloys both in vivo and in vitro. Twenty-one discs of each alloy were constructed and divided into seven groups. Three specimens from each group were immersed in a buffered saline solution over a period of 1, 3, 5, 7, 14, 21, and 28 days. Twenty-eight participants were also included in the study, where the study group consisted of 14 mandibular partially edentulous patients, and the control group consisted of 14 volunteers. The study group was further divided into two equal groups: the first group received removable partial dentures (RPDs) constructed from Co-Cr-Mo alloy, while the second group received RPDs constructed from Ti6Al4V alloy. Saliva samples were collected from each participant over the same study period. The conditioning media and saliva samples were analyzed using a spectrophotometer. One-way ANOVA and Tukey tests were used for statistical analysis (p < 0.05). The concentrations of metal ions released from the studied alloys were significantly higher in the in vitro than in the in vivo study group during the follow-up periods. A statistically significant increase in ion concentrations of the different elements for both alloys was found with time (p < 0.05). The amounts of released metallic ions from Co-Cr-Mo and Ti6Al4V alloys were higher in the buffered saline solutions than in the studied saliva samples and control groups; however, these amounts were still within the physiological limit of trace elements in the human body. © 2013 by the American College of Prosthodontists.

A new supramolecular based liquid solid microextraction method for preconcentration and determination of trace bismuth in human blood serum and hair samples by electrothermal atomic absorption spectrometry.

PubMed

Kahe, Hadi; Chamsaz, Mahmoud

2016-11-01

A simple and reliable supramolecule-aggregated liquid solid microextraction method is described for preconcentration and determination of trace amounts of bismuth in water as well as human blood serum and hair samples. Catanionic microstructures of cetyltrimethylammonium bromide (CTAB) and sodium dodecyl sulfate (SDS) surfactants, dissolved in deionized water/propanol, are used as a green solvent to extract bismuth (III)-diethyldithiocarbamate complexes by dispersive microextraction methodology. The extracted solid phase is easily removed and dissolved in 50 μL propanol for subsequent measurement by electrothermal atomic absorption spectrometry (ET-AAS). The procedure benefits the merits of supramolecule aggregates' properties and dispersive microextraction technique using water as the main component of disperser solvent, leading to direct interaction with analyte. Phase separation behavior of extraction solvent and different parameters influencing the extraction efficiency of bismuth ion such as salt concentration, pH, centrifugation time, amount of chelating agent, SDS:CTAB mole ratio, and solvent amounts were thoroughly optimized. Under the optimal experimental conditions, the calibration curve was linear in the range of 0.3-6 μg L -1 Bi (III) with a limit of detection (LOD) of 0.16 μg L -1 (S/N = 3). The relative standard deviations (RSD) of determination were obtained to be 5.1 and 6.2 % for 1 and 3 μg L -1 of Bi (III), respectively. The developed method was successfully applied as a sensitive and accurate technique for determination of bismuth ion in human blood serum, hair samples, and a certified reference material.

Flame atomic absorption spectrometric determination of trace amounts of nickel after extraction and preconcentration onto natural modified analcime zeolite loaded with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol.

PubMed

Afzali, Darush; Taher, Mohammad Ali; Mostafavi, Ali; Mahani, Mohammad Khayatzadeh

2005-01-01

Nickel is a moderately toxic element compared with other transition metals. However, inhalation of nickel and its compounds leads to serious problems, including cancer of the respiratory system and a skin disorder, nickel-eczema. Thus, attention has focused on the toxicity of nickel at low concentrations, and the development of reliable, analytical approaches for the determination of trace amounts of nickel is needed. This paper describes a simple, rapid, and sensitive flame atomic absorption spectrometric method for the determination of trace amounts of nickel in various samples after adsorption of its 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex on a modified Analcime column in the pH range of 7.5-10.5. The retained analyte on the Analcime is recovered with 5.0 mL 2 M nitric acid and determined by flame atomic absorption spectrometry. The detection limit is 20 ng/mL, and the calibration curve is linear for analyte concentrations in the range of 0.1-8 microg/mL final solution, with a correlation coefficient of 0.9993. Eight replicate determinations of nickel at 2 microg/mL in the final solution gave an absorbance of 0.1222, with a relative standard deviation (RSD) of +/-1.2%. The interference of a large number of anions and cations was studied, and the proposed method was used for the determination of nickel in various standard reference samples. The accuracy of the proposed method was evaluated by analyzing standard reference samples, and the results were satisfactory (recoveries of >96%; RSD of <3.5%).

Limits to preference and the sensitivity of choice to rate and amount of food.

PubMed

Aparicio, Carlos F; Baum, William M; Hughes, Christine E; Pitts, Raymond C

2016-03-01

Studies of choice holding food-amount ratio constant while varying food-rate ratio within sessions showed that local changes in preference depend on relative amount of food. The present study investigated whether sensitivity of choice to food-rate ratio and sensitivity to food-amount ratio are independent of one another when food-rate ratios are varied across sessions and food-amount ratios are varied within sessions. Food deliveries for rats' presses on the left and right levers were scheduled according to three different food-rate ratios of 1:1, 9:1, and 1:9; each food-rate ratio lasted for 106 sessions and was arranged independently of seven food-amount ratios (7:1, 6:2, 5:3, 4:4, 3:5, 2:6, and 1:7 food pellets) occurring within sessions in random sequence. Each amount ratio lasted for 10 food deliveries and was separated from another by a 60-s blackout. Sensitivity to rate ratio was high (1.0) across food deliveries. Sensitivity to amount ratio was low when food rates were equal across alternatives, but was high when rate ratio and amount ratio opposed one another. When rate ratio and amount ratio went in the same direction, choice ratio reached an elevenfold limit which reduced sensitivity to approximately zero. We conclude that three factors affect sensitivity to amount: (1) the limit to preference, (2) the equal effect on preference of amounts greater than four pellets, and (3) the absence of differential effects of switches in amount in the equal-rates (1:1) condition. Taken together, these findings indicate that rate and amount only sometimes combine independently as additive variables to determine preference when amount ratios vary frequently within sessions. © 2016 Society for the Experimental Analysis of Behavior.

The U.S. Geological Survey coal quality (COALQUAL) database version 3.0

USGS Publications Warehouse

Palmer, Curtis A.; Oman, Charles L.; Park, Andy J.; Luppens, James A.

2015-12-21

Because of database size limits during the development of COALQUAL Version 1.3, many analyses of individual bench samples were merged into whole coal bed averages. The methodology for making these composite intervals was not consistent. Size limits also restricted the amount of georeferencing information and forced removal of qualifier notations such as "less than detection limit" (<) information, which can cause problems when using the data. A review of the original data sheets revealed that COALQUAL Version 2.0 was missing information that was needed for a complete understanding of a coal section. Another important database issue to resolve was the USGS "remnant moisture" problem. Prior to 1998, tests for remnant moisture (as-determined moisture in the sample at the time of analysis) were not performed on any USGS major, minor, or trace element coal analyses. Without the remnant moisture, it is impossible to convert the analyses to a usable basis (as-received, dry, etc.). Based on remnant moisture analyses of hundreds of samples of different ranks (and known residual moisture) reported after 1998, it was possible to develop a method to provide reasonable estimates of remnant moisture for older data to make it more useful in COALQUAL Version 3.0. In addition, COALQUAL Version 3.0 is improved by (1) adding qualifiers, including statistical programming to deal with the qualifiers; (2) clarifying the sample compositing problems; and (3) adding associated samples. Version 3.0 of COALQUAL also represents the first attempt to incorporate data verification by mathematically crosschecking certain analytical parameters. Finally, a new database system was designed and implemented to replace the outdated DOS program used in earlier versions of the database.

The evaluation of total mercury and arsenic in skin bleaching creams commonly used in Trinidad and Tobago and their potential risk to the people of the Caribbean.

PubMed

Mohammed, Terry; Mohammed, Elisabeth; Bascombe, Shermel

2017-12-13

Background. Skin lightening is very popular among women and some men of the Caribbean, and its popularity appears to be growing. The lightening of skin colour is done to produce a lighter complexion which is believed to increase attractiveness, social standing and improves one's potential of being successful. Design and Methods. Fifteen (15) common skin lightening creams found in pharmacies and cosmetic retailers throughout Trinidad and Tobago were evaluated for Mercury by Cold Vapor Atomic Absorption Spectrophotometry (CVAAS) and Arsenic by Hydride Generation Atomic Absorption Spectrophotometry (HGAAS). The results obtained were compared to global standards and previous research. Results. Fourteen (14) of the fifteen samples analysed contained Mercury in the range of 0.473 μg/g to 0.766 μg/g. One sample had a Mercury content of 14,507.74±490.75 μg/g which was over 14,000 times higher than the USFDA limit for mercury in cosmetics of 1 μg/g. All samples contained Arsenic in the range 1.016 μg/g to 6.612 μg/g, which exceeds the EU limit for cosmetics of 0 μg/g. Conclusions. All the samples analysed contained significant amounts of Mercury and Arsenic and none of them can be considered safe for prolonged human use. The samples that contained Mercury levels which were lower than the USFDA limit contained Arsenic levels which exceeded the EU standard of 0 μg/g in cosmetics. The popularity of these skin lightening creams in the Caribbean region places the population at elevated risk of chronic Mercury and Arsenic poisoning and possibly acute Mercury Poisoning.

Exposure to 4,4'-methylenediphenyl diisocyanate (MDI) during moulding of rigid polyurethane foam: determination of airborne MDI and urinary 4,4'-methylenedianiline (MDA).

PubMed

Kääriä, K; Hirvonen, A; Norppa, H; Piirilä, P; Vainio, H; Rosenberg, C

2001-04-01

Occupational exposure to 4,4'-methylenediphenyl diisocyanate (MDI) was measured during moulding of rigid polyurethane foam. The aim of the study was to find out whether an MDI-derived urinary amine metabolite could be detected in the urine of workers exposed to apparently low levels of MDI. Airborne MDI was sampled on 1-(2-methoxyphenyl)-piperazine (2MP)-impregnated glass fibre filters and determined by high-performance liquid chromatography (HPLC) using ultraviolet (UV) and electrochemical (EC) detection. The limit of detection of MDI was 3 ng ml-1 for a 20 microliters injection. The precision of sample preparation, expressed as relative standard deviation (RSD), was 1.3% with UV detection and 2.1% with EC detection at a concentration of 70 ng MDI ml-1 (n = 6). The 2MP-MDI derivative was stable at +4 degrees C up to eight weeks. The accuracy of the method was validated in an international quality control programme. Workers (n = 57) from three different factories participated in the study. Urinary 4,4'-methylenedianiline (MDA) metabolite was determined after acid hydrolysis as heptafluorobutyric anhydride derivatives by gas chromatography-mass spectrometry using chemical ionisation and monitoring negative ions. The limit of detection in urine was 0.2 nmol l-1. The precision of six analyses for a urine sample spiked to a concentration of 1 nmol l-1 was 29% (RSD). The MDI concentrations were below the limit of detection in most (64%) of the air samples collected in the worker's breathing zone. Still, detectable amounts of MDA were found in 97% of the urine samples. Monitoring of urinary MDA appears to be an appropriate method of assessing MDI exposure in work environments with low or undetectable MDI concentrations in the workplace air.

Does Plant Biomass Manipulation in Static Chambers Affect Nitrous Oxide Emissions from Soils?

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

Collier, Sarah M.; Dean, Andrew P.; Oates, Lawrence G.

One of the most widespread approaches for measurement of greenhouse gas emissions from soils involves the use of static chambers. This method is relatively inexpensive, is easily replicated, and is ideally suited to plot-based experimental systems. Among its limitations is the loss of detection sensitivity with increasing chamber height, which creates challenges for deployment in systems including tall vegetation. It is not always possible to avoid inclusion of plants within chambers or to extend chamber height to fully accommodate plant growth. Thus, in many systems, such as perennial forages and biomass crops, plants growing within static chambers must either bemore » trimmed or folded during lid closure. Currently, data on how different types of biomass manipulation affect measured results is limited. For this study, we compare the effects of cutting vs. folding of biomass on nitrous oxide measurements in switchgrass (Panicum virgatum L.) and alfalfa (Medicago sativa L.) systems. We report only limited evidence of treatment effects during discrete sampling events and little basis for concern that effects may intensify over time as biomass manipulation is repeatedly imposed. However, nonsignificant treatment effects that were consistently present amounted to significant overall trends in three out of the four systems studied. Such minor disparities in flux could amount to considerable quantities over time, suggesting that caution should be exercised when comparing cumulative emission values from studies using different biomass manipulation strategies.« less

Does Plant Biomass Manipulation in Static Chambers Affect Nitrous Oxide Emissions from Soils?

DOE PAGES

Collier, Sarah M.; Dean, Andrew P.; Oates, Lawrence G.; ...

2016-01-22

One of the most widespread approaches for measurement of greenhouse gas emissions from soils involves the use of static chambers. This method is relatively inexpensive, is easily replicated, and is ideally suited to plot-based experimental systems. Among its limitations is the loss of detection sensitivity with increasing chamber height, which creates challenges for deployment in systems including tall vegetation. It is not always possible to avoid inclusion of plants within chambers or to extend chamber height to fully accommodate plant growth. Thus, in many systems, such as perennial forages and biomass crops, plants growing within static chambers must either bemore » trimmed or folded during lid closure. Currently, data on how different types of biomass manipulation affect measured results is limited. For this study, we compare the effects of cutting vs. folding of biomass on nitrous oxide measurements in switchgrass (Panicum virgatum L.) and alfalfa (Medicago sativa L.) systems. We report only limited evidence of treatment effects during discrete sampling events and little basis for concern that effects may intensify over time as biomass manipulation is repeatedly imposed. However, nonsignificant treatment effects that were consistently present amounted to significant overall trends in three out of the four systems studied. Such minor disparities in flux could amount to considerable quantities over time, suggesting that caution should be exercised when comparing cumulative emission values from studies using different biomass manipulation strategies.« less

Micro-scale NMR Screening of New Detergents for Membrane Protein Structural Biology

PubMed Central

Zhang, Qinghai; Horst, Reto; Geralt, Michael; Ma, Xingquan; Hong, Wen-Xu; Finn, M. G.; Stevens, Raymond C.; Wüthrich, Kurt

2008-01-01

The rate limiting step in biophysical characterization of membrane proteins is often the availability of suitable amounts of protein material. It was therefore of interest to demonstrate that micro-coil nuclear magnetic resonance (NMR) technology can be used to screen microscale quantities of membrane proteins for proper folding in samples destined for structural studies. Micoscale NMR was then used to screen a series of newly designed zwitterionic phosphocholine detergents for their ability to reconstitute membrane proteins, using the previously well characterized β-barrel E.coli outer membrane protein OmpX as a test case. Fold screening was thus achieved with μg-amounts of uniformly 2H,15N-labeld OmpX and affordable amounts of the detergents, and prescreening with SDS-gel electrophoresis ensured efficient selection of the targets for NMR studies. A systematic approach to optimize the phosphocholine motif for membrane protein refolding led to the identification of two new detergents, 138-Fos and 179-Fos, that yield 2D [15N,1H]-TROSY correlation NMR spectra of natively folded reconstituted OmpX. PMID:18479092

Determination of sudan dyes in red wine and fruit juice using ionic liquid-based liquid-liquid microextraction and high-performance liquid chromatography.

PubMed

Sun, Shuo; Wang, Ying; Yu, Wenzhi; Zhao, Tianqi; Gao, Shiqian; Kang, Mingqin; Zhang, Yupu; Zhang, Hanqi; Yu, Yong

2011-07-01

The liquid-liquid microextraction (LLME) was developed for extracting sudan dyes from red wine and fruit juice. Room temperature ionic liquid was used as the extraction solvent. The target analytes were determined by high-performance liquid chromatography. The extraction parameters were optimized. The optimal conditions are as follows: volume of [C(6)MIM][PF(6)] 50 μL; the extraction time 10 min; pH value of the sample solution 7.0; NaCl concentration in sample solution 5%. The extraction recoveries for the analytes in red wine and fruit samples are 86.79-108.28 and 68.54-85.66%, whereas RSDs are 1.42-5.12 and 1.43-6.19%, respectively. The limits of detection and quantification were 0.428 and 1.426 ng/mL for sudan I, 0.938 and 3.127 ng/mL for sudan II, 1.334 and 4.445 ng/mL for sudan III, 1.454 and 4.846 ng/mL for sudan IV, respectively. Compared with conventional liquid-liquid extraction (CLLE) and ultrasonic extraction (UE), when LLME was applied, the sample amount was less (LLME: 4 mL; CLLE: 10 mL; UE: 10 mL), the extraction time was shorter (LLME: 15 min; CLLE: 110 min; UE: 50 min) and the extraction solvent amount was less (LLME: 0.05 mL IL; CLLE: 15 mL hexane; UE: 20 mL hexane). The proposed method offers a simple, rapid and efficient sample preparation for determining sudan dyes in red wine and fruit juice samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

NanoDrop Microvolume Quantitation of Nucleic Acids

PubMed Central

Desjardins, Philippe; Conklin, Deborah

2010-01-01

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

Microarray-based comparison of three amplification methods for nanogram amounts of total RNA

PubMed Central

Singh, Ruchira; Maganti, Rajanikanth J.; Jabba, Sairam V.; Wang, Martin; Deng, Glenn; Heath, Joe Don; Kurn, Nurith; Wangemann, Philine

2007-01-01

Gene expression profiling using microarrays requires microgram amounts of RNA, which limits its direct application for the study of nanogram RNA samples obtained using microdissection, laser capture microscopy, or needle biopsy. A novel system based on Ribo-SPIA technology (RS, Ovation-Biotin amplification and labeling system) was recently introduced. The utility of the RS system, an optimized prototype system for picogram RNA samples (pRS), and two T7-based systems involving one or two rounds of amplification (OneRA, Standard Protocol, or TwoRA, Small Sample Prototcol, version II) were evaluated in the present study. Mouse kidney (MK) and mouse universal reference (MUR) RNA samples, 0.3 ng to 10 μg, were analyzed using high-density Affymetrix Mouse Genome 430 2.0 GeneChip arrays. Call concordance between replicates, correlations of signal intensity, signal intensity ratios, and minimal fold increase necessary for significance were determined. All systems amplified partially overlapping sets of genes with similar signal intensity correlations. pRS amplified the highest number of genes from 10-ng RNA samples. We detected 24 of 26 genes verified by RT-PCR in samples prepared using pRS. TwoRA yielded somewhat higher call concordances than did RS and pRS (91.8% vs. 89.3% and 88.1%, respectively). Although all target preparation methods were suitable, pRS amplified the highest number of targets and was found to be suitable for amplification of as little as 0.3 ng of total RNA. In addition, RS and pRS were faster and simpler to use than the T7-based methods and resulted in the generation of cDNA, which is more stable than cRNA. PMID:15613496

Testing the effectiveness of an international conservation agreement: marketplace forensics and CITES caviar trade regulation.

PubMed

Doukakis, Phaedra; Pikitch, Ellen K; Rothschild, Anna; DeSalle, Rob; Amato, George; Kolokotronis, Sergios-Orestis

2012-01-01

The international wildlife trade is a key threat to biodiversity. Temporal genetic marketplace monitoring can determine if wildlife trade regulation efforts such as the Convention on International Trade in Endangered Species (CITES) are succeeding. Protected under CITES effective 1997, sturgeons and paddlefishes, the producers of black caviar, are flagship CITES species. We test whether CITES has limited the amount of fraudulent black caviar reaching the marketplace. Using mitochondrial DNA-based methods, we compare mislabeling in caviar and meat purchased in the New York City area pre and post CITES listing. Our recent sampling of this market reveals a decrease in mislabeled caviar (2006-2008; 10%; n = 90) compared to pre-CITES implementation (1995-1996; 19%; n = 95). Mislabeled caviar was found only in online purchase (n = 49 online/41 retail). Stricter controls on importing and exporting as per CITES policies may be having a positive conservation effect by limiting the amount of fraudulent caviar reaching the marketplace. Sturgeons and paddlefishes remain a conservation priority, however, due to continued overfishing and habitat degradation. Other marine and aquatic species stand to benefit from the international trade regulation that can result from CITES listing.

Analytical study of endocrine-disrupting chemicals in leachate treatment process of municipal solid waste (MSW) landfill sites.

PubMed

Asakura, Hiroshi; Matsuto, Toshihiko; Tanaka, Nobutoshi

2007-01-01

Influent and processed water were sampled at different points in the leachate treatment facilities of five municipal solid waste (MSW) landfill sites. Then, the concentrations of endocrine-disrupting chemicals (EDCs), namely, alkylphenols (APs), bisphenol A (BPA), phthalic acid esters (PAEs) and organotin compounds (OTs), in the treated leachate samples were determined and the behavior of the EDCs in the treatment processes was discussed. The concentrations of APs were as low as those in surface waters, and no OTs were detected (detection limit: 0.01 microg/L). Meanwhile, diethylhexyl phthalate (DEHP), which was the most abundant of the four substances measured as PAEs, and BPA were found in all of the influent samples. BPA was considerably degraded by aeration, except when the water temperature was low and the total organic carbon (TOC) was high. By contrast, aeration, biological treatment, and coagulation/sedimentation removed only a small amount of DEHP.

A new catalytic-spectrophotometric method for quantification of trace amounts of nitrite in fruit juice samples.

PubMed

Sobhanardakani, S; Farmany, A; Abbasi, S; Cheraghi, J; Hushmandfar, R

2013-03-01

A new kinetic method has been developed for the determination of nitrite in fruit juice samples. The method is based on the catalytic effect of nitrite with the oxidation of Nile Blue A (NBA) by KBrO(3) in the sulfuric acid medium. The optimum conditions obtained are 1.2 mM sulfuric acid, 0.034 mM of NBA, 2.8 × 10(-3) M KBrO(3), reaction temperature of 20 °C, and reaction time of 100 s at 595.5 nm. Under the optimized conditions, the method allowed the quantification of nitrite in a range of 0.2-800 μg/mL with a detection limit of 0.02 μg/mL. The method was applied to the determination of nitrite in 15 brands of fruit juice samples.

Efficacy of water-dispersible formulations of biological control strains of Aspergillus flavus for aflatoxin management in corn.

PubMed

Weaver, Mark A; Abbas, Hamed K; Jin, Xixuan; Elliott, Brad

2016-01-01

Field experiments were conducted in 2011 and 2012 to evaluate the efficacy of water-dispersible granule (WDG) formulations of biocontrol strains of Aspergillus flavus in controlling aflatoxin contamination of corn. In 2011, when aflatoxin was present at very high levels, there was no WDG treatment that could provide significant protection against aflatoxin contamination. The following year a new WDG formulation was tested that resulted in 100% reduction in aflatoxin in one field experiment and ≥ 49% reduction in all five WDG treatments with biocontrol strain 21882. Large sampling error, however, limited the resolution of various treatment effects. Corn samples were also subjected to microbial analysis to understand better the mechanisms of successful biocontrol. In the samples examined here, the size of the A. flavus population on the grain was associated with the amount of aflatoxin, but the toxigenic status of that population was a poor predictor of aflatoxin concentration.

Weighing the Facts: A Systematic Review of Expected Patterns of Weight Loss in Full-Term, Breastfed Infants.

PubMed

Thulier, Diane

2016-02-01

All breastfeeding infants lose some weight in the early days of life. Conventionally, 5% to 7% loss of birth weight has been accepted as the normal and expected amount of weight loss before infants begin to gain weight steadily. When infants lose more than 7% of their birth weight, breastfeeding adequacy is sometimes questioned and formula supplementation is often given. Despite the fact that 5% to 7% is well known and commonly cited, little reliable evidence exists that supports use of this figure as a guide to practice. A systematic review of studies that focused on infant weight loss was conducted. The main objective was to determine the mean amount of weight loss for healthy, full-term exclusively breastfed infants after birth. One previous review and 9 primary studies published since 2008 were examined. The reported mean infant weight loss ranged widely among studies from 3.79% to 8.6%. The point at which most infants have lost the most amount of weight occurs 2 to 4 days after birth. Close examination of the studies, however, revealed significant methodological flaws in the research. Study limitations commonly included gaps in data collection, lack of documented feeding type, sample groups that lacked adequate numbers of exclusively breastfed infants, and the exclusion of breastfed infants who lost the most weight. Well-designed clinical studies that address these limitations are needed. © The Author(s) 2015.

Applicability of direct total reflection X-ray fluorescence analysis for selenium determination in solutions related to environmental and geochemical studies

NASA Astrophysics Data System (ADS)

Marguí, E.; Floor, G. H.; Hidalgo, M.; Kregsamer, P.; Roman-Ross, G.; Streli, C.; Queralt, I.

2010-12-01

A significant amount of environmental studies related to selenium determination in different environmental compartments have been published in the last years due to the narrow range between the Se nutritious requirement as essential element and toxic effects upon exposure. However, the direct analysis of complex liquid samples like natural waters and extraction solutions presents significant problems related to the low Se concentrations and the complicated matrix of this type of samples. The goal of the present research was to study the applicability of direct TXRF analysis of different type of solutions commonly used in environmental and geochemical studies, confirm the absence or presence of matrix effects and evaluate the limits of detection and accuracy for Se determination in the different matrices. Good analytical results were obtained for the direct analysis of ground and rain water samples with limits of detection for Se two orders of magnitude lower than the permissible Se concentration in drinking waters ([Se] = 10 μg/L) according to the WHO. However, the Se detection limits for more complex liquid samples such as thermal waters and extraction solutions were in the μg/L range due to the presence of high contents of other elements present in the matrix (i.e., Br, Fe, Zn) or the high background of the TXRF spectrum that hamper the Se determination at trace levels. Our results give insight into the possibilities and drawbacks of direct TXRF analysis and to a certain extent the potential applications in the environmental and geochemical field.

Potential of sawdust as a green and economical sorbent for simultaneous preconcentration of trace amounts of cadmium, cobalt, and lead from water, biological, food, and herbal samples.

PubMed

Baki, Mostafa Hossein; Shemirani, Farzaneh; Khani, Rouhollah

2013-05-01

Application of treated sawdust with NaOH as a green and economical sorbent for simultaneous preconcentration of trace amounts of Cd(II), Co(II), and Pb(II) ions from liver, lettuce, fish, and water as test samples with complicated matrices was investigated. Various parameters, such as effect of pH and contact time, breakthrough volume, type, and concentration of eluent and interference of ions were studied. The sorption was quantitative in the pH of 5.0 to 7.0 and desorption occurred instantaneously with 5.0 mL of mixed solutions of ethanol and 2.0 mol/L HNO3 -HCl and the amount of ions was measured by using flame atomic absorption spectrometry. Linearity was maintained at 3 to 500 μg/L for cobalt, 5.0 to 800 μg/L for lead, and 2.0 to 300 μg/L for cadmium in the original solution. The relative standard deviation was less than 1.80% (n = 6, with concentration of 0.3 mg/L for cadmium and 0.5 mg/L for lead and cobalt). Detection limits and maximum capacity of the sorbent for Co (II), Cd (II), and Pb (II) in the original solution were 0.86, 0.50, and 1.7 μg/L and 28.5, 30.6, and 47.3 mg/g, respectively. The results for spiked real samples, effect of interfering ions, and adsorption capacity indicated that the applicability of this method for lead preconcentration is better than cadmium and cobalt preconcentration from complicated matrices. Practical Application: Sawdust can be applied as a green and economical sorbent for simultaneous preconcentration and solid-phase extraction of metal ions from food and environmental samples with complicated matrices. © 2013 Institute of Food Technologists®

Tunable Coarse Graining for Monte Carlo Simulations of Proteins via Smoothed Energy Tables: Direct and Exchange Simulations

PubMed Central

2015-01-01

Many commonly used coarse-grained models for proteins are based on simplified interaction sites and consequently may suffer from significant limitations, such as the inability to properly model protein secondary structure without the addition of restraints. Recent work on a benzene fluid (LettieriS.; ZuckermanD. M.J. Comput. Chem.2012, 33, 268−27522120971) suggested an alternative strategy of tabulating and smoothing fully atomistic orientation-dependent interactions among rigid molecules or fragments. Here we report our initial efforts to apply this approach to the polar and covalent interactions intrinsic to polypeptides. We divide proteins into nearly rigid fragments, construct distance and orientation-dependent tables of the atomistic interaction energies between those fragments, and apply potential energy smoothing techniques to those tables. The amount of smoothing can be adjusted to give coarse-grained models that range from the underlying atomistic force field all the way to a bead-like coarse-grained model. For a moderate amount of smoothing, the method is able to preserve about 70–90% of the α-helical structure while providing a factor of 3–10 improvement in sampling per unit computation time (depending on how sampling is measured). For a greater amount of smoothing, multiple folding–unfolding transitions of the peptide were observed, along with a factor of 10–100 improvement in sampling per unit computation time, although the time spent in the unfolded state was increased compared with less smoothed simulations. For a β hairpin, secondary structure is also preserved, albeit for a narrower range of the smoothing parameter and, consequently, for a more modest improvement in sampling. We have also applied the new method in a “resolution exchange” setting, in which each replica runs a Monte Carlo simulation with a different degree of smoothing. We obtain exchange rates that compare favorably to our previous efforts at resolution exchange (LymanE.; ZuckermanD. M.J. Chem. Theory Comput.2006, 2, 656−666). PMID:25400525

Ultrasensitive quantification of endogenous brassinosteroids in milligram fresh plant with a quaternary ammonium derivatization reagent by pipette-tip solid-phase extraction coupled with ultra-high-performance liquid chromatography tandem mass spectrometry.

PubMed

Deng, Ting; Wu, Dapeng; Duan, Chunfeng; Guan, Yafeng

2016-07-22

Determination of endogenous brassinosteroids (BRs) in limited sample amount is vital to elucidating their tissue- and even local tissue-specific signaling pathway and physiological effects on plant growth and development. In this work, an ultra-sensitive quantification method was established for endogenous BRs in milligram fresh plant by using pipette-tip solid-phase extraction coupled with ultra-performance liquid chromatography tandem mass spectrometry (PT-SPE-UPLC-MS/MS), in which a quaternary ammonium phenyl boronic acid, 4-borono-N,N,N-trimethylbenzenaminium iodide (BTBA) was first developed for chemical derivatization of BRs. Due to the cationic quaternary ammonium group of BTBA, the ionization efficiencies of the BRs chelates with BTBA (BTBA-BRs) were enhanced by 1190-448785 times, which is the highest response enhancement factor among all derivatization reagents reported for BRs. In addition, PT-SPE packed with C18 sorbent was first used for purifying BRs from plant extracts, so the required sample amount was minimized, and recoveries higher than 91% were achieved. Under the optimized conditions, the minimal detectable amounts (MDA) of five target BRs were in the range of 27-94 amol, and the correlation coefficients (R(2)) were >0.9985 over four orders of magnitude. The relative recoveries of 75.8-104.9% were obtained with the intra- and inter-day relative standard deviations (RSDs) less than 18.7% and 19.6%, respectively. Finally, three BRs were successfully quantified in only 5mg fresh rice plant samples, and 24-epiBL can even be detected in only 0.5mg FW rice leaf segments. It is the first time that the BRs content in sub-milligram fresh plant sample has been quantified. Copyright © 2016 Elsevier B.V. All rights reserved.

Rapid Method of Determining Factors Limiting Bacterial Growth in Soil

PubMed Central

Aldén, L.; Demoling, F.; Bååth, E.

2001-01-01

A technique to determine which nutrients limit bacterial growth in soil was developed. The method was based on measuring the thymidine incorporation rate of bacteria after the addition of C, N, and P in different combinations to soil samples. First, the thymidine incorporation method was tested in two different soils: an agricultural soil and a forest humus soil. Carbon (as glucose) was found to be the limiting substance for bacterial growth in both of these soils. The effect of adding different amounts of nutrients was studied, and tests were performed to determine whether the additions affected the soil pH and subsequent bacterial activity. The incubation time required to detect bacterial growth after adding substrate to the soil was also evaluated. Second, the method was used in experiments in which three different size fractions of straw (1 to 2, 0.25 to 1, and <0.25 mm) were mixed into the agricultural soil in order to induce N limitation for bacterial growth. When the straw fraction was small enough (<0.25 mm), N became the limiting nutrient for bacterial growth after about 3 weeks. After the addition of the larger straw fractions (1 to 2 and 0.25 to 1 mm), the soil bacteria were C limited throughout the incubation period (10 weeks), although an increase in the thymidine incorporation rate after the addition of C and N together compared with adding them separately was seen in the sample containing the size fraction from 0.25 to 1 mm. Third, soils from high-pH, limestone-rich areas were examined. P limitation was observed in one of these soils, while tendencies toward P limitation were seen in some of the other soils. PMID:11282640

Applicability of the ParaDNA(®) Screening System to Seminal Samples.

PubMed

Tribble, Nicholas D; Miller, Jamie A D; Dawnay, Nick; Duxbury, Nicola J

2015-05-01

Seminal fluid represents a common biological material recovered from sexual assault crime scenes. Such samples can be prescreened using different techniques to determine cell type and relative amount before submitting for full STR profiling. The ParaDNA(®) Screening System is a novel forensic test which identifies the presence of DNA through amplification and detection of two common STR loci (D16S539 and TH01) and the Amelogenin marker. The detection of the Y allele in samples could provide a useful tool in the triage and submission of sexual assault samples by enforcement authorities. Male template material was detected on a range of common sexual assault evidence items including cotton pillow cases, condoms, swab heads and glass surfaces and shows a detection limit of 1 in 1000 dilution of neat semen. These data indicate this technology has the potential to be a useful tool for the detection of male donor DNA in sexual assault casework. © 2015 American Academy of Forensic Sciences.

Chicxulub Impact Melts: Geochemical Signatures of Target Lithology Mixing and Post-Impact Hydrothermal Fluid Processes

NASA Technical Reports Server (NTRS)

Kring, David A.; Zurcher, Lukas; Horz, Freidrich; Mertzmann, Stanley A.

2004-01-01

Impact melts within complex impact craters are generally homogeneous, unless they differentiated, contain immiscible melt components, or were hydrothermally altered while cooling. The details of these processes, however, and their chemical consequences, are poorly understood. The best opportunity to unravel them may lie with the Chicxulub impact structure, because it is the world s most pristine (albeit buried) large impact crater. The Chicxulub Scientific Drilling Project recovered approx. 100 meters of impactites in a continuous core from the Yaxcopoil-1 (YAX-1) borehole. This dramatically increased the amount of melt available for analyses, which was previously limited to two small samples N17 and N19) recovered from the Yucatan-6 (Y-6) borehole and one sample (N10) recovered from the Chicxulub-1 (C-1) borehole. In this study, we describe the chemical compositions of six melt samples over an approx. 40 m section of the core and compare them to previous melt samples from the Y-6 and C-1 boreholes.

Nanophase Carbonates on Mars: Formation, Detection, and Implications

NASA Technical Reports Server (NTRS)

Archer, P. D.; Lauer, H. V.; Ming, D. W.; Niles, P. B.; Morris, R. V.; Rampe, E. B.; Sutter, B.

2014-01-01

Despite having an atmosphere composed primarily of CO2 and evidence for abundant water in the past, carbonate minerals have only been discovered on Mars in small amounts in martian dust, in soils in the Northern Plains, and in outcrops of limited spatial extent. Recently, carbonates have been identified as the possible source of CO2 released during thermal analysis of material from an aeolian deposit named Rocknest and drilled sample from the sheepbed mudstone, both samples analyzed by the Mars Science Laboratory (MSL) in Gale Crater. Both the Phoenix lander and MSL carry thermal analysis instruments, the Thermal and Evolved Gas Analyzer (TEGA) on Phoenix and the Sample Analysis at Mars (SAM) instrument on MSL. While thermal analysis does not provide definitive mineralogy, it can detect volatile-bearing minerals present at very low abundance and the temperature profiles of evolved gases can reveal physical properties of the sample. For example, the decomposition temperature of volatilebearing minerals depends heavily on the particle size of the mineral.

[Occurrence of 3-monochloropropane-1,2-diol (3-MCPD) in food products].

PubMed

Gawarska, Halina; Sawilska-Rautenstrauch, Dorota; Starski, Andrzej; Karłowski, Kazimierz

2009-01-01

3-Monochloropropane-1,2-diol (3-MCPD) is a contaminant belongs to a group of chemicals called chloropropanols. 3-MCPD can be formed in foods as result of processing or storage condition. At the beginning 3-MCPD was identified as a contaminant of the acid-hydrolysed vegetable protein, which is produced using hydrochloric acid and high temperature. Studies have shown that 3-MCPD is carcinogenic for rats, however genotoxic adverse effect was not observed in vivo. The purpose of this studies was determination of 3-MCPD amounts in retail food products and comparison with the EC legislative limit. 99 samples of foodstuffs was tested: soya sauce, hydrolysed vegetable protein (HVP), sugar, instant soups, stock cubes, bakery products, chips and edible fats. 3-MCPD was detected at levels below 10 microg/kg in 15% of the tested samples, and above 10 microg/kg in 63%. 3-MCPD was not occurred in 22% of the tested samples. The samples were analysed by gas chromatography-mass spectrometry (GC/MS).

Petrographic and petrological studies of lunar rocks. [Apollo 15 breccias and Russian tektites

NASA Technical Reports Server (NTRS)

Winzer, S. R.

1978-01-01

Clasts, rind glass, matrix glass, and matrix minerals from five Apollo 15 glass-coated breccias (15255, 15286, 15465, 15466, and 15505) were studied optically and with the SEM/microprobe. Rind glass compositions differ from sample to sample, but are identical, or nearly so, to the local soil, suggesting their origin by fusion of that soil. Most breccia samples contain green or colorless glass spheres identical to the Apollo 15 green glasses. These glasses, along with other glass shards and fragments, indicate a large soil component is present in the breccias. Clast populations include basalts and gabbros containing phases highly enriched in iron, indicative of extreme differentiation or fractional crystallization. Impact melts, anorthosites, and minor amounts of ANT suite material are also present among the clasts. Tektite glasses, impact melts, and breccias from the Zhamanshin structure, USSR, were also studied. Basic tektite glasses were found to be identical in composition to impact melts from the structure, but no satisfactory parent material has been identified in the limited suite of samples available.

Vortex-Assisted Dispersive Micro-Solid Phase Extraction Using CTAB-Modified Zeolite NaY Sorbent Coupled with HPLC for the Determination of Carbamate Insecticides.

PubMed

Salisaeng, Pawina; Arnnok, Prapha; Patdhanagul, Nopbhasinthu; Burakham, Rodjana

2016-03-16

A vortex-assisted dispersive micro-solid phase extraction (VA-D-μ-SPE) based on cetyltrimethylammonium bromide (CTAB)-modified zeolite NaY was developed for preconcentration of carbamate pesticides in fruits, vegetables, and natural surface water prior to analysis by high performance liquid chromatography with photodiode array detection. The small amounts of solid sorbent were dispersed in a sample solution, and extraction occurred by adsorption in a short time, which was accelerated by vortex agitation. Finally, the sorbents were filtered from the solution, and the analytes were subsequently desorbed using an appropriate solvent. Parameters affecting the VA-D-μ-SPE performance including sorbent amount, sample volume, desorption solvent ,and vortex time were optimized. Under the optimum condition, linear dynamic ranges were achieved between 0.004-24.000 mg kg(-1) (R(2) > 0.9946). The limits of detection (LODs) ranged from 0.004-4.000 mg kg(-1). The applicability of the developed procedure was successfully evaluated by the determination of the carbamate residues in fruits (dragon fruit, rambutan, and watermelon), vegetables (cabbage, cauliflower, and cucumber), and natural surface water.

Determination of urinary aromatic amines in smokers and nonsmokers using a MIPs-SPE coupled with LC-MS/MS method.

PubMed

Yu, Jingjing; Wang, Sheng; Zhao, Ge; Wang, Bing; Ding, Li; Zhang, Xiaobing; Xie, Jianping; Xie, Fuwei

2014-05-01

Urinary aromatic amines (AAs) could be used as biomarkers for human exposure to AAs in cigarette smoke. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of urinary AAs (i.e. 1-naphthylamine (1-NA), 2-naphthylamine (2-NA), 3-aminobiphenyl (3-ABP) and 4-aminobiphenyl (4-ABP)) in smokers and nonsmokers. A molecularly imprinted polymers (MIPs) solid phase extraction (SPE) cartridge was applied to purify urine samples and no derivatization reaction was involved. Each analytes used respective stable isotope internal standards, which could well compensate matrix effect. Lower limit of detections (LODs) for four AAs were obtained and in the range of 1.5-5ngL(-1). Recovery ranged from 87.7±4.5% to 111.3±6.4% and precision were less than 9.9%. The method was applied to analyze urine samples of 40 smokers and 10 nonsmokers. The 24h urinary excretion amounts of total AAs were higher for smokers compared with nonsmokers. What's more, 1-NA, 3-ABP and 4-ABP excretion amounts showed significant differences (p<0.05) between smokers and nonsmokers. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of molybenum in soils and rocks: A geochemical semimicro field method

USGS Publications Warehouse

Ward, F.N.

1951-01-01

Reconnaissance work in geochemical prospecting requires a simple, rapid, and moderately accurate method for the determination of small amounts of molybdenum in soils and rocks. The useful range of the suggested procedure is from 1 to 32 p.p.m. of molybdenum, but the upper limit can be extended. Duplicate determinations on eight soil samples containing less than 10 p.p.m. of molybdenum agree within 1 p.p.m., and a comparison of field results with those obtained by a conventional laboratory procedure shows that the method is sufficiently accurate for use in geochemical prospecting. The time required for analysis and the quantities of reagents needed have been decreased to provide essentially a "test tube" method for the determination of molybdenum in soils and rocks. With a minimum amount of skill, one analyst can make 30 molybdenum determinations in an 8-hour day.

Higher certainty of the laser-induced damage threshold test with a redistributing data treatment

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

Jensen, Lars; Mrohs, Marius; Gyamfi, Mark

2015-10-15

As a consequence of its statistical nature, the measurement of the laser-induced damage threshold holds always risks to over- or underestimate the real threshold value. As one of the established measurement procedures, the results of S-on-1 (and 1-on-1) tests outlined in the corresponding ISO standard 21 254 depend on the amount of data points and their distribution over the fluence scale. With the limited space on a test sample as well as the requirements on test site separation and beam sizes, the amount of data from one test is restricted. This paper reports on a way to treat damage testmore » data in order to reduce the statistical error and therefore measurement uncertainty. Three simple assumptions allow for the assignment of one data point to multiple data bins and therefore virtually increase the available data base.« less

A rapid and practical strategy for the determination of platinum, palladium, ruthenium, rhodium, iridium and gold in large amounts of ultrabasic rock by inductively coupled plasma optical emission spectrometry combined with ultrasound extraction

NASA Astrophysics Data System (ADS)

Zhang, Gai; Tian, Min

2015-04-01

This proposed method regulated the determination of platinum, palladium, ruthenium, rhodium, iridium and gold in platinum-group ores by nickel sulfide fire assay—inductively coupled plasma optical emission spectrometry (ICP-OES) combined with ultrasound extraction for the first time. The quantitative limits were 0.013-0.023μg/g. The samples were fused to separate the platinum-group elements from matrix. The nickel sulfide button was then dissolved with hydrochloric acid and the insoluble platinum-group sulfide residue was dissolved with aqua regia by ultrasound bath and finally determined by ICP-OES. The proposed method has been applied into the determination of platinum-group element and gold in large amounts of ultrabasic rocks from the Great Dyke of Zimbabwe.

Airborne isocyanate exposures in the collision repair industry and a comparison to occupational exposure limits.

PubMed

Reeb-Whitaker, Carolyn; Whittaker, Stephen G; Ceballos, Diana M; Weiland, Elisa C; Flack, Sheila L; Fent, Kenneth W; Thomasen, Jennifer M; Trelles Gaines, Linda G; Nylander-French, Leena A

2012-01-01

Isocyanate exposure was evaluated in 33 spray painters from 25 Washington State autobody shops. Personal breathing zone samples (n = 228) were analyzed for isophorone diisocyanate (IPDI) monomer, 1,6-hexamethylene diisocyanate (HDI) monomer, IPDI polyisocyanate, and three polyisocyanate forms of HDI. The objective was to describe exposures to isocyanates while spray painting, compare them with short-term exposure limits (STELs), and describe the isocyanate composition in the samples. The composition of polyisocyanates (IPDI and HDI) in the samples varied greatly, with maximum amounts ranging from up to 58% for HDI biuret to 96% for HDI isocyanurate. There was a significant inverse relationship between the percentage composition of HDI isocyanurate to IPDI and to HDI uretdione. Two 15-min STELs were compared: (1) Oregon's Occupational Safety and Health Administration (OR-OSHA) STEL of 1000 μg/m(3) for HDI polyisocyanate, and (2) the United Kingdom's Health and Safety Executive (UK-HSE) STEL of 70 μg NCO/m(3) for all isocyanates. Eighty percent of samples containing HDI polyisocyanate exceeded the OR-OSHA STEL while 98% of samples exceeded the UK-HSE STEL. The majority of painters (67%) wore half-face air-purifying respirators while spray painting. Using the OR-OSHA and the UK-HSE STELs as benchmarks, 21% and 67% of painters, respectively, had at least one exposure that exceeded the respirator's OSHA-assigned protection factor. A critical review of the STELs revealed the following limitations: (1) the OR-OSHA STEL does not include all polyisocyanates, and (2) the UK-HSE STEL is derived from monomeric isocyanates, whereas the species present in typical spray coatings are polyisocyanates. In conclusion, the variable mixtures of isocyanates used by autobody painters suggest that an occupational exposure limit is required that includes all polyisocyanates. Despite the limitations of the STELs, we determined that a respirator with an assigned protection factor of 25 or greater is required to protect against isocyanate exposures during spray painting. Consequently, half-face air-purifying respirators, which are most commonly used and have an assigned protection factor of 10, do not afford adequate respiratory protection.

Airborne Isocyanate Exposures in the Collision Repair Industry and a Comparison to Occupational Exposure Limits

PubMed Central

Reeb-Whitaker, Carolyn; Whittaker, Stephen G.; Ceballos, Diana M.; Weiland, Elisa C.; Flack, Sheila L.; Fent, Kenneth W.; Thomasen, Jennifer M.; Gaines, Linda G. Trelles; Nylander-French, Leena A.

2014-01-01

Isocyanate exposure was evaluated in 33 spray painters from 25 Washington State autobody shops. Personal breathing zone samples (n = 228) were analyzed for isophorone diisocyanate (IPDI) monomer, 1,6-hexamethylene diisocyanate (HDI) monomer, IPDI polyisocyanate, and three polyisocyanate forms of HDI. The objective was to describe exposures to isocyanates while spray painting, compare them with short-term exposure limits (STELs), and describe the isocyanate composition in the samples. The composition of polyisocyanates (IPDI and HDI) in the samples varied greatly, with maximum amounts ranging from up to 58% for HDI biuret to 96% for HDI isocyanurate. There was a significant inverse relationship between the percentage composition of HDI isocyanurate to IPDI and to HDI uretdione. Two 15-min STELs were compared: (1) Oregon's Occupational Safety and Health Administration (OR-OSHA) STEL of 1000 μg/m3 for HDI polyisocyanate, and (2) the United Kingdom's Health and Safety Executive (UK-HSE) STEL of 70 μg NCO/m3 for all isocyanates. Eighty percent of samples containing HDI polyisocyanate exceeded the OR-OSHA STEL while 98% of samples exceeded the UKHSE STEL. The majority of painters (67%) wore half-face air-purifying respirators while spray painting. Using the OROSHA and the UK-HSE STELs as benchmarks, 21% and 67% of painters, respectively, had at least one exposure that exceeded the respirator's OSHA-assigned protection factor. A critical review of the STELs revealed the following limitations: (1) the OR-OSHA STEL does not include all polyisocyanates, and (2) the UK-HSE STEL is derived from monomeric isocyanates, whereas the species present in typical spray coatings are polyisocyanates. In conclusion, the variable mixtures of isocyanates used by autobody painters suggest that an occupational exposure limit is required that includes all polyisocyanates. Despite the limitations of the STELs, we determined that a respirator with an assigned protection factor of 25 or greater is required to protect against isocyanate exposures during spray painting. Consequently, half-face air-purifying respirators, which are most commonly used and have an assigned protection factor of 10, do not afford adequate respiratory protection. PMID:22500941

RBS and PIXE analysis of chlorine contamination in ALD-Grown TiN films on silicon

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

Meersschaut, J.; Witters, T.; Kaeyhkoe, M.

2013-04-19

The performance, strengths and limitations of RBS and PIXE for the characterization of trace amounts of Cl in TiN thin films are critically compared. The chlorine atomic concentration in ALD grown TiN thin films on Si is determined for samples grown at temperatures ranging from 350 Degree-Sign C to 550 Degree-Sign C. We show that routine Rutherford backscattering spectrometry measurements (1.5 MeV He{sup +}) and PIXE measurements (1.5 MeV H{sup +}) on 20 nm thick TiN films allow one to determine the Cl content down to 0.3 at% with an absolute statistical accuracy reaching 0.03 at%. Possible improvements to pushmore » the sensitivity limit for both approaches are proposed.« less

Study on methenamine detection in starch products through SERS technology

NASA Astrophysics Data System (ADS)

Cui, Yu; Qu, Zhou

2016-01-01

Using silver sol as a strengthened base, this paper concludes that l0ppb-0.1ppb methenamine aqueous solution has a better signal in 1052cm-1 Raman feature. And the lower limit of the aqueous solution is about 0.1ppb. Adding corresponding amount methenamine in vermicelli sample, the lower limit is about 10ppm. This is a safest and pollution-free detection process. Furthermore, the pretreatment process is simple, which will be finished in 20 minutes. Hence, it is better than other detection methods. SERS technology provides a simple, rapid and efficient detection method for field measurement and real time detection modulating disk of component, laser zooming system. Through the use of laser diode, Laser-beam riding guided system is likely to have smaller shape and very light.

Impregnated multiwalled carbon nanotubes as efficient sorbent for the solid phase extraction of trace amounts of heavy metal ions in food and water samples.

PubMed

Gouda, Ayman A; Al Ghannam, Sheikha M

2016-07-01

A new, sensitive and simple solid phase extraction (SPE), separation and preconcentration method of some heavy metal ions, Cd(II), Cu(II), Ni(II), Pb(II) and Zn(II) at trace levels using multiwalled carbon nanotubes (MWCNTs) impregnated with 2-(2-benzothiazolylazo)orcinol (BTAO) from food and water samples were investigated. The effect of analytical parameters was examined. The metals retained on the nanotubes at pH 7.0 were eluted by 5.0mL HNO3 (2.0molL(-1)). The influence of matrix ions on the proposed method was evaluated. The preconcentration factor was calculated and found to be 100. The detection limits (LODs) for Cd(II), Cu(II), Ni(II), Pb(II) and Zn(II) were found at 0.70, 1.2, 0.80, 2.6 and 2.2μgL(-1), respectively. The relative standard deviation (RSD) and the recoveries of the standard addition method were lower than 5.0% and 95-102%, respectively. The new procedure was successfully applied to the determination of trace amounts of the studied metal ions in various food and water samples and validated using certified reference materials SRM 1570A (spinach leaves) with satisfactory and compatible results. Copyright © 2016 Elsevier Ltd. All rights reserved.

Gold nanoparticle-based simple colorimetric and ultrasensitive dynamic light scattering assay for the selective detection of Pb(II) from paints, plastics, and water samples.

PubMed

Beqa, Lule; Singh, Anant Kumar; Khan, Sadia Afrin; Senapati, Dulal; Arumugam, Sri Ranjini; Ray, Paresh Chandra

2011-03-01

Pb (II) is a common water pollutant with high toxicity. According to the CDC, about 310,000 U.S. children of ages 1-5 have high levels of lead in their blood that it is due to the exposure to lead from plastic toys and other products. As a result, the development of ultrasensitive assays for the real-time detection of Pb(II) from plastic toys and paints is very important for water controlling, clinical toxicology and industrial processes. Driven by the need to detect trace amounts of Pb(II) from water samples, we report a label-free, highly selective and ultra sensitive glutathione modified gold nanoparticle based dynamic light scattering (DLS) probe for Pb(II) recognition in 100 ppt level from aqueous solution with excellent discrimination against other heavy metals. The sensitivity of our assay to detect Pb(II) level in water is almost 2 orders of magnitude higher than the EPA standard limit. We have also demonstrated that our DLS assay is capable of measuring the amount of Pb(II) in paint, plastic toys, and water from MS river. A possible mechanism and operating principles of our DLS assay have been discussed. Ultimately, this nanotechnology driven assay could have enormous potential applications in rapid, on-site monitoring of Pb(II) from day-to-day sample.

Sensitive determination of three aconitum alkaloids and their metabolites in human plasma by matrix solid-phase dispersion with vortex-assisted dispersive liquid-liquid microextraction and HPLC with diode array detection.

PubMed

Wang, Xiaozhong; Li, Xuwen; Li, Lanjie; Li, Min; Liu, Ying; Wu, Qian; Li, Peng; Jin, Yongri

2016-05-01

A simple and sensitive method for determination of three aconitum alkaloids and their metabolites in human plasma was developed using matrix solid-phase dispersion combined with vortex-assisted dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection. The plasma sample was directly purified by matrix solid-phase dispersion and the eluate obtained was concentrated and further clarified by vortex-assisted dispersive liquid-liquid microextraction. Some important parameters affecting the extraction efficiency, such as type and amount of dispersing sorbent, type and volume of elution solvent, type and volume of extraction solvent, salt concentration as well as sample solution pH, were investigated in detail. Under optimal conditions, the proposed method has good repeatability and reproducibility with intraday and interday relative standard deviations lower than 5.44 and 5.75%, respectively. The recoveries of the aconitum alkaloids ranged from 73.81 to 101.82%, and the detection limits were achieved within the range of 1.6-2.1 ng/mL. The proposed method offered the advantages of good applicability, sensitivity, simplicity, and feasibility, which makes it suitable for the determination of trace amounts of aconitum alkaloids in human plasma samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Modification of CMV DNA detection from dried blood spots for diagnosing congenital CMV infection.

PubMed

Binda, Sandro; Caroppo, Simona; Didò, Patrizia; Primache, Valeria; Veronesi, Licia; Calvario, Agata; Piana, Andrea; Barbi, Maria

2004-07-01

Detection of viral DNA in dried blood spots using the Guthrie card (DBS test) is a reliable and practical method of diagnosing congenital cytomegalovirus (CMV) infection. The test lends itself to epidemiological studies to establish the prevalence of the infection, but also to neonatal screening for secondary prevention of sequelae. These applications would be facilitated if it were possible to use smaller samples and do the test on pools of individual cases. To ascertain whether doing the test on smaller, pooled samples still accurately identifies neonates with congenital CMV infection. We tested DBS from: (A) 39 laboratory reference cases; (B) 156 neonates suspected of having congenital CMV infection; (C) 119 children examined for the retrospective diagnosis of congenital CMV; (D) mock specimens prepared with known amounts of viral DNA. The test using only one third of the usual amount of dried blood was 100% sensitive and specific compared to the standard DBS test (A) and to viral isolation (A and B). Pools of three single cases gave the same results as viral isolation (B) and the small-sample test (B and C). All the versions of the test gave a detection limit of 400 copies/ml. The modified procedure can accurately diagnose congenital CMV infection. It achieves savings in both the patient material and the costs of testing.

Constraining Type Ia Supernova Progenitor Scenarios with Extremely Late-time Photometry of Supernova SN 2013aa

NASA Astrophysics Data System (ADS)

Jacobson-Galán, Wynn V.; Dimitriadis, Georgios; Foley, Ryan J.; Kilpatrick, Charles D.

2018-04-01

We present Hubble Space Telescope observations and photometric measurements of the Type Ia supernova (SN Ia) SN 2013aa 1500 days after explosion. At this epoch, the luminosity is primarily dictated by the amounts of radioactive {}57{{Co}} and {}55{{Fe}}, while at earlier epochs, the luminosity depends on the amount of radioactive {}56{{Co}}. The ratio of odd-numbered to even-numbered isotopes depends significantly on the density of the progenitor white dwarf (WD) during the SN explosion, which, in turn, depends on the details of the progenitor system at the time of ignition. From a comprehensive analysis of the entire light curve of SN 2013aa, we measure a M({}57{{Co}})/M({}56{{Co}}) ratio of {0.02}-0.02+0.01, which indicates a relatively low central density for the progenitor WD at the time of explosion, consistent with DD progenitor channels. We estimate M({}56{{Ni}}) = 0.732 +/- 0.151 {M}ȯ , and place an upper limit on the abundance of {}55{{Fe}}. A recent study reported a possible correlation between M({}57{{Co}})/M({}56{{Co}}) and stretch for four SNe Ia. SN 2013aa, however, does not fit this trend, indicating either SN 2013aa is an extreme outlier or the correlation does not hold up with a larger sample. The M({}57{{Co}})/M({}56{{Co}}) measured for the expanded sample of SNe Ia with photometry at extremely late times has a much larger range than that of explosion models, perhaps limiting conclusions about SN Ia progenitors drawn from extremely late-time photometry.

Methylxanthine Content in Commonly Consumed Foods in Spain and Determination of Its Intake during Consumption

PubMed Central

2017-01-01

Methylxanthines present psychostimulant effects. These compounds have low toxicity and their consumption at moderate levels presents some beneficial health effects, whereas some significant risk appears at high levels. Samples of common types of methylxanthine-containing beverages and foods consumed in Spain were analyzed to determine their content. Caffeine was the methylxanthine that was most found in the samples investigated. Instant coffees gave the highest caffeine percentage (18–44 mg·g−1). Green and scented teas were found to have a caffeine dry-weight content (8–26 mg·g−1) equivalent to ground coffees (13–23 mg·g−1), but black and pu-erh teas (18–30 mg·g−1) had a higher caffeine content. The evaluation of the most conventional methods for preparing espresso coffees showed that an espresso contains between 88–116 mg of caffeine. In the case of tea beverages, the amount of caffeine present was 2–3 times smaller than in espresso coffees. Energy drinks showed a similar caffeine content (80–106 mg) as espresso coffees. Chocolates had the lowest caffeine content. It has been found that none of the foods evaluated reach the recommended daily intake limit of 400 mg of caffeine with a single dose. This limit can be reached with 4–5 doses in the case of coffees and energy drinks. In the case of chocolates, the methylxanthine compound detected at large levels was theobromine, with amounts ranging from 4 to 10 mg·g−1 for dark chocolates. PMID:29207513

Soil pH on mobility of imazaquin in oxisols with positive balance of charges.

PubMed

Regitano, Jussara B; da Rocha, Wadson S D; Alleoni, Luís R F

2005-05-18

The influence of soil pH on the leaching potential of the ionizable herbicide imazaquin was assessed on the profile of two highly weathered soils having a net positive charge in the B horizon, in contrast to a soil having a net negative charge in the whole profile, using packed soil column experiments. Imazaquin leached to a large extent and faster at Kd values lower than 1.0 L kg(-1), a much more lenient limit than usually proposed for pesticides in the literature (Kd < 5.0 L kg(-1)). The amount of imazaquin leached increased with soil pH. As the soil pH increased, the percentage of imazaquin in the anionic forms, the negative surface potential of the soils, as well as imazaquin water solubility also increased, thus reducing sorption because of repulsive electrostatic forces (hydrophilic interactions). For all surface samples (0-0.2 m), imazaquin did not leach at soil pH values lower than pKa (3.8) and more than 80% of the applied amount was leached at pH values higher than 5.5. For subsurface samples from the acric soils, imazaquin only began to leach at soil pH values > zero point of salt effects (ZPSE > 5.7). In conclusion, the use of surface K(oc) values to predict the amount of imazaquin leached within soil profiles having a positive balance of charges may greatly overestimate its actual leaching potential.

A fluorescent-based HPLC assay for quantification of cysteine and cysteamine adducts in Escherichia coli-derived proteins.

PubMed

Soriano, Brian D; Tam, Lei-Ting T; Lu, Hsieng S; Valladares, Violeta G

2012-01-01

Recombinant proteins expressed in Escherichia coli are often produced as unfolded, inactive forms accumulated in inclusion bodies. Redox-coupled thiols are typically employed in the refolding process in order to catalyze the formation of correct disulfide bonds at maximal folding efficiency. These thiols and the recombinant proteins can form mixed disulfide bonds to generate thiol-protein adducts. In this work, we apply a fluorescent-based assay for the quantification of cysteine and cysteamine adducts as observed in E. coli-derived proteins. The thiols are released by reduction of the adducted protein, collected and labeled with a fluorescent reagent, 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate. The derivatized thiols are separated by reversed-phase HPLC and can be accurately quantified after method optimization. The estimated thiol content represents total amount of adducted forms present in the analyzed samples. The limit of quantification (LOQ) was established; specifically, the lowest amount of quantifiable cysteine adduction is 30 picograms and the lowest amount of quantifiable cysteamine adduction is 60 picograms. The assay is useful for quantification of adducts in final purified products as well as in-process samples from various purification steps. The assay indicates that the purification process accomplishes a decrease in cysteine adduction from 0.19 nmol adduct/nmol protein to 0.03 nmol adduct/nmol protein as well as a decrease in cysteamine adduction from 0.24 nmol adduct/nmol protein to 0.14 nmol adduct/nmol protein. Copyright © 2011. Published by Elsevier B.V.

Comparison between splines and fractional polynomials for multivariable model building with continuous covariates: a simulation study with continuous response.

PubMed

Binder, Harald; Sauerbrei, Willi; Royston, Patrick

2013-06-15

In observational studies, many continuous or categorical covariates may be related to an outcome. Various spline-based procedures or the multivariable fractional polynomial (MFP) procedure can be used to identify important variables and functional forms for continuous covariates. This is the main aim of an explanatory model, as opposed to a model only for prediction. The type of analysis often guides the complexity of the final model. Spline-based procedures and MFP have tuning parameters for choosing the required complexity. To compare model selection approaches, we perform a simulation study in the linear regression context based on a data structure intended to reflect realistic biomedical data. We vary the sample size, variance explained and complexity parameters for model selection. We consider 15 variables. A sample size of 200 (1000) and R(2)  = 0.2 (0.8) is the scenario with the smallest (largest) amount of information. For assessing performance, we consider prediction error, correct and incorrect inclusion of covariates, qualitative measures for judging selected functional forms and further novel criteria. From limited information, a suitable explanatory model cannot be obtained. Prediction performance from all types of models is similar. With a medium amount of information, MFP performs better than splines on several criteria. MFP better recovers simpler functions, whereas splines better recover more complex functions. For a large amount of information and no local structure, MFP and the spline procedures often select similar explanatory models. Copyright © 2012 John Wiley & Sons, Ltd.

Cooking methods and the formation of PhIP (2-Amino, 1-methyl, 6-phenylimidazo[4,5-b] pyridine) in the crust of the habitually consumed meat in Argentina.

PubMed

Reartes, Gabriela Angelina; Di Paola Naranjo, Romina Daniela; Eynard, Aldo Renato; Muñoz, Sonia Edith

2016-06-01

Content of carcinogenic molecules like, 2-Amino, 1-methyl, 6-phenylimidazo[4,5-b] pyridine in meals is one of the main mutagenic substances formed during meat cooking, and it can be used as a dietary exposure marker. Our objective was to estimate the amount of PhIP consumed from habitual Argentinean diet, rich in red meats, comparing different cooking procedures and meat type. Samples (n = 240) of lean and fatty beef, chicken, pork, and fish were cooked using different methods: griddle, grill, sauté pan, and oven. Samples were: Overcooked, or cooked with a microbiologically suitable or "healthy technique" (HT). The PhIP was determined by HPLC-MS. Meats cooked using HT formed little crust amounts and PhIP was below the detection levels. In overcooked meats, large amounts of crust were formed in lean meats, fatty beef, fatty chicken and baked pork. PhIP was measured in lean meats sauted or cooked on a griddle, a method reaching temperatures until 250 °C.It was estimated that Argentine people eats about 12,268.0 ng/day of PhIP being these values above those tolerated limits for total dietary heterocyclic amines in some developed countries. Hence, cooking small meat portions, at medium temperature, avoiding prolonged cooking and preferring baked lean meats could be recommended as a healthier habit. Copyright © 2016. Published by Elsevier Ltd.

Chemical-mineralogical characterization of C&D waste recycled aggregates from São Paulo, Brazil.

PubMed

Angulo, S C; Ulsen, C; John, V M; Kahn, H; Cincotto, M A

2009-02-01

This study presents a methodology for the characterization of construction and demolition (C&D) waste recycled aggregates based on a combination of analytical techniques (X-ray fluorescence (XRF), soluble ions, semi-quantitative X-ray diffraction (XRD), thermogravimetric analysis (TGA-DTG) and hydrochloric acid (HCl) selective dissolution). These combined analytical techniques allow for the estimation of the amount of cement paste, its most important hydrated and carbonated phases, as well as the amount of clay and micas. Details of the methodology are presented here and the results of three representative C&D samples taken from the São Paulo region in Brazil are discussed. Chemical compositions of mixed C&D aggregate samples have mostly been influenced by particle size rather than the visual classification of C&D into red or grey and geographical origin. The amount of measured soluble salts in C&D aggregates (0.15-25.4mm) is lower than the usual limits for mortar and concrete production. The content of porous cement paste in the C&D aggregates is around 19.3% (w/w). However, this content is significantly lower than the 43% detected for the C&D powders (<0.15 mm). The clay content of the powders was also high, potentially resulting from soil intermixed with the C&D waste, as well as poorly burnt red ceramic. Since only about 50% of the measured CaO is combined with CO(2), the powders have potential use as raw materials for the cement industry.

Nearly half of the adolescents in an Italian school-based study exceeded the recommended upper limits for daily caffeine consumption.

PubMed

Santangelo, Barbara; Lapolla, Rosa; Rutigliano, Irene; Pettoello Mantovani, Massimo; Campanozzi, Angelo

2018-06-01

No data are available on caffeine consumption among Italian adolescents. We investigated caffeine intake from coffee, soft drinks and energy drinks in a sample of Italian adolescents and determined if they exceeded the recommended limits. The study comprised 1213 adolescents with a mean age of 15.1 years (range 12-19) from four schools in Foggia, southern Italy. Caffeine intake was assessed using an anonymous self-reported questionnaire during the 2013/2014 school year. We calculated the percentage of daily caffeine consumers, their mean intake of caffeine from beverages and the contribution of each beverage category to the total caffeine intake. Approximately 76% of the sample consumed caffeine every day, amounting to 125.5 ± 69.2 mg/day and 2.1 ± 1.2 mg/kg/day. When we applied the reference values from the Academy of Pediatrics, we found that 46% of the adolescents exceeded the recommended upper limits. Coffee was the most frequently consumed caffeinated drink and the main contributor to daily caffeine intake. More than three quarters (76%) of the Italian adolescents in our study drank coffee on a daily basis and nearly half (46%) exceeded the recommended upper limits. Strategies are needed to reduce caffeine consumption by adolescents. ©2018 Foundation Acta Paediatrica. Published by John Wiley & Sons Ltd.

A thermal and chemical degradation approach to decipher pristane and phytane precursors in sedimentary organic matter

USGS Publications Warehouse

Koopmans, M.P.; Rijpstra, W.I.C.; Klapwijk, M.M.; De Leeuw, J. W.; Lewan, M.D.; Sinninghe, Damste J.S.

1999-01-01

A thermal and chemical degradation approach was followed to determine the precursors of pristane (Pr) and phytane (Ph) in samples from the Gessoso-solfifera, Ghareb and Green River Formations. Hydrous pyrolysis of these samples yields large amounts of Pr and Ph carbon skeletons, indicating that their precursors are predominantly sequestered in high-molecular-weight fractions. However, chemical degradation of the polar fraction and the kerogen of the unheated samples generally does not release large amounts of Pr and Ph. Additional information on the precursors of Pr and Ph is obtained from flash pyrolysis analyses of kerogens and residues after hydrous pyrolysis and after chemical degradation. Multiple precursors for Pr and Ph are recognised in these three samples. The main increase of the Pr/Ph ratio with increasing maturation temperature, which is associated with strongly increasing amounts of Pr and Ph, is probably due to the higher amount of precursors of Pr compared to Ph, and not to the different timing of generation of Pr and Ph.A thermal and chemical degradation approach was followed to determine the precursors of pristane (Pr) and phytane (Ph) in samples from the Gessoso-solfifera, Ghareb and Green River Formations. Hydrous pyrolysis of these samples yields large amounts of Pr and Ph carbon skeletons, indicating that their precursors are predominantly sequestered in high-molecular-weight fractions. However, chemical degradation of the polar fraction and the kerogen of the unheated samples generally does not release large amounts of Pr and Ph. Additional information on the precursors of Pr and Ph is obtained from flash pyrolysis analyses of kerogens and residues after hydrous pyrolysis and after chemical degradation. Multiple precursors for Pr and Ph are recognised in these three samples. The main increase of the Pr/Ph ratio with increasing maturation temperature, which is associated with strongly increasing amounts of Pr and Ph, is probably due to the higher amount of precursors of Pr compared to Ph, and not to the different timing of generation of Pr and Ph.

Leaching of pesticides through normal-tillage and low-tillage soil--a lysimeter study. I. Isoproturon.

PubMed

Fomsgaard, Inge S; Spliid, Niels Henrik; Felding, Gitte

2003-01-01

Isoproturon is a herbicide, which was used in Denmark against grass weeds and broad-leaved weeds until 1998. Isoproturon has frequently been detected in ground water monitoring studies. Leaching of isoproturon (N,N-dimethyl-N'-(4-(1-methylethyl)-phenyl)urea) and its metabolites, N'-(4-isopropylphenyl)-N-methylurea and N'-(4-isopropylphenyl)urea was studied in four lysimetres, two of them being replicates from a low-tillage field (lysimeter 3 and 4), the other two being replicates from a normal tillage field (lysimeter 5 and 6). In both cases the soil was a sandy loam soil with 13-14% clay. The lysimetres had a surface area of 0.5 m2 and a depth of 110 cm. Lysimeter 3 and 4 were sprayed with unlabelled isoproturon while lysimeter 5 and 6 was sprayed with a mixture of 14C-labelled and unlabelled isoproturon. The total amount of isoproturon sprayed onto each lysimeter was 63 mg, corresponding to 1.25 kg active ingredient per ha. The lysimeters were sprayed with isoproturon on October 26, 1997. The lysimetres were installed in an outdoor system in Research Centre Flakkebjerg and were thus exposed to normal climatic conditions of the area. A mean of 360 l drainage water were collected from lysimeter 3 and 4 and a mean of 375 litres from lysimeter 5 and 6. Only negligible amounts of isoproturon and its primary metabolites were found in the drainage water samples, and thus no significant difference between the two lysimeter sets was shown. In a total of 82 drainage water samples, evenly distributed between the four lysimetres isoproturon was found in detectable amounts in two samples and N'-(4-isopropylphenyl)urea was found in detectable amounts in two other samples. The detection limit for all the compounds was 0.02 microg/l. 48% and 54% of the added radioactivity were recovered from the upper 10 cm soil layer in lysimeter 5 and 6, respectively, and 17 and 14% from 10-20 cm's depth. By extraction first with an aquatic CaCl2 solution 0.49% of the added radioactivity was extracted from the upper 10 cm layer in lysimeter 5. In the subsequent extraction with acetonitril, 1.19% of the added radioactivity was extracted. In lysimeter 6, upper 10 cm, 0.2% were extracted with water and 0.56% were extracted with acetonitril. Below 10 cm's depth no measurable amounts could be extracted.

A review of dioxins/furans and methyl mercury in fish from the Penobscot river, located near Lincoln, Maine.

PubMed

Williams, Robert L; Cseh, Larry

2007-04-01

The Agency for Toxic Substances and Disease Registry (ATSDR) was requested to review the analytical results of tissue samples from fish caught in the Penobscot river in Maine, calculate fish consumption limits and provide a public health opinion regarding the health implications associated with eating the contaminated fish. Fish consumption limits were calculated to provide guidance on the amount of fish that a person may eat monthly that would probably not pose a public health threat. Earlier, in 1987, the Maine Bureau of Health (BOH) issued a fish consumption advisory for portions of the Penobscot river to protect the public from exposures to dioxins/furans and methyl mercury-contaminated fish. From 1988 to 2003 the state of Maine conducted fish surveys at four locations along the Penobscot river to monitor the levels of dioxins/furans and methyl mercury contamination. In 2005, ATSDR reviewed the sampling results for two fish species (i.e., bottom feeders and predators) collected from the Penobscot river that revealed various levels of dioxins/furans and methyl mercury. The United States Environmental Protection Agency's (US EPA) guidance for evaluating potential health threats associated with contaminated fish recommends that a minimum of two target species be sampled including one predatory and one bottom feeding species. Target species are chosen to meet the following criteria: (1) known to accumulate high concentrations of target contaminants in their tissues; (2) normally populate the freshwater system being studied; (3) are routinely caught and consumed by anglers; (4) nonmigratory; (5) pollutant-tolerant; (6) easily identified; (7) abundant and easy to collect and (8) of sufficient size to provide adequate tissue samples for analyses of contaminants (US EPA, 2000). The analytical results of these fish tissue samples appear to indicate that toxic equivalency quotients concentrations of dioxins/furans have slightly decreased since 1988. In contrast, fish tissue levels of methyl mercury appear to have increased slightly since 1988. Dioxins/furans and methyl mercury levels detected in fish tissue samples caught in the Penobscot river located near Lincoln, Maine, may continue to pose a public health hazard to persons who consume the fish daily, depending on the amount consumed. The ATSDR concurred with Maine BOH's fish advisory for dioxins/furans and methyl mercury, that is, currently in place for portions of the Penobscot river near Lincoln.

Statistical analysis of hydrological response in urbanising catchments based on adaptive sampling using inter-amount times

NASA Astrophysics Data System (ADS)

ten Veldhuis, Marie-Claire; Schleiss, Marc

2017-04-01

In this study, we introduced an alternative approach for analysis of hydrological flow time series, using an adaptive sampling framework based on inter-amount times (IATs). The main difference with conventional flow time series is the rate at which low and high flows are sampled: the unit of analysis for IATs is a fixed flow amount, instead of a fixed time window. We analysed statistical distributions of flows and IATs across a wide range of sampling scales to investigate sensitivity of statistical properties such as quantiles, variance, skewness, scaling parameters and flashiness indicators to the sampling scale. We did this based on streamflow time series for 17 (semi)urbanised basins in North Carolina, US, ranging from 13 km2 to 238 km2 in size. Results showed that adaptive sampling of flow time series based on inter-amounts leads to a more balanced representation of low flow and peak flow values in the statistical distribution. While conventional sampling gives a lot of weight to low flows, as these are most ubiquitous in flow time series, IAT sampling gives relatively more weight to high flow values, when given flow amounts are accumulated in shorter time. As a consequence, IAT sampling gives more information about the tail of the distribution associated with high flows, while conventional sampling gives relatively more information about low flow periods. We will present results of statistical analyses across a range of subdaily to seasonal scales and will highlight some interesting insights that can be derived from IAT statistics with respect to basin flashiness and impact urbanisation on hydrological response.

Standardization of a Continuous Assay for Glycosidases and Its Use for Screening Insect Gut Samples at Individual and Populational Levels

PubMed Central

Profeta, Gerson S.; Pereira, Jessica A. S.; Costa, Samara G.; Azambuja, Patricia; Garcia, Eloi S.; Moraes, Caroline da Silva; Genta, Fernando A.

2017-01-01

Glycoside Hydrolases (GHs) are enzymes able to recognize and cleave glycosidic bonds. Insect GHs play decisive roles in digestion, in plant-herbivore, and host-pathogen interactions. GH activity is normally measured by the detection of a release from the substrate of products as sugars units, colored, or fluorescent groups. In most cases, the conditions for product release and detection differ, resulting in discontinuous assays. The current protocols result in using large amounts of reaction mixtures for the obtainment of time points in each experimental replica. These procedures restrain the analysis of biological materials with limited amounts of protein and, in the case of studies regarding small insects, implies in the pooling of samples from several individuals. In this respect, most studies do not assess the variability of GH activities across the population of individuals from the same species. The aim of this work is to approach this technical problem and have a deeper understanding of the variation of GH activities in insect populations, using as models the disease vectors Rhodnius prolixus (Hemiptera: Triatominae) and Lutzomyia longipalpis (Diptera: Phlebotominae). Here we standardized continuous assays using 4-methylumbelliferyl derived substrates for the detection of α-Glucosidase, β-Glucosidase, α-Mannosidase, N-acetyl-hexosaminidase, β-Galactosidase, and α-Fucosidase in the midgut of R. prolixus and L. longipalpis with results similar to the traditional discontinuous protocol. The continuous assays allowed us to measure GH activities using minimal sample amounts with a higher number of measurements, resulting in data that are more reliable and less time and reagent consumption. The continuous assay also allows the high-throughput screening of GH activities in small insect samples, which would be not applicable to the previous discontinuous protocol. We applied continuous GH measurements to 90 individual samples of R. prolixus anterior midgut homogenates using a high-throughput protocol. α-Glucosidase and α-Mannosidase activities showed the normal distribution in the population. β-Glucosidase, β-Galactosidase, N-acetyl-hexosaminidase, and α-Fucosidase activities showed non-normal distributions. These results indicate that GHs fluorescent-based high-throughput assays apply to insect samples and that the frequency distribution of digestive activities should be considered in data analysis, especially if a small number of samples is used. PMID:28553236

Determination of Ni Release in NiTi SMA with Surface Modification by Nitrogen Plasma Immersion Ion Implantation

NASA Astrophysics Data System (ADS)

de Camargo, Eliene Nogueira; Oliveira Lobo, Anderson; Silva, Maria Margareth Da; Ueda, Mario; Garcia, Edivaldo Egea; Pichon, Luc; Reuther, Helfried; Otubo, Jorge

2011-07-01

NiTi SMA is a promising material in the biomedical area due to its mechanical properties and biocompatibility. However, the nickel in the alloy may cause allergic and toxic reactions and thus limiting its applications. It was evaluated the influence of surface modification in NiTi SMA by nitrogen plasma immersion ion implantation (varying temperatures, and exposure time as follows: <250 °C/2 h, 290 °C/2 h, and 560 °C/1 h) in the amount of nickel released using immersion test in simulated body fluid. The depth of the nitrogen implanted layer increased as the implantation temperature increased resulting in the decrease of nickel release. The sample implanted in high implantation temperature presented 35% of nickel release reduction compared to reference sample.

Enhanced spectrophotometric detection of Hg in water samples by surface plasmon resonance of Au nanoparticles after preconcentration with vortex-assisted liquid-liquid microextraction

NASA Astrophysics Data System (ADS)

Martinis, Estefanía M.; Wuilloud, Rodolfo G.

2016-10-01

This article presents an efficient, simple, and cost-effective method for the determination of trace amounts of Hg by vortex-assisted liquid-liquid microextraction (VALLME) coupled to microvolume UV-Vis spectrophotometry. This method correlates changes in the intensity of localized surface plasmon resonance (LSPR) of tetraoctylammonium bromide (TOABr) coated Au nanoparticles (NPs) after interaction with Hg2+ ion. Spectroscopic measurements of the TOABr-coated Au NPs phase with particular absorption properties (strong and well-defined absorption bands) after analyte extraction by VALLME, provide an accurate and sensitive determination of Hg in water samples, comparable with measurements obtained by atomic absorption spectrometry (AAS). Different variables including sample volume, extraction time, and TOABr-coated Au NPs dispersion volume were carefully studied; final experimental conditions were 5 mL, 120 μL and 5 min respectively. The limit of detection (LOD) was 0.8 ng mL- 1. The calibration curve was linear at concentrations between the limit of quantification (LOQ) (4.9 ng mL- 1) and up to at least 120 ng mL- 1 of Hg. The relative standard deviation for six replicate determinations of 20 ng mL- 1 of Hg was 4.7%. This method exhibited an excellent analytical performance in terms of selectivity and sensitivity and it was finally applied for Hg determination in spiked tap and mineral water samples.

Magnetic hydrophilic-lipophilic balance sorbent for efficient extraction of chemical warfare agents from water samples.

PubMed

Singh, Varoon; Purohit, Ajay Kumar; Chinthakindi, Sridhar; Goud D, Raghavender; Tak, Vijay; Pardasani, Deepak; Shrivastava, Anchal Roy; Dubey, Devendra Kumar

2016-02-19

Magnetic hydrophilic-lipophilic balance (MHLB) hybrid resin was prepared by precipitation polymerization using N-vinylpyrrolidone (PVP) and divinylbenzene (DVB) as monomers and Fe2O3 nanoparticles as magnetic material. These resins were successfully applied for the extraction of chemical warfare agents (CWAs) and their markers from water samples through magnetic dispersive solid-phase extraction (MDSPE). By varying the ratios of monomers, resin with desired hydrophilic-lipophilic balance was prepared for the extraction of CWAs and related esters of varying polarities. Amongst different composites Fe2O3 nanoparticles coated with 10% PVP+90% DVB exhibited the best recoveries varying between 70.32 and 97.67%. Parameters affecting the extraction efficiencies, such as extraction time, desorption time, nature and volume of desorption solvent, amount of extraction sorbent and the effect of salts on extraction were investigated. Under the optimized conditions, linearity was obtained in the range of 0.5-500 ng mL(-1) with correlation ranging from 0.9911-0.9980. Limits of detection and limits of quantification were 0.5-1.0 and 3.0-5.0 ng mL(-1) respectively with RSDs varying from 4.88-11.32% for markers of CWAs. Finally, the developed MDSPE method was employed for extraction of analytes from water samples of various sources and the OPCW proficiency test samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Label-free virus detection using silicon photonic microring resonators.

PubMed

McClellan, Melinda S; Domier, Leslie L; Bailey, Ryan C

2012-01-15

Viruses represent a continual threat to humans through a number of mechanisms, which include disease, bioterrorism, and destruction of both plant and animal food resources. Many contemporary techniques used for the detection of viruses and viral infections suffer from limitations such as the need for extensive sample preparation or the lengthy window between infection and measurable immune response, for serological methods. In order to develop a method that is fast, cost-effective, and features reduced sample preparation compared to many other virus detection methods, we report the application of silicon photonic microring resonators for the direct, label-free detection of intact viruses in both purified samples as well as in a complex, real-world analytical matrix. As a model system, we demonstrate the quantitative detection of Bean pod mottle virus, a pathogen of great agricultural importance, with a limit of detection of 10 ng/mL. By simply grinding a small amount of leaf sample in buffer with a mortar and pestle, infected leaves can be identified over a healthy control with a total analysis time of less than 45 min. Given the inherent scalability and multiplexing capability of the semiconductor-based technology, we feel that silicon photonic microring resonators are well-positioned as a promising analytical tool for a number of viral detection applications. Copyright © 2011 Elsevier B.V. All rights reserved.

Gold nanoparticle-based enzyme-linked antibody-aptamer sandwich assay for detection of Salmonella Typhimurium.

PubMed

Wu, Wenhe; Li, Jun; Pan, Dun; Li, Jiang; Song, Shiping; Rong, Mingge; Li, Zixi; Gao, Jimin; Lu, Jianxin

2014-10-08

Enzyme-linked immunosorbent assay (ELISA) provides a convenient means for the detection of Salmonella enterica serovar Typhimurium (STM), which is important for rapid diagnosis of foodborne pathogens. However, conventional ELISA is limited by antibody-antigen immunoreactions and suffers from poor sensitivity and tedious sample pretreatment. Therefore, development of novel ELISA remains challenging. Herein, we designed a comprehensive strategy for rapid, sensitive, and quantitative detection of STM with high specificity by gold nanoparticle-based enzyme-linked antibody-aptamer sandwich (nano-ELAAS) method. STM was captured and preconcentrated from samples with aptamer-modified magnetic particles, followed by binding with detector antibodies. Then nanoprobes carrying a large amount of reporter antibodies and horseradish peroxidase molecules were used for colorimetric signal amplification. Under the optimized reaction conditions, the nano-ELAAS assay had a quantitative detection range from 1 × 10(3) to 1 × 10(8) CFU mL(-1), a limit of detection of 1 × 10(3) CFU mL(-1), and a selectivity of >10-fold for STM in samples containing other bacteria at higher concentration with an assay time less than 3 h. In addition, the developed nanoprobes were improved in terms of detection range and/or sensitivity when compared with two commercial enzyme-labeled antibody signal reporters. Finally, the nano-ELAAS method was demonstrated to work well in milk samples, a common source of STM contamination.

Green and simple analytical method to determine benzimidazoles in milk samples by using salting-out assisted liquid-liquid extraction and capillary liquid chromatography.

PubMed

Tejada-Casado, Carmen; Del Olmo-Iruela, Monsalud; García-Campaña, Ana M; Lara, Francisco J

2018-08-01

A green and simple multiresidue method using capillary liquid chromatography (CLC) with UV-diode array detection (DAD) has been developed for the determination of sixteen benzimidazoles (BZs) and its metabolites in milk samples. The separation was achieved in <32 min, using a Zorbax XDB-C18 column (150 mm × 0.5 mm I.D, 5 μm), with a mobile phase consisting of 50 mM ammonium acetate (solvent A) and a mixture of acetonitrile/methanol (1:1 v/v) (solvent B), at a flow rate of 9 μL min -1 . The temperature of the column was 20 °C and 6 μL of sample were injected. In spite of the complexity of milk samples, an effective, simple and fast sample preparation method called salting out-assisted liquid-liquid extraction (SALLE) was developed for the analysis of these compounds in cow milk samples. To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized including the amount of sample, type and volume of the extraction solvent, and the nature and amount of the salt. Good linearity was obtained (R 2  > 0.9985 for all BZs) with limits of detection (LOD) between 1.0 and 2.8 μg kg -1 . Relative standard deviations of repeatability and intermediate precision were below 1.6 and 14.2%, respectively. Satisfactory recoveries between 79.1 and 99.6% were also obtained for three types of milk samples (cow, sheep and goat). The advantages of a miniaturized technique such as CLC in terms of better efficiencies and reduced solvent consumption, combined with the simplicity of the SALLE procedure, make this method a useful alternative for the monitoring of these residues at trace level. Copyright © 2018 Elsevier B.V. All rights reserved.

Ionic liquid-salt aqueous two-phase extraction based on salting-out coupled with high-performance liquid chromatography for the determination of sulfonamides in water and food.

PubMed

Han, Juan; Wang, Yun; Liu, Yan; Li, Yanfang; Lu, Yang; Yan, Yongsheng; Ni, Liang

2013-02-01

Ionic liquid-salt aqueous two-phase extraction coupled with high-performance liquid chromatography with ultraviolet detection was developed for the determination of sulfonamides in water and food samples. In the procedure, the analytes were extracted from the aqueous samples into the ionic liquid top phase in one step. Three sulfonamides, sulfamerazine, sulfamethoxazole, and sulfamethizole were selected here as model compounds for developing and evaluating the method. The effects of various experimental parameters in extraction step were studied using two optimization methods, one variable at a time and Box-Behnken design. The results showed that the amount of sulfonamides did not have effect on the extraction efficiency. Therefore, a three-level Box-Behnken experimental design with three factors, which combined the response surface modeling, was used to optimize sulfonamides extraction. Under the most favorable extraction parameters, the detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target compounds were achieved within the range of 0.15-0.3 ng/mL and 0.5-1.0 ng/mL from spiked samples, respectively, which are lower than or comparable with other reported approaches applied to the determination of the same compounds. Finally, the proposed method was successfully applied to the determination of sulfonamide compounds in different water and food samples and satisfactory recoveries of spiked target compounds in real samples were obtained.

Porphyrin-based magnetic nanocomposites for efficient extraction of polycyclic aromatic hydrocarbons from water samples.

PubMed

Yu, Jing; Zhu, Shukui; Pang, Liling; Chen, Pin; Zhu, Gang-Tian

2018-03-09

Stable and reusable porphyrin-based magnetic nanocomposites were successfully synthesized for efficient extraction of polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. Meso-Tetra (4-carboxyphenyl) porphyrin (TCPP), a kind of porphyrin, can connect the copolymer after amidation and was linked to Fe 3 O 4 @SiO 2 magnetic nanospheres via cross-coupling. Several characteristic techniques such as field emission scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Fourier transform infrared spectrometry, vibrating sample magnetometry and a tensiometer were used to characterize the as-synthesized materials. The structure of the copolymer was similar to that of graphene, possessing sp 2 -conjugated carbon rings, but with an appropriate amount of delocalized π-electrons giving rise to the higher extraction efficiency for heavy PAHs without sacrificing the performance in the extraction of light PAHs. Six extraction parameters, including the TCPP:Fe 3 O 4 @SiO 2 (m:m) ratio, the amount of adsorbents, the type of desorption solvent, the desorption solvent volume, the adsorption time and the desorption time, were investigated. After the optimization of extraction conditions, a comparison of the extraction efficiency of Fe 3 O 4 @SiO 2 -TCPP and Fe 3 O 4 @SiO 2 @GO was carried out. The adsorption mechanism of TCPP to PAHs was studied by first-principles density functional theory (DFT) calculations. Combining experimental and calculated results, it was shown that the π-π stacking interaction was the main adsorption mechanism of TCPP for PAHs and that the amount of delocalized π-electrons plays an important role in the elution process. Under the optimal conditions, Fe 3 O 4 @SiO 2 -porphyrin showed good precision in intra-day (<8.9%) and inter-day (<13.0%) detection, low method detection limits (2-10 ng L -1 ), and wide linearity (10-10000 ng L -1 ). The method was applied to simultaneous analysis of 15 PAHs with acceptable recoveries, which were 71.1%-106.0% for ground water samples and 73.7%-107.1% for Yangtze River water samples, respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

Trace analysis of nitrite ions in environmental samples by using in-situ synthesized Zein biopolymeric nanoparticles as the novel green solid phase extractor.

PubMed

Hatamie, Amir; Nassiri, Mahmoud; Alivand, Meghdad Doust; Bhatnagar, Amit

2018-01-01

For the first time, a novel green method using Zein biopolymeric nanoparticles as a green dispersive solid-phase extractor is reported for the separation and preconcentration of trace amount of nitrite (NO 2 - ) ions in ppb levels. The Zein protein is a biodegradable hydrophobic plant protein that is obtained from corn and is composed of a number of hydrophobic amino acids. Zein bionanoparticles were synthesized in an anti-solvent process and used as a new biosorbent in the extraction technique. In the proposed technique, by using a standard method at first, a mixture of 1-naphthylamine and sulphanilic acid as selective regents was added to the samples, and in the presence of the nitrite ion, a red azo product was formed. After that, the ethanolic Zein solution (equal to 15mg) was injected rapidly into the sample, based on the anti-solvent process. Zein bionanoparticles (BNPs) were produced, the adsorbed colour product was separated by centrifugation, and finally samples were analysed with the spectrophotometric method. The influence of different variables such as pH, buffer and amount of buffer, amount of adsorbent and effect of time on extraction were investigated and Zein BNPs were characterized by TEM, SEM, and FT-IR techniques. The main advantages of Zein as a new solid-phase extractor are that this biopolymer is non-toxic, stable, widely available, biodegradable, very hydrophobic, and can be fabricated easily. Under optimal experimental conditions, the linear correlation coefficient (r 2 ) was found to be 0.9972 at the concentration range of 5.0-1000ngmL -1 . The limit of detection was 2.3ngmL -1 (0.05μM). This method was applied successfully for the analysis of sea and river waters as well as industrial wastewater samples. Finally, this method follows the US EPA (US Environmental Protection Agency) and WHO (World Health Organization) international standards for nitrite analysis. In addition, it has several advantages to warrant its applicability in the near future in separation science as a green biosorbent in both dispersive and normal solid-phase extraction. Copyright © 2017. Published by Elsevier B.V.

Whole genome amplification and real-time PCR in forensic casework

PubMed Central

Giardina, Emiliano; Pietrangeli, Ilenia; Martone, Claudia; Zampatti, Stefania; Marsala, Patrizio; Gabriele, Luciano; Ricci, Omero; Solla, Gianluca; Asili, Paola; Arcudi, Giovanni; Spinella, Aldo; Novelli, Giuseppe

2009-01-01

Background WGA (Whole Genome Amplification) in forensic genetics can eliminate the technical limitations arising from low amounts of genomic DNA (gDNA). However, it has not been used to date because any amplification bias generated may complicate the interpretation of results. Our aim in this paper was to assess the applicability of MDA to forensic SNP genotyping by performing a comparative analysis of genomic and amplified DNA samples. A 26-SNPs TaqMan panel specifically designed for low copy number (LCN) and/or severely degraded genomic DNA was typed on 100 genomic as well as amplified DNA samples. Results Aliquots containing 1, 0.1 and 0.01 ng each of 100 DNA samples were typed for a 26-SNPs panel. Similar aliquots of the same DNA samples underwent multiple displacement amplification (MDA) before being typed for the same panel. Genomic DNA samples showed 0% PCR failure rate for all three dilutions, whilst the PCR failure rate of the amplified DNA samples was 0% for the 1 ng and 0.1 ng dilutions and 0.077% for the 0.01 ng dilution. The genotyping results of both the amplified and genomic DNA samples were also compared with reference genotypes of the same samples obtained by direct sequencing. The genomic DNA samples showed genotype concordance rates of 100% for all three dilutions while the concordance rates of the amplified DNA samples were 100% for the 1 ng and 0.1 ng dilutions and 99.923% for the 0.01 ng dilution. Moreover, ten artificially-degraded DNA samples, which gave no results when analyzed by current forensic methods, were also amplified by MDA and genotyped with 100% concordance. Conclusion We investigated the suitability of MDA material for forensic SNP typing. Comparative analysis of amplified and genomic DNA samples showed that a large number of SNPs could be accurately typed starting from just 0.01 ng of template. We found that the MDA genotyping call and accuracy rates were only slightly lower than those for genomic DNA. Indeed, when 10 pg of input DNA was used in MDA, we obtained 99.923% concordance, indicating a genotyping error rate of 1/1299 (7.7 × 10-4). This is quite similar to the genotyping error rate of STRs used in current forensic analysis. Such efficiency and accuracy of SNP typing of amplified DNA suggest that MDA can also generate large amounts of genome-equivalent DNA from a minimal amount of input DNA. These results show for the first time that MDA material is suitable for SNP-based forensic protocols and in general when samples fail to give interpretable STR results. PMID:19366436

Aldicarb-pesticide contamination of ground water in eastern Suffolk County, Long Island, New York

USGS Publications Warehouse

Soren, Julian; Stelz, W.G.

1984-01-01

Aldicarb, a toxic oxime-carbamate pesticide that was believed incapable of reaching ground water, was used in potato-farming areas of eastern Suffolk County, New York during 1975-80. In 1979, aldicarb was found in substantial concentrations in ground water throughout the area. The New York State Department of Health set a limit of 7 micrograms per liter for aldicarb in drinking water. Extensive ground-water sampling into 1980 showed widespread contamination ranging from small amounts to as much as 515 micrograms per liter. In 1980, the U.S. Environmental Protection Agency banned the use of aldicarb on Long Island at the manufacturer 's request. A 1982 sampling study found aldicarb to have penetrated to about 40 feet below the water table in concentrations ranging from below detection limit to 239 micrograms per liter. Despite reputed toxicity, no instance of aldicarb poisoning on Long Island has been documented. The excessive aldicarb concentrations in the ground water of eastern Long Island may persist for decades; the duration has not been precisely determined and remains under investigation. (USGS)

Determination of Chlorine in Milk via Molecular Absorption of SrCl Using High-Resolution Continuum Source Graphite Furnace Atomic Absorption Spectrometry.

PubMed

Ozbek, Nil; Akman, Suleyman

2016-07-20

Total chlorine in milk was determined via the molecular absorption of diatomic strontium monochloride at 635.862 nm using high-resolution continuum source graphite furnace atomic absorption spectrometry. The effects of coating the graphite furnace, using different modifiers, amount of molecule-forming element, and different calibrants were investigated and optimized. Chlorine concentrations in milk samples were determined in a Zr-coated graphite furnace using 25 μg of Sr as the molecule-forming reagent and applying a pyrolysis temperature of 600 °C and a molecule-forming temperature of 2300 °C. Linearity was maintained up to 500 μg mL(-1) of Cl. The method was tested by analyzing a certified reference wastewater. The results were in the uncertainty limits of the certified value. The limit of detection of the method was 1.76 μg mL(-1). The chlorine concentrations in various cow milk samples taken from the market were found in the range of 588-1472 mg L(-1).

Comprehensive sample analysis using high performance liquid chromatography with multi-detection.

PubMed

Pravadali, Sercan; Bassanese, Danielle N; Conlan, Xavier A; Francis, Paul S; Smith, Zoe M; Terry, Jessica M; Shalliker, R Andrew

2013-11-25

Herein we assess the separation space offered by a liquid chromatography system with an optimised uni-dimensional separation for the determination of the key chemical entities in the highly complex matrix of a tobacco leaf extract. Multiple modes of detection, including UV-visible absorbance, chemiluminescence (acidic potassium permanganate, manganese(IV), and tris(2,2'-bipyridine)ruthenium(III)), mass spectrometry and DPPH radical scavenging were used in an attempt to systematically reduce the data complexity of the sample whilst obtaining a greater degree of molecule-specific information. A large amount of chemical data was obtained, but several limitations in the ability to assign detector responses to particular compounds, even with the aid of complementary detection systems, were observed. Thirty-three compounds were detected via MS on the tobacco extract and 12 out of 32 compounds gave a peak height ratio (PHR) greater than 0.33 on one or more detectors. This paper serves as a case study of these limitations, illustrating why multidimensional chromatography is an important consideration when developing a comprehensive chemical detection system. Copyright © 2013 Elsevier B.V. All rights reserved.

Separation and quantification of monoclonal-antibody aggregates by hollow-fiber-flow field-flow fractionation.

PubMed

Fukuda, Jun; Iwura, Takafumi; Yanagihara, Shigehiro; Kano, Kenji

2014-10-01

Hollow-fiber-flow field-flow fractionation (HF5) separates protein molecules on the basis of the difference in the diffusion coefficient, and can evaluate the aggregation ratio of proteins. However, HF5 is still a minor technique because information on the separation conditions is limited. We examined in detail the effect of different settings, including the main-flow rate, the cross-flow rate, the focus point, the injection amount, and the ionic strength of the mobile phase, on fractographic characteristics. On the basis of the results, we proposed optimized conditions of the HF5 method for quantification of monoclonal antibody in sample solutions. The HF5 method was qualified regarding the precision, accuracy, linearity of the main peak, and quantitation limit. In addition, the HF5 method was applied to non-heated Mab A and heat-induced-antibody-aggregate-containing samples to evaluate the aggregation ratio and the distribution extent. The separation performance was comparable with or better than that of conventional methods including analytical ultracentrifugation-sedimentation velocity and asymmetric-flow field-flow fractionation.

Azocasein Substrate for Determination of Proteolytic Activity: Reexamining a Traditional Method Using Bromelain Samples.

PubMed

Coêlho, Diego F; Saturnino, Thais Peron; Fernandes, Fernanda Freitas; Mazzola, Priscila Gava; Silveira, Edgar; Tambourgi, Elias Basile

2016-01-01

Given the importance of protease's worldwide market, the determination of optimum conditions and the development of a standard protocol are critical during selection of a reliable method to determine its bioactivity. This paper uses quality control theory to validate a modified version of a method proposed by Charney and Tomarelli in 1947. The results obtained showed that using azocasein substrate bromelain had its optimum at 45°C and pH 9 (Glycine-NaOH 100 mM). We also quantified the limit of detection (LoD) and limit of quantification (LoQ) in the above-mentioned optimum (0.072 and 0.494 mg·mL(-1) of azocasein, resp.) and a calibration curve that correlates optical density with the amount of substrate digested. In all analysed samples, we observed a significant decrease in response after storage (around 17%), which suggests its use must be immediately after preparation. Thus, the protocol presented in this paper offers a significant improvement, given that subjective definitions are commonly used in the literature and this simple mathematical approach makes it clear and concise.

Azocasein Substrate for Determination of Proteolytic Activity: Reexamining a Traditional Method Using Bromelain Samples

PubMed Central

Mazzola, Priscila Gava

2016-01-01

Given the importance of protease's worldwide market, the determination of optimum conditions and the development of a standard protocol are critical during selection of a reliable method to determine its bioactivity. This paper uses quality control theory to validate a modified version of a method proposed by Charney and Tomarelli in 1947. The results obtained showed that using azocasein substrate bromelain had its optimum at 45°C and pH 9 (Glycine-NaOH 100 mM). We also quantified the limit of detection (LoD) and limit of quantification (LoQ) in the above-mentioned optimum (0.072 and 0.494 mg·mL−1 of azocasein, resp.) and a calibration curve that correlates optical density with the amount of substrate digested. In all analysed samples, we observed a significant decrease in response after storage (around 17%), which suggests its use must be immediately after preparation. Thus, the protocol presented in this paper offers a significant improvement, given that subjective definitions are commonly used in the literature and this simple mathematical approach makes it clear and concise. PMID:26925415

Fast and direct screening of copper in micro-volumes of distilled alcoholic beverages by high-resolution continuum source graphite furnace atomic absorption spectrometry.

PubMed

Ajtony, Zsolt; Laczai, Nikoletta; Dravecz, Gabriella; Szoboszlai, Norbert; Marosi, Áron; Marlok, Bence; Streli, Christina; Bencs, László

2016-12-15

HR-CS-GFAAS methods were developed for the fast determination of Cu in domestic and commercially available Hungarian distilled alcoholic beverages (called pálinka), in order to decide if their Cu content exceeds the permissible limit, as legislated by the WHO. Some microliters of samples were directly dispensed into the atomizer. Graphite furnace heating programs, effects/amounts of the Pd modifier, alternative wavelengths (e.g., Cu I 249.2146nm), external calibration and internal standardization methods were studied. Applying a fast graphite furnace heating program without any chemical modifier, the Cu content of a sample could be quantitated within 1.5min. The detection limit of the method is 0.03mg/L. Calibration curves are linear up to 10-15mg/L Cu. Spike-recoveries ranged from 89% to 119% with an average of 100.9±8.5%. Internal calibration could be applied with the assistance of Cr, Fe, and/or Rh standards. The accuracy of the GFAAS results was verified by TXRF analyses. Copyright © 2016 Elsevier Ltd. All rights reserved.

Fully-automated in-syringe dispersive liquid-liquid microextraction for the determination of caffeine in coffee beverages.

PubMed

Frizzarin, Rejane M; Maya, Fernando; Estela, José M; Cerdà, Víctor

2016-12-01

A novel fully-automated magnetic stirring-assisted lab-in-syringe analytical procedure has been developed for the fast and efficient dispersive liquid-liquid microextraction (DLLME) of caffeine in coffee beverages. The procedure is based on the microextraction of caffeine with a minute amount of dichloromethane, isolating caffeine from the sample matrix with no further sample pretreatment. Selection of the relevant extraction parameters such as the dispersive solvent, proportion of aqueous/organic phase, pH and flow rates have been carefully evaluated. Caffeine quantification was linear from 2 to 75mgL(-1), with detection and quantification limits of 0.46mgL(-1) and 1.54mgL(-1), respectively. A coefficient of variation (n=8; 5mgL(-1)) of a 2.1% and a sampling rate of 16h(-1), were obtained. The procedure was satisfactorily applied to the determination of caffeine in brewed, instant and decaf coffee samples, being the results for the sample analysis validated using high-performance liquid chromatography. Copyright © 2016 Elsevier Ltd. All rights reserved.

Hypercrosslinked particles for the extraction of sweeteners using dispersive solid-phase extraction from environmental samples.

PubMed

Lakade, Sameer S; Zhou, Qing; Li, Aimin; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa M

2018-04-01

This work presents a new extraction material, namely, Q-100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid-phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q-100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior toward sweeteners. Different dispersive solid-phase extraction parameters such as amount of magnetic particles or extraction time were optimized. Under optimum conditions, Q-100 showed suitable apparent recovery, ranging in the case of river water sample from 21 to 88% for all the sweeteners, except for alitame (12%). The validated method based on dispersive solid-phase extraction using Q-100 followed by liquid chromatography with tandem mass spectrometry provided good linearity and limits of quantification between 0.01 and 0.1 μg/L. The method was applied to analyze samples from river water and effluent wastewater, and four sweeteners (acesulfame, saccharin, cyclamate, and sucralose) were found in both types of sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A simple, rapid and novel method based on salting-out assisted liquid-liquid extraction for ochratoxin A determination in beer samples prior to ultra-high performance liquid chromatography coupled to tandem mass spectrometry.

PubMed

Mariño-Repizo, Leonardo; Goicoechea, Hector; Raba, Julio; Cerutti, Soledad

2018-06-07

A novel, simple, easy and cheap sample treatment strategy based on salting-out assisted liquid-liquid extraction (SALLE) for ochratoxin A (OTA) ultra-trace analysis in beer samples using ultra-high performance liquid chromatography-tandem mass spectrometry determination was developed. The factors involved in the efficiency of pretreatment were studied employing factorial design in the screening phase and the optimal conditions of the significant variables on the analytical response were evaluated using a central composite face-centred design (CCF). Consequently, the amount of salt ((NH 4 ) 2 SO 4 ), together with the volumes of sample, hydrophilic (acetone) and nonpolar (toluene) solvents, and times of vortexing and centrifugation were optimized. Under optimized conditions, the limits of detection (LOD) and quantification (LOQ) were 0.02 µg l -1 and 0.08 µg l -1 respectively. OTA extraction recovery by SALLE was approximately 90% (0.2 µg l -1 ). Furthermore, the methodology was in agreement with EU Directive requirements and was successfully applied for analysis of beer samples.

A combined method for DNA analysis and radiocarbon dating from a single sample.

PubMed

Korlević, Petra; Talamo, Sahra; Meyer, Matthias

2018-03-07

Current protocols for ancient DNA and radiocarbon analysis of ancient bones and teeth call for multiple destructive samplings of a given specimen, thereby increasing the extent of undesirable damage to precious archaeological material. Here we present a method that makes it possible to obtain both ancient DNA sequences and radiocarbon dates from the same sample material. This is achieved by releasing DNA from the bone matrix through incubation with either EDTA or phosphate buffer prior to complete demineralization and collagen extraction utilizing the acid-base-acid-gelatinization and ultrafiltration procedure established in most radiocarbon dating laboratories. Using a set of 12 bones of different ages and preservation conditions we demonstrate that on average 89% of the DNA can be released from sample powder with minimal, or 38% without any, detectable collagen loss. We also detect no skews in radiocarbon dates compared to untreated samples. Given the different material demands for radiocarbon dating (500 mg of bone/dentine) and DNA analysis (10-100 mg), combined DNA and collagen extraction not only streamlines the sampling process but also drastically increases the amount of DNA that can be recovered from limited sample material.

Coupling detergent lysis/clean-up methodology with intact protein fractionation for enhanced proteome characterization

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

Sharma, Ritin; Dill, Brian; Chourey, Karuna

2012-01-01

The expanding use of surfactants for proteome sample preparations has prompted the need to systematically optimize the application and removal of these MS-deleterious agents prior to proteome measurements. Here we compare four different detergent clean-up methods (Trichloroacetic acid (TCA) precipitation, Chloroform/Methanol/Water (CMW) extraction, commercial detergent removal spin column method (DRS) and filter-aided sample preparation(FASP)) with respect to varying amounts of protein biomass in the samples, and provide efficiency benchmarks with respect to protein, peptide, and spectral identifications for each method. Our results show that for protein limited samples, FASP outperforms the other three clean-up methods, while at high protein amountmore » all the methods are comparable. This information was used in a dual strategy of comparing molecular weight based fractionated and unfractionated lysates from three increasingly complex samples (Escherichia coli, a five microbial isolate mixture, and a natural microbial community groundwater sample), which were all lysed with SDS and cleaned up using FASP. The two approaches complemented each other by enhancing the number of protein identifications by 8%-25% across the three samples and provided broad pathway coverage.« less

Simulated nutrient dissolution of Asian aerosols in various atmospheric waters: Potential links to marine primary productivity

NASA Astrophysics Data System (ADS)

Wang, Lingyan; Bi, Yanfeng; Zhang, Guosen; Liu, Sumei; Zhang, Jing; Xu, Zhaomeng; Ren, Jingling; Zhang, Guiling

2017-09-01

To probe the bioavailability and environmental mobility of aerosol nutrient elements (N, P, Si) in atmospheric water (rainwater, cloud and fog droplets), ten total suspended particulate (TSP) samples were collected at Fulong Mountain, Qingdao from prevailing air mass trajectory sources during four seasons. Then, a high time-resolution leaching experiment with simulated non-acidic atmospheric water (non-AAW, Milli-Q water, pH 5.5) and subsequently acidic atmospheric water (AAW, hydrochloric acid solution, pH 2) was performed. We found that regardless of the season or source, a monotonous decreasing pattern was observed in the dissolution of N, P and Si compounds in aerosols reacted with non-AAW, and the accumulated dissolved curves of P and Si fit a first-order kinetic model. No additional NO3- + NO2- dissolved out, while a small amount of NH4+ in Asian dust (AD) samples was released in AAW. The similar dissolution behaviour of P and Si from non-AAW to AAW can be explained by the Transition State Theory. The sources of aerosols related to various minerals were the natural reasons that affected the amounts of bioavailable phosphorus and silicon in aerosols (i.e., solubility), which can be explained by the dissolution rate constant of P and Si in non-AAW with lower values in mineral aerosols. The acid/particle ratio and particle/liquid ratio also have a large effect on the solubility of P and Si, which was implied by Pearson correlation analysis. Acid processing of aerosols may have great significance for marine areas with limited P and Si and post-acidification release increases of 1.1-10-fold for phosphorus and 1.2-29-fold for silicon. The decreasing mole ratio of P and Si in AAW indicates the possibility of shifting from a Si-limit to a P-limit in aerosols in the ocean, which promotes the growth of diatoms prior to other algal species.

Imaging study of using radiopharmaceuticals labeled with cyclotron-produced 99mTc.

PubMed

Hou, X; Tanguay, J; Vuckovic, M; Buckley, K; Schaffer, P; Bénard, F; Ruth, T J; Celler, A

2016-12-07

Cyclotron-produced 99m Tc (CPTc) has been recognized as an attractive and practical substitution of reactor/generator based 99m Tc. However, the small amount of 92-98 Mo in the irradiation of enriched 100 Mo could lead to the production of other radioactive technetium isotopes (Tc-impurities) which cannot be chemically separated. Thus, these impurities could contribute to patient dose and affect image quality. The potential radiation dose caused by these Tc-impurities produced using different targets, irradiation conditions, and corresponding to different injection times have been investigated, leading us to create dose-based limits of these parameters for producing clinically acceptable CPTc. However, image quality has been not considered. The aim of the present work is to provide a comprehensive and quantitative analysis of image quality for CPTc. The impact of Tc-impurities in CPTc on image resolution, background noise, and contrast is investigated by performing both Monte-Carlo simulations and phantom experiments. Various targets, irradiation, and acquisition conditions are employed for investigating the image-based limits of CPTc production parameters. Additionally, the relationship between patient dose and image quality of CPTc samples is studied. Only those samples which meet both dose- and image-based limits should be accepted in future clinical studies.

Imaging study of using radiopharmaceuticals labeled with cyclotron-produced 99mTc

NASA Astrophysics Data System (ADS)

Hou, X.; Tanguay, J.; Vuckovic, M.; Buckley, K.; Schaffer, P.; Bénard, F.; Ruth, T. J.; Celler, A.

2016-12-01

Cyclotron-produced 99mTc (CPTc) has been recognized as an attractive and practical substitution of reactor/generator based 99mTc. However, the small amount of 92-98Mo in the irradiation of enriched 100Mo could lead to the production of other radioactive technetium isotopes (Tc-impurities) which cannot be chemically separated. Thus, these impurities could contribute to patient dose and affect image quality. The potential radiation dose caused by these Tc-impurities produced using different targets, irradiation conditions, and corresponding to different injection times have been investigated, leading us to create dose-based limits of these parameters for producing clinically acceptable CPTc. However, image quality has been not considered. The aim of the present work is to provide a comprehensive and quantitative analysis of image quality for CPTc. The impact of Tc-impurities in CPTc on image resolution, background noise, and contrast is investigated by performing both Monte-Carlo simulations and phantom experiments. Various targets, irradiation, and acquisition conditions are employed for investigating the image-based limits of CPTc production parameters. Additionally, the relationship between patient dose and image quality of CPTc samples is studied. Only those samples which meet both dose- and image-based limits should be accepted in future clinical studies.

34 CFR 682.506 - Limitations on maximum loan amounts.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 34 Education 3 2010-07-01 2010-07-01 false Limitations on maximum loan amounts. 682.506 Section 682.506 Education Regulations of the Offices of the Department of Education (Continued) OFFICE OF POSTSECONDARY EDUCATION, DEPARTMENT OF EDUCATION FEDERAL FAMILY EDUCATION LOAN (FFEL) PROGRAM Federal Guaranteed...

High-throughput simultaneous analysis of RNA, protein, and lipid biomarkers in heterogeneous tissue samples.

PubMed

Reiser, Vladimír; Smith, Ryan C; Xue, Jiyan; Kurtz, Marc M; Liu, Rong; Legrand, Cheryl; He, Xuanmin; Yu, Xiang; Wong, Peggy; Hinchcliffe, John S; Tanen, Michael R; Lazar, Gloria; Zieba, Renata; Ichetovkin, Marina; Chen, Zhu; O'Neill, Edward A; Tanaka, Wesley K; Marton, Matthew J; Liao, Jason; Morris, Mark; Hailman, Eric; Tokiwa, George Y; Plump, Andrew S

2011-11-01

With expanding biomarker discovery efforts and increasing costs of drug development, it is critical to maximize the value of mass-limited clinical samples. The main limitation of available methods is the inability to isolate and analyze, from a single sample, molecules requiring incompatible extraction methods. Thus, we developed a novel semiautomated method for tissue processing and tissue milling and division (TMAD). We used a SilverHawk atherectomy catheter to collect atherosclerotic plaques from patients requiring peripheral atherectomy. Tissue preservation by flash freezing was compared with immersion in RNAlater®, and tissue grinding by traditional mortar and pestle was compared with TMAD. Comparators were protein, RNA, and lipid yield and quality. Reproducibility of analyte yield from aliquots of the same tissue sample processed by TMAD was also measured. The quantity and quality of biomarkers extracted from tissue prepared by TMAD was at least as good as that extracted from tissue stored and prepared by traditional means. TMAD enabled parallel analysis of gene expression (quantitative reverse-transcription PCR, microarray), protein composition (ELISA), and lipid content (biochemical assay) from as little as 20 mg of tissue. The mean correlation was r = 0.97 in molecular composition (RNA, protein, or lipid) between aliquots of individual samples generated by TMAD. We also demonstrated that it is feasible to use TMAD in a large-scale clinical study setting. The TMAD methodology described here enables semiautomated, high-throughput sampling of small amounts of heterogeneous tissue specimens by multiple analytical techniques with generally improved quality of recovered biomolecules.

Modified thermal-optical analysis using spectral absorption selectivity to distinguish black carbon from pyrolized organic carbon.

PubMed

Hadley, Odelle L; Corrigan, Craig E; Kirchstetter, Thomas W

2008-11-15

This study presents a method for analyzing the black carbon (BC) mass loading on a quartz fiber filter using a modified thermal-optical analysis method, wherein light transmitted through the sample is measured over a spectral region instead of at a single wavelength. Evolution of the spectral light transmission signal depends on the relative amounts of light-absorbing BC and char, the latter of which forms when organic carbon in the sample pyrolyzes during heating. Absorption selectivities of BC and char are found to be distinct and are used to apportion the amount of light attenuated by each component in the sample. Light attenuation is converted to mass concentration on the basis of derived mass attenuation efficiencies (MAEs) of BC and char. The fractions of attenuation due to each component are scaled by their individual MAE values and added together as the total mass of light absorbing carbon (LAC). An iterative algorithm is used to find the MAE values for both BC and char that provide the best fit to the carbon mass remaining on the filter (derived from direct measurements of thermally evolved CO2) at temperatures higher than 480 degrees C. This method was applied to measure the BC concentration in precipitation samples collected in northern California. The uncertainty in the measured BC concentration of samples that contained a high concentration of organics susceptible to char ranged from 12% to 100%, depending on the mass loading of BC on the filter. The lower detection limit for this method was approximately 0.35 microg of BC, and the uncertainty approached 20% for BC mass loading greater than 1.0 microg of BC.

Understanding shallow gas occurrences in the Gulf of Lions

USGS Publications Warehouse

Garcia-Garcia, Ana; Tesi, Tommaso; Orange, Daniel L.; Lorenson, T.; Miserocchi, Stefano; Langone, L.; Herbert, I.; Dougherty, J.

2007-01-01

New coring data have been acquired along the western Gulf of Lions showing anomalous concentrations of methane (up to 95,700 ppm) off the Rho??ne prodelta and the head of the southern canyons Lacaze-Duthiers and Cap de Creus. Sediment cores were acquired with box and kasten cores during 2004-2005 on several EuroSTRATAFORM cruises. Anomalous methane concentrations are discussed and integrated with organic carbon data. Sampled sites include locations where previous surveys identified acoustic anomalies in high-resolution seismic profiles, which may be related to the presence of gas. Interpretation of the collected data has enabled us to discuss the nature of shallow gas along the Gulf of Lions, and its association with recent sedimentary dynamics. The Rho??ne prodelta flood deposits deliver significant amounts of terrigenous organic matter that can be rapidly buried, effectively removing this organic matter from aerobic oxidation and biological uptake, and leading to the potential for methanogenesis with burial. Away from the flood-related sediments off the Rho??ne delta, the organic matter is being reworked and remineralized on its way along the western coast of the Gulf of Lions, with the result that the recent deposits in the canyon contain little reactive carbon. In the southernmost canyons, Lacaze-Duthiers and Cap de Creus, the gas analyses show relatively little shallow gas in the core samples. Samples with anomalous gas (up to 5,000 ppm methane) are limited to local areas where the samples also show higher amounts of organic matter. The anomalous samples at the head of the southern canyons may be related to methanogenesis of recent drape or of older sidewall canyon infills. ?? Springer-Verlag 2007.

Chemical and mineralogical analysis of devonian black-shale samples from Martin County, Kentucky; Carroll and Washington counties, Ohio; Wise County, Virginia; and Overton County, Tennessee, U.S.A.

USGS Publications Warehouse

Leventhal, J.S.; Hosterman, J.W.

1982-01-01

Core samples of Devonian shales from five localities in the Appalachian basin have been analyzed chemically and mineralogically. The amounts of major elements are similar; however, the minor constituents, organic C, S, phosphate and carbonate show ten-fold variations in amounts. Trace elements Mo, Ni, Cu, V, Co, U, Zn, Hg, As and Mn show variations in amounts that can be related to the minor constituents. All samples contain major amounts of quartz, illite, two types of mixed-layer clays, and chlorite in differing quantities. Pyrite, calcite, feldspar and kaolinite are also present in many samples in minor amounts. Dolomite, apatite, gypsum, barite, biotite and marcasite are present in a few samples in trace amounts. Trace elements listed above are strongly controlled by organic C with the exception of Mn which is associated with carbonate minerals. Amounts of organic C generally range from 3 to 6%, and S is in the range of 2-5%. Amounts of trace elements show the following general ranges in ppm (parts per million): Co, 20-40; Cu, 40-70; U, 10-40; As, 20-40; V, 150-300; Ni, 80-150; high values are as much as twice these values. The organic C was probably the concentrating agent, and the organic C and sulfide S together created an environment that immobilized and preserved these trace elements. Closely spaced samples showing an abrupt transition in color also show changes in organic C, S and trace-element contents. Several associations exist between mineral and chemical content. Pyrite and marcasite are the only minerals found to contain sulfide-S. In general, the illite-chlorite mixed-layer clay mineral shows covariation with organic C if calcite is not present. The enriched trace elements are not related to the clay types, although the clay and organic matter are intimately associated as the bulk fabric of the rock. ?? 1982.

Solvent cleaning of pole transformers containing PCB contaminated insulating oil.

PubMed

Kanbe, H; Shibuya, M

2001-01-01

In 1989, it was discovered that the recycled insulation oil in pole transformers for electric power supply was contaminated with trace amounts of polychlorinated biphenyls (PCBs; maximum 50 mg-PCB/kg-insulation oil). In order to remove the PCBs from transformer components using n-hexane as a solvent, we investigated the relationship between progressive stages of dismantling and cleaning results. The results are summarized as follows: (1) Based on the cleaning test results, we made an estimate of the residual PCB amount on iron and copper components. By dismantling the test pole transformers into the "iron core and coil portion" and cleaning the components, we achieved a residual PCB amount that was below the limit of detection (0.05 mg-PCB/kg-material). To achieve a residual PCB amount below the limit of detection for the transformer paper component, it was necessary to cut the paper into pieces smaller than 5 mm. We were unable to achieve a residual PCB amount below the limit of detection for the wood component. (2) Compared to Japan's stipulated limited concentration standard values for PCBs, the results of the cleaning test show that cleaning iron or copper components with PCBs only on their surface with the solvent n-hexane will satisfy the limited concentration standard values when care is taken to ensure the component surfaces have adequate contact with the cleaning solvent.

A comprehensive and scalable database search system for metaproteomics.

PubMed

Chatterjee, Sandip; Stupp, Gregory S; Park, Sung Kyu Robin; Ducom, Jean-Christophe; Yates, John R; Su, Andrew I; Wolan, Dennis W

2016-08-16

Mass spectrometry-based shotgun proteomics experiments rely on accurate matching of experimental spectra against a database of protein sequences. Existing computational analysis methods are limited in the size of their sequence databases, which severely restricts the proteomic sequencing depth and functional analysis of highly complex samples. The growing amount of public high-throughput sequencing data will only exacerbate this problem. We designed a broadly applicable metaproteomic analysis method (ComPIL) that addresses protein database size limitations. Our approach to overcome this significant limitation in metaproteomics was to design a scalable set of sequence databases assembled for optimal library querying speeds. ComPIL was integrated with a modified version of the search engine ProLuCID (termed "Blazmass") to permit rapid matching of experimental spectra. Proof-of-principle analysis of human HEK293 lysate with a ComPIL database derived from high-quality genomic libraries was able to detect nearly all of the same peptides as a search with a human database (~500x fewer peptides in the database), with a small reduction in sensitivity. We were also able to detect proteins from the adenovirus used to immortalize these cells. We applied our method to a set of healthy human gut microbiome proteomic samples and showed a substantial increase in the number of identified peptides and proteins compared to previous metaproteomic analyses, while retaining a high degree of protein identification accuracy and allowing for a more in-depth characterization of the functional landscape of the samples. The combination of ComPIL with Blazmass allows proteomic searches to be performed with database sizes much larger than previously possible. These large database searches can be applied to complex meta-samples with unknown composition or proteomic samples where unexpected proteins may be identified. The protein database, proteomic search engine, and the proteomic data files for the 5 microbiome samples characterized and discussed herein are open source and available for use and additional analysis.

Analysis of antibody aggregate content at extremely high concentrations using sedimentation velocity with a novel interference optics.

PubMed

Schilling, Kristian; Krause, Frank

2015-01-01

Monoclonal antibodies represent the most important group of protein-based biopharmaceuticals. During formulation, manufacturing, or storage, antibodies may suffer post-translational modifications altering their physical and chemical properties. Such induced conformational changes may lead to the formation of aggregates, which can not only reduce their efficiency but also be immunogenic. Therefore, it is essential to monitor the amount of size variants to ensure consistency and quality of pharmaceutical antibodies. In many cases, antibodies are formulated at very high concentrations > 50 g/L, mostly along with high amounts of sugar-based excipients. As a consequence, all routine aggregation analysis methods, such as size-exclusion chromatography, cannot monitor the size distribution at those original conditions, but only after dilution and usually under completely different solvent conditions. In contrast, sedimentation velocity (SV) allows to analyze samples directly in the product formulation, both with limited sample-matrix interactions and minimal dilution. One prerequisite for the analysis of highly concentrated samples is the detection of steep concentration gradients with sufficient resolution: Commercially available ultracentrifuges are not able to resolve such steep interference profiles. With the development of our Advanced Interference Detection Array (AIDA), it has become possible to register interferograms of solutions as highly concentrated as 150 g/L. The other major difficulty encountered at high protein concentrations is the pronounced non-ideal sedimentation behavior resulting from repulsive intermolecular interactions, for which a comprehensive theoretical modelling has not yet been achieved. Here, we report the first SV analysis of highly concentrated antibodies up to 147 g/L employing the unique AIDA ultracentrifuge. By developing a consistent experimental design and data fit approach, we were able to provide a reliable estimation of the minimum content of soluble aggregates in the original formulations of two antibodies. Limitations of the procedure are discussed.

Whole Genome Amplification and Reduced-Representation Genome Sequencing of Schistosoma japonicum Miracidia

PubMed Central

Shortt, Jonathan A.; Card, Daren C.; Schield, Drew R.; Liu, Yang; Zhong, Bo; Castoe, Todd A.

2017-01-01

Background In areas where schistosomiasis control programs have been implemented, morbidity and prevalence have been greatly reduced. However, to sustain these reductions and move towards interruption of transmission, new tools for disease surveillance are needed. Genomic methods have the potential to help trace the sources of new infections, and allow us to monitor drug resistance. Large-scale genotyping efforts for schistosome species have been hindered by cost, limited numbers of established target loci, and the small amount of DNA obtained from miracidia, the life stage most readily acquired from humans. Here, we present a method using next generation sequencing to provide high-resolution genomic data from S. japonicum for population-based studies. Methodology/Principal Findings We applied whole genome amplification followed by double digest restriction site associated DNA sequencing (ddRADseq) to individual S. japonicum miracidia preserved on Whatman FTA cards. We found that we could effectively and consistently survey hundreds of thousands of variants from 10,000 to 30,000 loci from archived miracidia as old as six years. An analysis of variation from eight miracidia obtained from three hosts in two villages in Sichuan showed clear population structuring by village and host even within this limited sample. Conclusions/Significance This high-resolution sequencing approach yields three orders of magnitude more information than microsatellite genotyping methods that have been employed over the last decade, creating the potential to answer detailed questions about the sources of human infections and to monitor drug resistance. Costs per sample range from $50-$200, depending on the amount of sequence information desired, and we expect these costs can be reduced further given continued reductions in sequencing costs, improvement of protocols, and parallelization. This approach provides new promise for using modern genome-scale sampling to S. japonicum surveillance, and could be applied to other schistosome species and other parasitic helminthes. PMID:28107347

New Measurements of the Particle Size Distribution of Apollo 11 Lunar Soil 10084

NASA Technical Reports Server (NTRS)

McKay, D.S.; Cooper, B.L.; Riofrio, L.M.

2009-01-01

We have initiated a major new program to determine the grain size distribution of nearly all lunar soils collected in the Apollo program. Following the return of Apollo soil and core samples, a number of investigators including our own group performed grain size distribution studies and published the results [1-11]. Nearly all of these studies were done by sieving the samples, usually with a working fluid such as Freon(TradeMark) or water. We have measured the particle size distribution of lunar soil 10084,2005 in water, using a Microtrac(TradeMark) laser diffraction instrument. Details of our own sieving technique and protocol (also used in [11]). are given in [4]. While sieving usually produces accurate and reproducible results, it has disadvantages. It is very labor intensive and requires hours to days to perform properly. Even using automated sieve shaking devices, four or five days may be needed to sieve each sample, although multiple sieve stacks increases productivity. Second, sieving is subject to loss of grains through handling and weighing operations, and these losses are concentrated in the finest grain sizes. Loss from handling becomes a more acute problem when smaller amounts of material are used. While we were able to quantitatively sieve into 6 or 8 size fractions using starting soil masses as low as 50mg, attrition and handling problems limit the practicality of sieving smaller amounts. Third, sieving below 10 or 20microns is not practical because of the problems of grain loss, and smaller grains sticking to coarser grains. Sieving is completely impractical below about 5- 10microns. Consequently, sieving gives no information on the size distribution below approx.10 microns which includes the important submicrometer and nanoparticle size ranges. Finally, sieving creates a limited number of size bins and may therefore miss fine structure of the distribution which would be revealed by other methods that produce many smaller size bins.

Ground cloud effluent measurements during the May 30, 1974, Titan 3 launch at the Air Force eastern test range

NASA Technical Reports Server (NTRS)

Bendura, R. J.; Crumbly, K. H.

1977-01-01

Surface-level exhaust effluent measurements of HCl, CO, and particulates, ground-cloud behavior, and some comparisons with model predictions for the launch of a Titan 3 rocket are presented along with a limited amount of airborne sampling measurements of other cloud species (O3, NO, NOX). Values above background levels for these effluents were obtained at 20 of the 30 instrument sites; these values were lower than model predictions and did not exceed public health standards. Cloud rise rate, stabilization altitude, and volume are compared with results from previous launches.

Molecular Typing of Lung Adenocarcinoma on Cytological Samples Using a Multigene Next Generation Sequencing Panel

PubMed Central

Fassan, Matteo; Rachiglio, Anna Maria; Cappellesso, Rocco; Antonello, Davide; Amato, Eliana; Mafficini, Andrea; Lambiase, Matilde; Esposito, Claudia; Bria, Emilio; Simonato, Francesca; Scardoni, Maria; Turri, Giona; Chilosi, Marco; Tortora, Giampaolo; Fassina, Ambrogio; Normanno, Nicola

2013-01-01

Identification of driver mutations in lung adenocarcinoma has led to development of targeted agents that are already approved for clinical use or are in clinical trials. Therefore, the number of biomarkers that will be needed to assess is expected to rapidly increase. This calls for the implementation of methods probing the mutational status of multiple genes for inoperable cases, for which limited cytological or bioptic material is available. Cytology specimens from 38 lung adenocarcinomas were subjected to the simultaneous assessment of 504 mutational hotspots of 22 lung cancer-associated genes using 10 nanograms of DNA and Ion Torrent PGM next-generation sequencing. Thirty-six cases were successfully sequenced (95%). In 24/36 cases (67%) at least one mutated gene was observed, including EGFR, KRAS, PIK3CA, BRAF, TP53, PTEN, MET, SMAD4, FGFR3, STK11, MAP2K1. EGFR and KRAS mutations, respectively found in 6/36 (16%) and 10/36 (28%) cases, were mutually exclusive. Nine samples (25%) showed concurrent alterations in different genes. The next-generation sequencing test used is superior to current standard methodologies, as it interrogates multiple genes and requires limited amounts of DNA. Its applicability to routine cytology samples might allow a significant increase in the fraction of lung cancer patients eligible for personalized therapy. PMID:24236184

Sensitive and affordable diagnostic assay for the quantitative detection of anaplastic lymphoma kinase (ALK) alterations in patients with non-small cell lung cancer

PubMed Central

Dama, Elisa; Tillhon, Micol; Bertalot, Giovanni; de Santis, Francesca; Troglio, Flavia; Pessina, Simona; Passaro, Antonio; Pece, Salvatore; de Marinis, Filippo; Dell'Orto, Patrizia; Viale, Giuseppe; Spaggiari, Lorenzo; Di Fiore, Pier Paolo; Bianchi, Fabrizio; Barberis, Massimo; Vecchi, Manuela

2016-01-01

Accurate detection of altered anaplastic lymphoma kinase (ALK) expression is critical for the selection of lung cancer patients eligible for ALK-targeted therapies. To overcome intrinsic limitations and discrepancies of currently available companion diagnostics for ALK, we developed a simple, affordable and objective PCR-based predictive model for the quantitative measurement of any ALK fusion as well as wild-type ALK upregulation. This method, optimized for low-quantity/−quality RNA from FFPE samples, combines cDNA pre-amplification with ad hoc generated calibration curves. All the models we derived yielded concordant predictions when applied to a cohort of 51 lung tumors, and correctly identified all 17 ALK FISH-positive and 33 of the 34 ALK FISH-negative samples. The one discrepant case was confirmed as positive by IHC, thus raising the accuracy of our test to 100%. Importantly, our method was accurate when using low amounts of input RNA (10 ng), also in FFPE samples with limited tumor cellularity (5–10%) and in FFPE cytology specimens. Thus, our test is an easily implementable diagnostic tool for the rapid, efficacious and cost-effective screening of ALK status in patients with lung cancer. PMID:27206799

Natural radioactivity in groundwater from the south-eastern Arabian Peninsula and environmental implications.

PubMed

Murad, A; Zhou, X D; Yi, P; Alshamsi, D; Aldahan, A; Hou, X L; Yu, Z B

2014-10-01

Groundwater is the most valuable resource in arid regions, and recognizing radiological criteria among other water quality parameters is essential for sustainable use. In the investigation presented here, gross-α and gross-β were measured in groundwater samples collected in the south-eastern Arabian Peninsula, 67 wells in Unite Arab Emirates (UAE), as well as two wells and one spring in Oman. The results show a wide gross-α and gross-β activities range in the groundwater samples that vary at 0.01∼19.5 Bq/l and 0.13∼6.6 Bq/l, respectively. The data show gross-β and gross-α values below the WHO permissible limits for drinking water in the majority of the investigated samples except those in region 4 (Jabel Hafit and surroundings). No correlation between groundwater pH and the gross-α and gross-β, while high temperatures probably enhance leaching of radionuclides from the aquifer body and thereby increase the radioactivity in the groundwater. This conclusion is also supported by the positive correlation between radioactivity and amount of total dissolved solid. Particular water purification technology and environmental impact assessments are essential for sustainable and secure use of the groundwater in regions that show radioactivity values far above the WHO permissible limit for drinking water.

Determination of scandium in acid mine drainage by ICP-OES with flow injection on-line preconcentration using oxidized multiwalled carbon nanotubes.

PubMed

Jerez, Javier; Isaguirre, Andrea C; Bazán, Cristian; Martinez, Luis D; Cerutti, Soledad

2014-06-01

An on-line scandium preconcentration and determination system implemented with inductively coupled plasma optical emission spectrometry associated with flow injection was studied. Trace amounts of scandium were preconcentrated by sorption on a minicolumn packed with oxidized multiwalled carbon nanotubes, at pH 1.5. The retained analyte was removed from the minicolumn with 30% (v/v) nitric acid. A total enrichment factor of 225-fold was obtained within a preconcentration time of 300 s (for a 25 mL sample volume). The overall time required for preconcentration and elution of 25 mL of sample was about 6 min; the throughput was about 10 samples per hour. The value of the detection limit was 4 ng L(-1) and the precision for 10 replicate determinations at 100 ng L(-1) Sc level was 5% relative standard deviation, calculated from the peak heights obtained. The calibration graph using the preconcentration system was linear with a correlation coefficient of 0.9996 at levels near the detection limits up to at least 10 mg L(-1). After optimization, the method was successfully applied to the determination of Sc in an acid drainage from an abandoned mine located in the province of San Luis, Argentina. Copyright © 2014 Elsevier B.V. All rights reserved.

Migration limits for children's toys are nothing to play with.

PubMed

Krätke, Renate; Beausoleil, Claire; Carroquino, Maria José; Duarte-Davidson, Raquel; Fernandes, Teresa; Schoeters, Greet

2016-10-01

The European Commission and its independent Scientific Committee on Health and Environmental Risks (SCHER) published their final Opinion on estimates of the amount of toy materials ingested by children. The SCHER was asked to review available data on the ingestion of the following three types of toy material by children, and evaluate whether the ingestion amounts which formed the basis for the migration limits of 19 elements in the Toy Safety Directive are still appropriate or whether they should be changed. In the final Opinion the SCHER considers the ingestion amounts mentioned above to be appropriate, and that these ingestion amounts should remain classified as daily amounts rather than weekly. Copyright © 2016 Elsevier Inc. All rights reserved.

High-throughput receptor-based assay for the detection of spirolides by chemiluminescence.

PubMed

Rodríguez, Laura P; Vilariño, Natalia; Molgó, Jordi; Aráoz, Rómulo; Botana, Luis M

2013-12-01

The spirolides are marine toxins that belong to a new class of macrocyclic imines produced by dinoflagellates. In this study a previously described solid-phase receptor-based assay for the detection of spirolides was optimized for high-throughput screening and prevalidated. This method is based on the competition between 13-desmethyl spirolide C and biotin-α-bungarotoxin immobilized on a streptavidin-coated surface, for binding to nicotinic acetylcholine receptors. In this inhibition assay the amount of nAChR bound to the well surface is quantified using a specific antibody, followed by a second anti-mouse IgG antibody labeled with horseradish peroxidase (HRP). The assay protocol was optimized for 384-well microplates, which allowed a reduction of the amount of reagents per sample and an increase of the number of samples per plate versus previously published receptor-based assays. The sensitivity of the assay for 13-desmethyl spirolide C ranged from 5 to 150 ng mL(-1). The performance of the assay in scallop extracts was adequate, with an estimated detection limit for 13-desmethyl spirolide C of 50 μg kg(-1) of shellfish meat. The recovery rate of 13-desmethyl spirolide C for spiked samples with this assay was 80% and the inter-assay coefficient of variation was 8%. This 384-well microplate, chemiluminescence method can be used as a high-throughput screening assay to detect 13-desmethyl spirolide C in shellfish meat in order to reduce the number of samples to be processed through bioassays or analytical methods. Copyright © 2013 Elsevier Ltd. All rights reserved.

Highly efficient and ultra-small volume separation by pressure-driven liquid chromatography in extended nanochannels.

PubMed

Ishibashi, Ryo; Mawatari, Kazuma; Kitamori, Takehiko

2012-04-23

The rapidly developing interest in nanofluidic analysis, which is used to examine liquids ranging in amounts from the attoliter to the femtoliter scale, correlates with the recent interest in decreased sample amounts, such as in the field of single-cell analysis. For general nanofluidic analysis, the fact that a pressure-driven flow does not limit the choice of solvents (aqueous or organic) is important. This study shows the first pressure-driven liquid chromatography technique that enables separation of atto- to femtoliter sample volumes, with a high separation efficiency within a few seconds. The apparent diffusion coefficient measurement of the unretentive sample suggests that there is no increase in the viscosity of toluene in the extended nanospace, unlike in aqueous solvents. Evaluation of the normal phase separation, therefore, should involve only the examination of the effect of the small size of the extended nanospace. Compared to a conventionally packed high-performance liquid chromatography column, the separation here results in a faster separation (4 s) by 2 orders of magnitude, a smaller injection volume (10(0) fL) by 9 orders, and a higher separation efficiency (440,000 plates/m) by 1 order. Moreover, the separation behavior agrees with the theory showing that this high efficiency was due to the small and controlled size of the separation channel, where the diffusion through the channel depth direction is fast enough to be neglected. Our chip-based platform should allow direct and real-time analysis or screening of ultralow volume of sample. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultra-high performance liquid chromatography with fluorescence detection following salting-out assisted liquid-liquid extraction for the analysis of benzimidazole residues in farm fish samples.

PubMed

Tejada-Casado, Carmen; Lara, Francisco J; García-Campaña, Ana M; Del Olmo-Iruela, Monsalud

2018-03-30

Ultra-high performance liquid chromatography (UHPLC) coupled with fluorescence detection (FL) has been proposed for the first time to determine thirteen benzimidazoles (BZs) in farmed fish samples. In order to optimize the chromatographic separation, parameters such as mobile phase composition and flow rate were carefully studied, establishing a gradient mode with a mobile phase consisted of water (solvent A) and acetonitrile (solvent B) at a flow rate of 0.4 mL/min. The separation was performed on a Zorbax Eclipse Plus RRHD C 18 column (50 × 2.1 mm, 1.8 μm), involving a total analysis time lower than 12 min. Salting-out assisted liquid-liquid extraction (SALLE) was applied as sample treatment to different types of farmed fish (trout, sea bream and sea bass). To obtain satisfactory extraction efficiencies for the studied analytes, several parameters affecting the SALLE procedure were optimized including the amount of sample, type and volume of the extraction solvent, and the nature and amount of the salt used. Characterization of the method in terms of performance characteristics was carried out, obtaining satisfactory results for the linearity (R 2  ≥ 0.997), repeatability (RSD ≤ 6.1%), reproducibility (RSD ≤ 10.8%) and recoveries (R ≥ 79%; RSD ≤ 7.8%). Detection limits between 0.04-29.9 μg kg -1 were obtained, demonstrating the applicability of this fast, simple and environmentally friendly method. Copyright © 2018 Elsevier B.V. All rights reserved.

7 CFR 3550.63 - Maximum loan amount.

Code of Federal Regulations, 2010 CFR

2010-01-01

... self-help housing will be calculated by adding the total of the market value of the lot (including... amount. Total secured indebtedness must not exceed the area loan limit or market value limitations... appraisal, tax monitoring fee, and the charge to establish an escrow account for taxes and insurance will...

7 CFR 3550.63 - Maximum loan amount.

Code of Federal Regulations, 2013 CFR

2013-01-01

... self-help housing will be calculated by adding the total of the market value of the lot (including... amount. Total secured indebtedness must not exceed the area loan limit or market value limitations... appraisal, tax monitoring fee, and the charge to establish an escrow account for taxes and insurance will...

7 CFR 3550.63 - Maximum loan amount.

Code of Federal Regulations, 2012 CFR

2012-01-01

... self-help housing will be calculated by adding the total of the market value of the lot (including... amount. Total secured indebtedness must not exceed the area loan limit or market value limitations... appraisal, tax monitoring fee, and the charge to establish an escrow account for taxes and insurance will...

7 CFR 3550.63 - Maximum loan amount.

Code of Federal Regulations, 2011 CFR

2011-01-01

... self-help housing will be calculated by adding the total of the market value of the lot (including... amount. Total secured indebtedness must not exceed the area loan limit or market value limitations... appraisal, tax monitoring fee, and the charge to establish an escrow account for taxes and insurance will...

7 CFR 3550.63 - Maximum loan amount.

Code of Federal Regulations, 2014 CFR

2014-01-01

... self-help housing will be calculated by adding the total of the market value of the lot (including... amount. Total secured indebtedness must not exceed the area loan limit or market value limitations... appraisal, tax monitoring fee, and the charge to establish an escrow account for taxes and insurance will...

42 CFR 409.61 - General limitations on amount of benefits.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 42 Public Health 2 2010-10-01 2010-10-01 false General limitations on amount of benefits. 409.61 Section 409.61 Public Health CENTERS FOR MEDICARE & MEDICAID SERVICES, DEPARTMENT OF HEALTH AND HUMAN SERVICES MEDICARE PROGRAM HOSPITAL INSURANCE BENEFITS Scope of Hospital Insurance Benefits § 409.61 General...

Production, Stocks and Characteristics of Wildfire Charcoal in Canadian Boreal Forests; a Preliminary Synthesis

NASA Astrophysics Data System (ADS)

Preston, C. M.; Simard, M.

2016-12-01

Crowning wildfires are a major driver of carbon stocks and ecosystem development in Canadian boreal forests, but there is insufficient information to incorporate pyrogenic carbon (PyC) into models and management strategies. Data comparison is challenging because of varied experimental design, and studies are often limited to forest floor; nonetheless we have attempted a synthesis limited to visually determined PyC, hereafter designated "charcoal". Sources include our study of amounts, depth distribution (forest floor plus variable amounts of upper mineral soil) and chemical properties of charcoal (>2 mm) from a fire chronosequence in the Abitibi region of Quebec (51 jack pine (Pinus banksiana) and black spruce (Picea mariana) sites, 24 to 2355 years since fire). Complete charcoal production of 7900 kg/ha (forest floor, down wood, standing stems) was determined from an experimental crownfire in jack pine near Fort Providence (NWT) in 2012. Published data were assembled mainly from boreal conifer studies, but using more disparate sources for production, plus laboratory charring studies. Typical findings include high spatial variability, with depth distributions often showing a maximum around the organic-mineral interface. Stocks varied widely (up to ca. 5500 kg/ha), with little initial discernable trend with time, but were much lower in the few older sites (>700y). Total C and N were widely scattered for younger samples, but older samples were mainly 500-600 g C/kg with C/N values around 100. Similarly, carbon-13 NMR spectra show wider variation in young samples, with the oldest samples being highly aromatic. These initial variations are consistent with field reports of highly variable temperatures and duration of charring and many laboratory studies. As a starting point, it may be possibly suggested that a boreal crowning wildfire might produce some 5000-10000 kg/ha of charred material of 550-650 g C/kg, with half to two-thirds on forest floor and down wood and most of the rest on standing stems. Our synthesis mainly highlights future research needs, including more measurements on stems and down wood and chemical analysis of the black carbon component of charcoal.

Improved method for analysis of RNA present in long-term preserved thyroid cancer tissue of atomic bomb survivors.

PubMed

Hamatani, Kiyohiro; Eguchi, Hidetaka; Mukai, Mayumi; Koyama, Kazuaki; Taga, Masataka; Ito, Reiko; Hayashi, Yuzo; Nakachi, Kei

2010-01-01

Since many thyroid cancer tissue samples from atomic bomb (A-bomb) survivors have been preserved for several decades as unbuffered formalin-fixed, paraffin-embedded specimens, molecular oncological analysis of such archival specimens is indispensable for clarifying the mechanisms of thyroid carcinogenesis in A-bomb survivors. Although RET gene rearrangements are the most important targets, it is a difficult task to examine all of the 13 known types of RET gene rearrangements with the use of the limited quantity of RNA that has been extracted from invaluable paraffin-embedded tissue specimens of A-bomb survivors. In this study, we established an improved 5' rapid amplification of cDNA ends (RACE) method using a small amount of RNA extracted from archival thyroid cancer tissue specimens. Three archival thyroid cancer tissue specimens from three different patients were used as in-house controls to determine the conditions for an improved switching mechanism at 5' end of RNA transcript (SMART) RACE method; one tissue specimen with RET/PTC1 rearrangement and one with RET/PTC3 rearrangement were used as positive samples. One other specimen, used as a negative sample, revealed no detectable expression of the RET gene tyrosine kinase domain. We established a 5' RACE method using an amount of RNA as small as 10 ng extracted from long-term preserved, unbuffered formalin-fixed, paraffin-embedded thyroid cancer tissue by application of SMART technology. This improved SMART RACE method not only identified common RET gene rearrangements, but also isolated a clone containing a 93-bp insert of rare RTE/PTC8 in RNA extracted from formalin-fixed, paraffin-embedded thyroid cancer specimens from one A-bomb survivor who had been exposed to a high radiation dose. In addition, in the papillary thyroid cancer of another high-dose A-bomb survivor, this method detected one novel type of RET gene rearrangement whose partner gene is acyl coenzyme A binding domain 5, located on chromosome 10p. We conclude that our improved SMART RACE method is expected to prove useful in molecular analyses using archival formalin-fixed, paraffin-embedded tissue samples of limited quantity.

The disappearance rate and risk assessment of thiacloprid residues in Asian pear using liquid chromatography confirmed with tandem mass spectrometry.

PubMed

Kabir, Md Humayun; Abd El-Aty, A M; Rahman, Md Musfiqur; Kim, Sung-Woo; Choi, Jeong-Heui; Lee, Young-Jun; Truong, Lieu T B; Lee, Kang-Bong; Kim, Mi-Ra; Shin, Ho-Chul; Shim, Jae-Han

2017-05-01

This study was undertaken to quantify the residue levels and propose the dissipation kinetics of thiacloprid formulated as suspension concentrate in field-incurred Asian pears grown under two different open-field conditions. Samples were extracted with 20% distilled water in acetonitrile; partitioned with brine water and dichloromethane; and purified with a Florisil solid phase extraction cartridge. The analyte was identified with an LC ultraviolet detector, and field-incurred samples were confirmed using LC-MS/MS. The calibration curve was linear over the range 0.05-5.0 mg/L with a satisfactory coefficient of determination (R 2  = 0.9994). The limits of detection and limits of quantification (LOQ) were 0.003 and 0.01 mg/kg, respectively. The recovery rate fortified to blank samples at LOQ, 10× LOQ, and the maximum residue limit (MRL) were between 73.7 and 86.2% with relative standard deviation ≤9.0%. The residual concentrations at both sites were considerably lower than the MRL (0.7 mg/kg) set by the Korean Ministry of Food Drug Safety, with biological half-lives of 5.0 and 7.4 days, for sites 1 and 2, respectively. From the pre-harvest residue limit curve, it was predicted that if the residues were <1.13 or 1.40 mg/kg 10 days before harvest, the residue level would be lower than the MRL during harvest. Risk assessment on day 0 showed an acceptable daily intake (%) of 13.0% and 11.0% for sites 1 and site 2, respectively, which indicates that the residual amounts are not hazardous to the Korean population. Copyright © 2016 John Wiley & Sons, Ltd.

Quantification of free formaldehyde in carrageenan and processed Eucheuma seaweed using high-performance liquid chromatography.

PubMed

Hornshøj, Bettina Høj; Kobbelgaard, Sara; Blakemore, William R; Stapelfeldt, Henrik; Bixler, Harris J; Klinger, Markus

2015-01-01

In 2010 the European Commission placed a limit on the amount of free formaldehyde in carrageenan and processed Eucheuma seaweed (PES) of 5 mg kg(-1). Formaldehyde is not used in carrageenan and PES processing and accordingly one would not expect free formaldehyde to be present in carrageenan and PES. However, surprisingly high levels up to 10 mg kg(-1) have been found using the generally accepted AOAC and Hach tests. These findings are, per proposed reaction pathways, likely due to the formation of formaldehyde when sulphated galactose, the backbone of carrageenan, is hydrolysed with the strong acid used in these conventional tests. In order to minimise the risk of false-positives, which may lead to regulatory non-compliance, a new high-performance liquid chromatography (HPLC) method has been developed. Initially, carrageenan or PES is extracted with 2-propanol and subsequently reacted with 2,4-dinitrophenylhydrazine (DNPH) to form the chromophore formaldehyde-DNPH, which is finally quantified by reversed-phase HPLC with ultraviolet light detection at 355 nm. This method has been found to have a limit of detection of 0.05 mg kg(-1) and a limit of quantification of 0.2 mg kg(-1). Recoveries from samples spiked with known quantities of formaldehyde were 95-107%. Using this more specific technique, 20 samples of carrageenan and PES were tested for formaldehyde. Only one sample had a detectable content of formaldehyde (0.40 mg kg(-1)), thus demonstrating that the formaldehyde content of commercial carrageenan and PES products are well below the European Commission maximum limit of 5 mg kg(-1).

Validity of the WISC-IV Spanish for a clinically referred sample of Hispanic children.

PubMed

San Miguel Montes, Liza E; Allen, Daniel N; Puente, Antonio E; Neblina, Cris

2010-06-01

The Wechsler Intelligence Scale for Children (WISC) is the most commonly used intelligence test for children. Five years ago, a Spanish version of the WISC-IV was published (WISC-IV Spanish; Wechsler, 2005), but a limited amount of published information is available regarding its utility when assessing clinical samples. The current study included 107 children who were Spanish speaking and of Puerto Rican descent that had been administered the WISC-IV Spanish. They were subdivided into a clinical sample of 35 children with diagnoses of various forms of brain dysfunction (primarily learning disability, attention-deficit/hyperactivity disorder, and epilepsy) and a comparison group made up of 72 normal children who were part of the WISC-IV Spanish version standardization sample. Comparisons between these groups and the standardization sample were performed for the WISC-IV Spanish index and subtest scores. Results indicated that the clinical sample performed worse than the comparison samples on the Working Memory and Processing Speed Indexes, although findings varied to some extent depending on whether the clinical group was compared with the normal comparison group or the standardization sample. These findings provide support for the criterion validity of the WISC-IV Spanish when it is used to assess a clinically referred sample with brain dysfunction.

Effects of fecal sampling on preanalytical and analytical phases in quantitative fecal immunochemical tests for hemoglobin.

PubMed

Rapi, Stefano; Berardi, Margherita; Cellai, Filippo; Ciattini, Samuele; Chelazzi, Laura; Ognibene, Agostino; Rubeca, Tiziana

2017-07-24

Information on preanalytical variability is mandatory to bring laboratories up to ISO 15189 requirements. Fecal sampling is greatly affected by lack of harmonization in laboratory medicine. The aims of this study were to obtain information on the devices used for fecal sampling and to explore the effect of different amounts of feces on the results from the fecal immunochemical test for hemoglobin (FIT-Hb). Four commercial sample collection devices for quantitative FIT-Hb measurements were investigated. The volume of interest (VOI) of the probes was measured from diameter and geometry. Quantitative measurements of the mass of feces were carried out by gravimetry. The effects of an increased amount of feces on the analytical environment were investigated measuring the Hb values with a single analytical method. VOI was 8.22, 7.1 and 9.44 mm3 for probes that collected a target of 10 mg of feces, and 3.08 mm3 for one probe that targeted 2 mg of feces. The ratio between recovered and target amounts of devices ranged from 56% to 121%. Different changes in the measured Hb values were observed, in adding increasing amounts of feces in commercial buffers. The amounts of collected materials are related to the design of probes. Three out 4 manufacturers declare the same target amount using different sampling volumes and obtaining different amounts of collected materials. The introduction of a standard probes to reduce preanalytical variability could be an useful step for fecal test harmonization and to fulfill the ISO 15189 requirements.

Ultrasensitive Ambient Mass Spectrometric Analysis with a Pin-to-Capillary Flowing Atmospheric-Pressure Afterglow Source

PubMed Central

Shelley, Jacob T.; Wiley, Joshua S.; Hieftje, Gary M.

2011-01-01

The advent of ambient desorption/ionization mass spectrometry has resulted in a strong interest in ionization sources that are capable of direct analyte sampling and ionization. One source that has enjoyed increasing interest is the Flowing Atmospheric-Pressure Afterglow (FAPA). FAPA has been proven capable of directly desorbing/ionizing samples in any phase (solid, liquid, or gas) and with impressive limits of detection (<100 fmol). The FAPA was also shown to be less affected by competitive-ionization matrix effects than other plasma-based sources. However, the original FAPA design exhibited substantial background levels, cluttered background spectra in the negative-ion mode, and significant oxidation of aromatic analytes, which ultimately compromised analyte identification and quantification. In the present study, a change in the FAPA configuration from a pin-to-plate to a pin-to-capillary geometry was found to vastly improve performance. Background signals in positive- and negative-ionization modes were reduced by 89% and 99%, respectively. Additionally, the capillary anode strongly reduced the amount of atomic oxygen that could cause oxidation of analytes. Temperatures of the gas stream that interacts with the sample, which heavily influences desorption capabilities, were compared between the two sources by means of IR thermography. The performance of the new FAPA configuration is evaluated through the determination of a variety of compounds in positive- and negative-ion mode, including agrochemicals and explosives. A detection limit of 4 amol was found for the direct determination of the agrochemical ametryn, and appears to be spectrometer-limited. The ability to quickly screen for analytes in bulk liquid samples with the pin-to-capillary FAPA is also shown. PMID:21627097

Ultrasensitive ambient mass spectrometric analysis with a pin-to-capillary flowing atmospheric-pressure afterglow source.

PubMed

Shelley, Jacob T; Wiley, Joshua S; Hieftje, Gary M

2011-07-15

The advent of ambient desorption/ionization mass spectrometry has resulted in a strong interest in ionization sources that are capable of direct analyte sampling and ionization. One source that has enjoyed increasing interest is the flowing atmospheric-pressure afterglow (FAPA). The FAPA has been proven capable of directly desorbing/ionizing samples in any phase (solid, liquid, or gas) and with impressive limits of detection (<100 fmol). The FAPA was also shown to be less affected by competitive-ionization matrix effects than other plasma-based sources. However, the original FAPA design exhibited substantial background levels, cluttered background spectra in the negative-ion mode, and significant oxidation of aromatic analytes, which ultimately compromised analyte identification and quantification. In the present study, a change in the FAPA configuration from a pin-to-plate to a pin-to-capillary geometry was found to vastly improve performance. Background signals in positive- and negative-ionization modes were reduced by 89% and 99%, respectively. Additionally, the capillary anode strongly reduced the amount of atomic oxygen that could cause oxidation of analytes. Temperatures of the gas stream that interacts with the sample, which heavily influences desorption capabilities, were compared between the two sources by means of IR thermography. The performance of the new FAPA configuration is evaluated through the determination of a variety of compounds in positive- and negative-ion mode, including agrochemicals and explosives. A detection limit of 4 amol was found for the direct determination of the agrochemical ametryn and appears to be spectrometer-limited. The ability to quickly screen for analytes in bulk liquid samples with the pin-to-capillary FAPA is also shown.

Determination of total concentration of chemically labeled metabolites as a means of metabolome sample normalization and sample loading optimization in mass spectrometry-based metabolomics.

PubMed

Wu, Yiman; Li, Liang

2012-12-18

For mass spectrometry (MS)-based metabolomics, it is important to use the same amount of starting materials from each sample to compare the metabolome changes in two or more comparative samples. Unfortunately, for biological samples, the total amount or concentration of metabolites is difficult to determine. In this work, we report a general approach of determining the total concentration of metabolites based on the use of chemical labeling to attach a UV absorbent to the metabolites to be analyzed, followed by rapid step-gradient liquid chromatography (LC) UV detection of the labeled metabolites. It is shown that quantification of the total labeled analytes in a biological sample facilitates the preparation of an appropriate amount of starting materials for MS analysis as well as the optimization of the sample loading amount to a mass spectrometer for achieving optimal detectability. As an example, dansylation chemistry was used to label the amine- and phenol-containing metabolites in human urine samples. LC-UV quantification of the labeled metabolites could be optimally performed at the detection wavelength of 338 nm. A calibration curve established from the analysis of a mixture of 17 labeled amino acid standards was found to have the same slope as that from the analysis of the labeled urinary metabolites, suggesting that the labeled amino acid standard calibration curve could be used to determine the total concentration of the labeled urinary metabolites. A workflow incorporating this LC-UV metabolite quantification strategy was then developed in which all individual urine samples were first labeled with (12)C-dansylation and the concentration of each sample was determined by LC-UV. The volumes of urine samples taken for producing the pooled urine standard were adjusted to ensure an equal amount of labeled urine metabolites from each sample was used for the pooling. The pooled urine standard was then labeled with (13)C-dansylation. Equal amounts of the (12)C-labeled individual sample and the (13)C-labeled pooled urine standard were mixed for LC-MS analysis. This way of concentration normalization among different samples with varying concentrations of total metabolites was found to be critical for generating reliable metabolome profiles for comparison.

Variability of pesticide residues in cauliflower units collected from a field trial and market places in Greece.

PubMed

Prodhan, M D H; Papadakis, Emmanouil-N; Papadopoulou-Mourkidou, Euphemia

2016-09-01

To estimate the variability of pesticide residue levels present in cauliflower units, a total of 142 samples were collected from a field trial of a cooperative farmer, and 120 samples were collected from different market places in Thessaloniki, Greece. The collected samples were extracted using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction technique, and the residues were determined by liquid chromatography-tandem mass spectrometry. The developed method was validated by evaluating the accuracy, precision, linearity, limit of detection (LOD), and limit of quantification (LOQ). The average recoveries for all the analytes, derived from the data of control samples fortified at 0.01, 0.05, 0.1, and 0.2 mg/kg, ranged from 74 to 110% with a relative standard deviation of ≤8%. The correlation coefficient (R(2)) was ≥0.997 for all the analytes using matrix-matched calibration standards. The LOD values ranged from 0.001 to 0.003 mg/kg, and the LOQ was determined at 0.01 mg/kg for all the sought analytes. The matrix effect was found to be at a considerable level, especially for cypermethrin and deltamethrin, amounting to +90% and +145%, respectively. For the field samples, the unit-to-unit variability factors (VFs) calculated for cypermethrin and deltamethrin were 2.38 and 2.32, respectively, while the average VF for the market basket samples was 5.11. In the market basket samples, residues of cypermethrin, deltamethrin, chlorpyrifos, and indoxacarb were found at levels ≥LOQ and their respective VFs were 7.12, 5.67, 5.28, and 2.40.

Non-linear mixing effects on mass-47 CO2 clumped isotope thermometry: Patterns and implications.

PubMed

Defliese, William F; Lohmann, Kyger C

2015-05-15

Mass-47 CO(2) clumped isotope thermometry requires relatively large (~20 mg) samples of carbonate minerals due to detection limits and shot noise in gas source isotope ratio mass spectrometry (IRMS). However, it is unreasonable to assume that natural geologic materials are homogenous on the scale required for sampling. We show that sample heterogeneities can cause offsets from equilibrium Δ(47) values that are controlled solely by end member mixing and are independent of equilibrium temperatures. A numerical model was built to simulate and quantify the effects of end member mixing on Δ(47). The model was run in multiple possible configurations to produce a dataset of mixing effects. We verified that the model accurately simulated real phenomena by comparing two artificial laboratory mixtures measured using IRMS to model output. Mixing effects were found to be dependent on end member isotopic composition in δ(13)C and δ(18)O values, and independent of end member Δ(47) values. Both positive and negative offsets from equilibrium Δ(47) can occur, and the sign is dependent on the interaction between end member isotopic compositions. The overall magnitude of mixing offsets is controlled by the amount of variability within a sample; the larger the disparity between end member compositions, the larger the mixing offset. Samples varying by less than 2 ‰ in both δ(13)C and δ(18)O values have mixing offsets below current IRMS detection limits. We recommend the use of isotopic subsampling for δ(13)C and δ(18)O values to determine sample heterogeneity, and to evaluate any potential mixing effects in samples suspected of being heterogonous. Copyright © 2015 John Wiley & Sons, Ltd.

Risk Assessment of Radiation Exposure using Molecular Biodosimetry

NASA Technical Reports Server (NTRS)

Elliott, Todd F.; George, K.; Hammond, D. K.; Cucinotta, F. A.

2007-01-01

Current cytogenetic biodosimetry methods would be difficult to adapt to spaceflight operations, because they require toxic chemicals and a substantial amount of time to perform. In addition, current biodosimetry techniques are limited to whole body doses over about 10cGy. Development of new techniques that assess radiation exposure response at the molecular level could overcome these limitations and have important implications in the advancement of biodosimetry. Recent technical advances include expression profiling at the transcript and protein level to assess multiple biomarkers of exposure, which may lead to the development of a radiation biomarker panel revealing possible fingerprints of individual radiation sensitivity. So far, many biomarkers of interest have been examined in their response to ionizing radiation, such as cytokines and members of the DNA repair pathway. New technology, such as the Luminex system can analyze many biomarkers simultaneously in one sample.

Method of quantitating dsDNA

DOEpatents

Stark, Peter C.; Kuske, Cheryl R.; Mullen, Kenneth I.

2002-01-01

A method for quantitating dsDNA in an aqueous sample solution containing an unknown amount of dsDNA. A first aqueous test solution containing a known amount of a fluorescent dye-dsDNA complex and at least one fluorescence-attenutating contaminant is prepared. The fluorescence intensity of the test solution is measured. The first test solution is diluted by a known amount to provide a second test solution having a known concentration of dsDNA. The fluorescence intensity of the second test solution is measured. Additional diluted test solutions are similarly prepared until a sufficiently dilute test solution having a known amount of dsDNA is prepared that has a fluorescence intensity that is not attenuated upon further dilution. The value of the maximum absorbance of this solution between 200-900 nanometers (nm), referred to herein as the threshold absorbance, is measured. A sample solution having an unknown amount of dsDNA and an absorbance identical to that of the sufficiently dilute test solution at the same chosen wavelength is prepared. Dye is then added to the sample solution to form the fluorescent dye-dsDNA-complex, after which the fluorescence intensity of the sample solution is measured and the quantity of dsDNA in the sample solution is determined. Once the threshold absorbance of a sample solution obtained from a particular environment has been determined, any similarly prepared sample solution taken from a similar environment and having the same value for the threshold absorbance can be quantified for dsDNA by adding a large excess of dye to the sample solution and measuring its fluorescence intensity.

High-speed imaging using CMOS image sensor with quasi pixel-wise exposure

NASA Astrophysics Data System (ADS)

Sonoda, T.; Nagahara, H.; Endo, K.; Sugiyama, Y.; Taniguchi, R.

2017-02-01

Several recent studies in compressive video sensing have realized scene capture beyond the fundamental trade-off limit between spatial resolution and temporal resolution using random space-time sampling. However, most of these studies showed results for higher frame rate video that were produced by simulation experiments or using an optically simulated random sampling camera, because there are currently no commercially available image sensors with random exposure or sampling capabilities. We fabricated a prototype complementary metal oxide semiconductor (CMOS) image sensor with quasi pixel-wise exposure timing that can realize nonuniform space-time sampling. The prototype sensor can reset exposures independently by columns and fix these amount of exposure by rows for each 8x8 pixel block. This CMOS sensor is not fully controllable via the pixels, and has line-dependent controls, but it offers flexibility when compared with regular CMOS or charge-coupled device sensors with global or rolling shutters. We propose a method to realize pseudo-random sampling for high-speed video acquisition that uses the flexibility of the CMOS sensor. We reconstruct the high-speed video sequence from the images produced by pseudo-random sampling using an over-complete dictionary.

Schnellverfahren zur flammenlosen AAS-Bestimmung von Spurenelementen in geologischen Proben

NASA Astrophysics Data System (ADS)

Schrön, W.; Bombach, G.; Beuge, P.

This paper reports experience with direct quantitative trace element determinations in powdered geological samples by nameless atomic absorption spectroscopy. Two methods were explored. The first one is based on the production of a sample aerosol by laser radiation in a specifically designed sample chamber and the subsequent transport of the aerosol into a graphite tube, which has been preheated to a stable temperature. This technique is suited for a large range of concentration and is relatively free from matrix interferences. The technique was tested for the elements Ag, As, Bi, Cd, Co, Mn, Ni, Pb, Sb, Se, Sr and Tl. The described sample chamber can be also used in combination with other spcctroscopic techniques. The second method explored permits the quantitative determination of trace elements at very low concentrations. Essentially an accurately weighed amount of sample is placed on a graphite rod and introduced into a graphite furnace by inserting the rod through the sample injection port. Atomization takes place also under stable temperature conditions. Using this technique detection limits were found to be 10 -11 g for Ag, 2 × 10 -11 g for Cd and 10 -10 g for Sb in silicate materials.

Local anesthesia for abdominoplasty, liposuction, and combined operations.

PubMed

Mottura, A A

1993-01-01

This article describes a procedure to perform abdominoplasty, liposuction, and combined operations under local anesthesia. With an anesthetic solution composed of 25 cc of 2% lidocaine, 25 cc of 0.5% bupivacaine, 1 cc of epinephrine or ornipresine, and 350 cc of saline solution, a satisfactory dilution with low concentration and lasting effects was obtained. After infiltration a large amount was lost in the incision, the dissection, and the resected dermofatty tissue. A small amount of anesthetic remained in the operated area to be metabolized by the liver. Low lidocaine levels were found in venous blood samples during surgery. This type of anesthesia is advised in minor, limited, and normal abdominoplasties in normal-sized patients, or major abdominoplasties in small patients. In liposuction procedures, it is possible to anesthetize the patient using the same procedure and operate in an equivalent area. As a high proportion of the infiltrated anesthesia was lost during the operation, a similar amount could be used to infiltrate and operate other areas so that an abdominoplasty might be combined with liposuction or mastoplasty. We have experience with 25 abdominoplasties and 21 liposuctions performed under local anesthesia. There were no complications related to local anesthesia and no one had unpleasant memories of intraoperative events.

Library Construction from Subnanogram DNA for Pelagic Sea Water and Deep-Sea Sediments

PubMed Central

Hirai, Miho; Nishi, Shinro; Tsuda, Miwako; Sunamura, Michinari; Takaki, Yoshihiro; Nunoura, Takuro

2017-01-01

Shotgun metagenomics is a low biased technology for assessing environmental microbial diversity and function. However, the requirement for a sufficient amount of DNA and the contamination of inhibitors in environmental DNA leads to difficulties in constructing a shotgun metagenomic library. We herein examined metagenomic library construction from subnanogram amounts of input environmental DNA from subarctic surface water and deep-sea sediments using two library construction kits: the KAPA Hyper Prep Kit and Nextera XT DNA Library Preparation Kit, with several modifications. The influence of chemical contaminants associated with these environmental DNA samples on library construction was also investigated. Overall, shotgun metagenomic libraries were constructed from 1 pg to 1 ng of input DNA using both kits without harsh library microbial contamination. However, the libraries constructed from 1 pg of input DNA exhibited larger biases in GC contents, k-mers, or small subunit (SSU) rRNA gene compositions than those constructed from 10 pg to 1 ng DNA. The lower limit of input DNA for low biased library construction in this study was 10 pg. Moreover, we revealed that technology-dependent biases (physical fragmentation and linker ligation vs. tagmentation) were larger than those due to the amount of input DNA. PMID:29187708

Tocopherol content and Fatty Acid profile of different Iranian date seed oils.

PubMed

Biglar, Mahmood; Khanavi, Mahnaz; Hajimahmoodi, Mannan; Hassani, Shokufeh; Moghaddam, Ghazaleh; Sadeghi, Naficeh; Oveisi, Mohammad Reza

2012-01-01

Date is one of the world's oldest food-producing plants wich has always played an important role in the economy and social life. Various researchers examined chemical composition and nutritional values of edible parts of dates while limited information about chemical composition and nutritional quality of date seed is available. In this study, fatty acid composition and total tocopherol content of 14 Iranian date seed oils were studied. Statistical analysis was performed through SPSS computing package. According to the fatty acid profiles, seven fatty acids were found through nearly 50% oleic acid in seeds. Shekar cultivar by 51.40% had the maximum amount and Lasht cultivar by 33.38% had the minimum amount of oleic acid. Tocopherol content in the samples varied between 33.86 μg vit E/g oil for Shahabi2 to 10.09 μg vit E/g oil for Shekar. Tocopherol content was 1.88 and 0.61 μg respectively in one-gram seed of these two cultivars. Iranian date seed oils classified as oleic-lauric oil, had a high amount of oleic acid and could serve as a profitable source of valuable oils for industrial applications.

Graphene oxide: an adsorbent for the extraction and quantification of aflatoxins in peanuts by high-performance liquid chromatography.

PubMed

Yu, Li; Li, Peiwu; Zhang, Qi; Zhang, Wen; Ding, Xiaoxia; Wang, Xiupin

2013-11-29

In this paper, graphene oxide (GO) was synthesized and specifically selected by centrifugation to extract four aflatoxins (B1, B2, G1, and G2) as an effective adsorbent. Then, the amount of aflatoxins was quantitatively measured by high-performance liquid chromatography (HPLC). The GO was characterized by X-ray diffraction (XRD), atomic force microscopy (AFM), and ultraviolet (UV) spectrophotometer. Several parameters that could affect the extraction efficiency, including the GO amount, methanol concentration in the extraction solvent, spiked amount, extraction time, and elution cycle, were also investigated and optimized in this work. Under optimal conditions, good linear relationships were achieved with the correlation coefficient (r) ranging from 0.99217 to 0.99995. The detection limit of this method for the four aflatoxins ranged from 0.08 to 0.65ng/g. Finally, the proposed method has been successfully applied to determine aflatoxins in peanut samples. The results show that the recoveries of the four aflatoxins range from 85.1% to 100.8% with the relative standard deviations between 2.1% and 7.9%. Copyright © 2013 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.

Amount of Genetics Education is Low Among Didactic Programs in Dietetics.

PubMed

Beretich, Kaitlan; Pope, Janet; Erickson, Dawn; Kennedy, Angela

2017-01-01

Nutritional genomics is a growing area of research. Research has shown registered dietitian nutritionists (RDNs) have limited knowledge of genetics. Limited research is available regarding how didactic programs in dietetics (DPDs) meet the genetics knowledge requirement of the Accreditation Council for Education in Nutrition and Dietetics (ACEND®). The purpose of this study was to determine the extent to which the study of nutritional genomics is incorporated into undergraduate DPDs in response to the Academy of Nutrition and Dietetics position statement on nutritional genomics. The sample included 62 DPD directors in the U.S. Most programs (63.9%) reported the ACEND genetics knowledge requirement was being met by integrating genetic information into the current curriculum. However, 88.7% of programs reported devoting only 1-10 clock hours to genetics education. While 60.3% of directors surveyed reported they were confident in their program's ability to teach information related to genetics, only 6 directors reported having specialized training in genetics. The overall amount of clock hours devoted to genetics education is low. DPD directors, faculty, and instructors are not adequately trained to provide this education to students enrolled in DPDs. Therefore, the primary recommendation of this study is the development of a standardized curriculum for genetics education in DPDs.

Testing the Effectiveness of an International Conservation Agreement: Marketplace Forensics and CITES Caviar Trade Regulation

PubMed Central

Doukakis, Phaedra; Pikitch, Ellen K.; Rothschild, Anna; DeSalle, Rob; Amato, George; Kolokotronis, Sergios-Orestis

2012-01-01

Background The international wildlife trade is a key threat to biodiversity. Temporal genetic marketplace monitoring can determine if wildlife trade regulation efforts such as the Convention on International Trade in Endangered Species (CITES) are succeeding. Protected under CITES effective 1997, sturgeons and paddlefishes, the producers of black caviar, are flagship CITES species. Methodology/Principal Findings We test whether CITES has limited the amount of fraudulent black caviar reaching the marketplace. Using mitochondrial DNA-based methods, we compare mislabeling in caviar and meat purchased in the New York City area pre and post CITES listing. Our recent sampling of this market reveals a decrease in mislabeled caviar (2006–2008; 10%; n = 90) compared to pre-CITES implementation (1995–1996; 19%; n = 95). Mislabeled caviar was found only in online purchase (n = 49 online/41 retail). Conclusions/Significance Stricter controls on importing and exporting as per CITES policies may be having a positive conservation effect by limiting the amount of fraudulent caviar reaching the marketplace. Sturgeons and paddlefishes remain a conservation priority, however, due to continued overfishing and habitat degradation. Other marine and aquatic species stand to benefit from the international trade regulation that can result from CITES listing. PMID:22848410

Education and job-based interventions for unmarried couples living with low incomes: Benefit or burden?

PubMed

Williamson, Hannah C; Karney, Benjamin R; Bradbury, Thomas N

2017-01-01

Government initiatives undertaken to improve the earning potential of disadvantaged unmarried parents assume that job training and additional schooling will strengthen these families, yet alternative models predict that these same interventions could overwhelm couples' limited resources, undermining family stability. We use 3 waves of dyadic data and propensity score analysis to test these competing perspectives by examining the effects of job-related and school-related interventions on 3-year marriage rates. The sample consists of unmarried new parents averaging $20,475 in household income, 52% of whom are African American and 20% of whom are Hispanic/Latino. Marriage rates decreased, from 17% to 10%, for couples in which men participated in school-related interventions. Mediation analyses indicate that school-related interventions reduce the amount of time men spend with their child and the amount of money they contribute to their household, reducing marriage rates in turn. Marriage rates were unaffected by women's participation in school-related interventions, and by men's and women's participation in job-related interventions. Implementing economic interventions that increase income while minimizing demands on the limited resources of economically distressed couples may prove necessary for strengthening society's most vulnerable families. (PsycINFO Database Record (c) 2017 APA, all rights reserved).

Experimental investigation to evaluate the potential environmental hazards of photovoltaic panels.

PubMed

Tammaro, Marco; Salluzzo, Antonio; Rimauro, Juri; Schiavo, Simona; Manzo, Sonia

2016-04-05

Recently the potential environmental hazard of photovoltaic modules together with their management as waste has attracted the attention of scientists. Particular concern is aroused by the several metals contained in photovoltaic panels whose potential release in the environment were scarcely investigated. Here, for the first time, the potential environmental hazard of panels produced in the last 30 years was investigated through the assessment of up to 18 releasable metals. Besides, the corresponding ecotoxicological effects were also evaluated. Experimental data were compared with the current European and Italian law limits for drinking water, discharge on soil and landfill inert disposal in order to understand the actual pollution load. Results showed that less than 3% of the samples respected all law limits and around 21% was not ecotoxic. By considering the technological evolutions in manufacturing, we have shown that during the years crystalline silicon panels have lower tendency to release hazardous metals with respect to thin film panels. In addition, a prediction of the amounts of lead, chromium, cadmium and nickel releasable from next photovoltaic waste was performed. The prevision up to 2050 showed high amounts of lead (30t) and cadmium (2.9t) releasable from crystalline and thin film panels respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

Prevention of clogging in a biological trickle-bed reactor removing toluene from contaminated air.

PubMed

Weber, F J; Hartmans, S

1996-04-05

Removal of organic compounds like toluene from waste gases with a trickle-bed reactor can result in clogging of the reactor due to the formation of an excessive amount of biomass. We therefore limited the amount of nutrients available for growth, to prevent clogging of the reactor. As a consequence of this nutrient limitation a lower removal rate was observed. However, when a fungal culture was used to inoculate the reactor, the toluene removal rate under nutrient limiting conditions was higher. Over a period of 375 days, an average removal rate of 27 g C/(m(3) h) was obtained with the reactor inoculated with the fungal culture. From the carbon balance over the reactor and the nitrogen availability it was concluded that, under these nutrient-limited conditions, large amounts of carbohydrates are probably formed. We also studied the application of a NaOH wash to remove excess biomass, as a method to prevent clogging. Under these conditions an average toluene removal rate of 35 g C/(m(3) h) was obtained. After about 50 days there was no net increase in the biomass content of the reactor. The amount of biomass which was formed in the reactor equaled the amount removed by the NaOH wash.

Minor-element composition and organic carbon content of marine and nonmarine shales of Late Cretaceous age in the western interior of the United States

USGS Publications Warehouse

Tourtelot, H.A.

1964-01-01

The composition of nonmarine shales of Cretaceous age that contain less than 1 per cent organic carbon is assumed to represent the inherited minor-element composition of clayey sediments delivered to the Cretaceous sea that occupied the western interior region of North America. Differences in minor-element content between these samples and samples of 1. (a) nonmarine carbonaceous shales (1 to 17 per cent organic carbon), 2. (b) nearshore marine shales (less than 1 per cent organic carbon), and 3. (c) offshore marine shales (as much as 8 per cent organic carbon), all of the same age, reveal certain aspects of the role played by clay minerals and organic materials in affecting the minor-element composition of the rocks. The organic carbon in the nonmarine rocks occurs in disseminated coaly plant remains. The organic carbon in the marine rocks occurs predominantly in humic material derived from terrestrial plants. The close similarity in composition between the organic isolates from the marine samples and low-rank coal suggests that the amount of marine organic material in these rocks is small. The minor-element content of the two kinds of nonmarine shales is the same despite the relatively large amount of organic carbon in the carbonaceous shales. The nearshore marine shales, however, contain larger median amounts of arsenic, boron, chromium, vanadium and zinc than do the nonmarine rocks; and the offshore marine shales contain even larger amounts of these elements. Cobalt, molybdenum, lead and zirconium show insignificant differences in median content between the nonmarine and marine rocks, although as much as 25 ppm molybdenum is present in some offshore marine samples. The gallium content is lower in the marine than in the nonmarine samples. Copper and selenium contents of the two kinds of nonmarine rocks and the nearshore marine samples are the same, but those of the offshore samples are larger. In general, arsenic, chromium, copper, molybdenum, selenium, vanadium and zinc are concentrated in those offshore marine samples having the largest amounts of organic carbon, but samples with equal amounts of vanadium, for instance, may differ by a factor of 3 in their amount of organic carbon. Arsenic and molybdenum occur in some samples chiefly in syngenetic pyrite but also are present in relatively large amounts in samples that contain little pyrite. The data on nonmarine carbonaceous shales indicate that organic matter of terrestrial origin in marine shales contributes little to the minor-element content of such rocks. It is possible that marine organic matter, even though seemingly small in amount in marine shales, contributes to the minor-element composition of the shales. In addition to any such contribution, however, the great effectiveness in sorption processes of humic materials in conjunction with clay minerals suggests that such processes must have played an important role as these materials moved from the relatively dilute solutions of the nonmarine environment to the relatively concentrated solution of sea water. The volumes of sea water sufficient to supply for sorption the amounts of most minor elements in the offshore marine samples are insignificant compared to the volumes of water with which the clay and organic matter were in contact during their transportation and sedimentation. Consequently, the chemical characteristics of the environment in which the clay minerals and organic matter accumulated and underwent diagenesis probably were the most important factors in controlling the degree to which sorption processes and the formation of syngenetic minerals affected the final composition of the rocks. ?? 1969.

31 CFR 360.10 - Amounts which may be purchased.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 31 Money and Finance:Treasury 2 2011-07-01 2011-07-01 false Amounts which may be purchased. 360.10 Section 360.10 Money and Finance: Treasury Regulations Relating to Money and Finance (Continued) FISCAL... follows: (a) General annual limitation, $5,000 (par value). (b) Special limitation, $4,000 (par value...

31 CFR 360.10 - Amounts which may be purchased.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 31 Money and Finance:Treasury 2 2012-07-01 2012-07-01 false Amounts which may be purchased. 360.10 Section 360.10 Money and Finance: Treasury Regulations Relating to Money and Finance (Continued) FISCAL... follows: (a) General annual limitation, $5,000 (par value). (b) Special limitation, $4,000 (par value...

10 CFR 605.14 - Limitation of DOE liability.

Code of Federal Regulations, 2012 CFR

2012-01-01

... PROGRAM § 605.14 Limitation of DOE liability. Awards under this part are subject to the requirement that the maximum DOE obligation to the recipient is the amount shown in the Notice of Financial Assistance Award as the amount of DOE funds obligated. DOE shall not be obligated to make any additional...

10 CFR 605.14 - Limitation of DOE liability.

Code of Federal Regulations, 2011 CFR

2011-01-01

... PROGRAM § 605.14 Limitation of DOE liability. Awards under this part are subject to the requirement that the maximum DOE obligation to the recipient is the amount shown in the Notice of Financial Assistance Award as the amount of DOE funds obligated. DOE shall not be obligated to make any additional...

10 CFR 605.14 - Limitation of DOE liability.

Code of Federal Regulations, 2010 CFR

2010-01-01

... PROGRAM § 605.14 Limitation of DOE liability. Awards under this part are subject to the requirement that the maximum DOE obligation to the recipient is the amount shown in the Notice of Financial Assistance Award as the amount of DOE funds obligated. DOE shall not be obligated to make any additional...

10 CFR 602.13 - Limitation of DOE liability.

Code of Federal Regulations, 2014 CFR

2014-01-01

... ASSISTANCE PROGRAM § 602.13 Limitation of DOE liability. Awards made under this part are subject to the requirement that the maximum DOE obligation to the recipient is the amount shown in the Notice of Financial Assistance Award as the amount of DOE funds obligated. DOE shall not be obligated to make any additional...

10 CFR 602.13 - Limitation of DOE liability.

Code of Federal Regulations, 2010 CFR

2010-01-01

... ASSISTANCE PROGRAM § 602.13 Limitation of DOE liability. Awards made under this part are subject to the requirement that the maximum DOE obligation to the recipient is the amount shown in the Notice of Financial Assistance Award as the amount of DOE funds obligated. DOE shall not be obligated to make any additional...

10 CFR 602.13 - Limitation of DOE liability.

Code of Federal Regulations, 2013 CFR

2013-01-01

... ASSISTANCE PROGRAM § 602.13 Limitation of DOE liability. Awards made under this part are subject to the requirement that the maximum DOE obligation to the recipient is the amount shown in the Notice of Financial Assistance Award as the amount of DOE funds obligated. DOE shall not be obligated to make any additional...

10 CFR 605.14 - Limitation of DOE liability.

Code of Federal Regulations, 2013 CFR

2013-01-01

... PROGRAM § 605.14 Limitation of DOE liability. Awards under this part are subject to the requirement that the maximum DOE obligation to the recipient is the amount shown in the Notice of Financial Assistance Award as the amount of DOE funds obligated. DOE shall not be obligated to make any additional...

10 CFR 602.13 - Limitation of DOE liability.

Code of Federal Regulations, 2012 CFR

2012-01-01

... ASSISTANCE PROGRAM § 602.13 Limitation of DOE liability. Awards made under this part are subject to the requirement that the maximum DOE obligation to the recipient is the amount shown in the Notice of Financial Assistance Award as the amount of DOE funds obligated. DOE shall not be obligated to make any additional...

10 CFR 605.14 - Limitation of DOE liability.

Code of Federal Regulations, 2014 CFR

2014-01-01

... PROGRAM § 605.14 Limitation of DOE liability. Awards under this part are subject to the requirement that the maximum DOE obligation to the recipient is the amount shown in the Notice of Financial Assistance Award as the amount of DOE funds obligated. DOE shall not be obligated to make any additional...

10 CFR 602.13 - Limitation of DOE liability.

Code of Federal Regulations, 2011 CFR

2011-01-01

... ASSISTANCE PROGRAM § 602.13 Limitation of DOE liability. Awards made under this part are subject to the requirement that the maximum DOE obligation to the recipient is the amount shown in the Notice of Financial Assistance Award as the amount of DOE funds obligated. DOE shall not be obligated to make any additional...

42 CFR 57.1508 - Amount of interest subsidy payments; limitations.

Code of Federal Regulations, 2010 CFR

2010-10-01

... payments will be made, and the level of such payments shall be determined by the Secretary on the basis of... consideration his analysis of the present and reasonable projected future financial ability of the applicant to... Profession Personnel § 57.1508 Amount of interest subsidy payments; limitations. The length of time for which...

42 CFR 423.336 - Risk-sharing arrangements.

Code of Federal Regulations, 2012 CFR

2012-10-01

... payments to a Part D sponsor subject to risk—(1) Adjusted allowable risk corridor costs. For purposes of... equal to— (1) The target amount for the plan; minus (2) An amount equal to the first threshold risk.... (B) Second threshold lower limit. The second threshold lower limit of the corridor is equal to— (1...

42 CFR 423.336 - Risk-sharing arrangements.

Code of Federal Regulations, 2013 CFR

2013-10-01

... payments to a Part D sponsor subject to risk—(1) Adjusted allowable risk corridor costs. For purposes of... equal to— (1) The target amount for the plan; minus (2) An amount equal to the first threshold risk.... (B) Second threshold lower limit. The second threshold lower limit of the corridor is equal to— (1...

42 CFR 423.336 - Risk-sharing arrangements.

Code of Federal Regulations, 2011 CFR

2011-10-01

... payments to a Part D sponsor subject to risk—(1) Adjusted allowable risk corridor costs. For purposes of... equal to— (1) The target amount for the plan; minus (2) An amount equal to the first threshold risk.... (B) Second threshold lower limit. The second threshold lower limit of the corridor is equal to— (1...

44 CFR 63.8 - Limitation on amount of benefits.

Code of Federal Regulations, 2013 CFR

2013-10-01

..., DEPARTMENT OF HOMELAND SECURITY INSURANCE AND HAZARD MITIGATION National Flood Insurance Program IMPLEMENTATION OF SECTION 1306(c) OF THE NATIONAL FLOOD INSURANCE ACT OF 1968 General § 63.8 Limitation on amount of benefits. (a) In section 1306(c)(3)(C) of the Act, the phrase under the flood insurance contract...

44 CFR 63.8 - Limitation on amount of benefits.

Code of Federal Regulations, 2014 CFR

2014-10-01

..., DEPARTMENT OF HOMELAND SECURITY INSURANCE AND HAZARD MITIGATION National Flood Insurance Program IMPLEMENTATION OF SECTION 1306(c) OF THE NATIONAL FLOOD INSURANCE ACT OF 1968 General § 63.8 Limitation on amount of benefits. (a) In section 1306(c)(3)(C) of the Act, the phrase under the flood insurance contract...

44 CFR 63.8 - Limitation on amount of benefits.

Code of Federal Regulations, 2010 CFR

2010-10-01

..., DEPARTMENT OF HOMELAND SECURITY INSURANCE AND HAZARD MITIGATION National Flood Insurance Program IMPLEMENTATION OF SECTION 1306(c) OF THE NATIONAL FLOOD INSURANCE ACT OF 1968 General § 63.8 Limitation on amount of benefits. (a) In section 1306(c)(3)(C) of the Act, the phrase under the flood insurance contract...

44 CFR 63.8 - Limitation on amount of benefits.

Code of Federal Regulations, 2011 CFR

2011-10-01

..., DEPARTMENT OF HOMELAND SECURITY INSURANCE AND HAZARD MITIGATION National Flood Insurance Program IMPLEMENTATION OF SECTION 1306(c) OF THE NATIONAL FLOOD INSURANCE ACT OF 1968 General § 63.8 Limitation on amount of benefits. (a) In section 1306(c)(3)(C) of the Act, the phrase under the flood insurance contract...

44 CFR 63.8 - Limitation on amount of benefits.

Code of Federal Regulations, 2012 CFR

2012-10-01

..., DEPARTMENT OF HOMELAND SECURITY INSURANCE AND HAZARD MITIGATION National Flood Insurance Program IMPLEMENTATION OF SECTION 1306(c) OF THE NATIONAL FLOOD INSURANCE ACT OF 1968 General § 63.8 Limitation on amount of benefits. (a) In section 1306(c)(3)(C) of the Act, the phrase under the flood insurance contract...

Medicare program; Medicare hospital reimbursement reforms: limitations on reimbursable costs and the rate of hospital cost increases--HCFA. Interim final rule with comment period.

PubMed

1982-09-30

These rules implement section 1886 of the Social Security Act (established by section 101 of the Tax Equity and Fiscal Responsibility Act of 1982). These rules amend current regulations on hospital cost limits, providing for new exemptions and exceptions. These amendments make exceptions available to hospitals consistent with the new cost limits published elsewhere in this issue of the Federal Register, and specifically exempt from those cost limits rural hospitals with less than 50 beds in existence as of the enactment of the law. These rules also set forth new regulations establishing a three-year ceiling on the allowable annual rate of increase in operating costs per case for inpatient hospital services. This ceiling takes the form of a target amount of cost per case against which a hospital's incurred cost per case will be compared. Hospitals are provided incentives to keep their cost increases below the target rate. A hospital that has costs per case less than the target amount will be paid a portion of the difference between actual cost and the target amount. A hospital that has costs per case that are greater than the target amount will be paid the target amount plus 25 percent of its costs in excess of the target for the first two years of the ceiling, and none of the excess in the third year. However, payment to a hospital under these new target rate regulations will not be greater than the amount determined under the new schedule of limits on hospital inpatient operating costs published elsewhere in this issue of the Federal Register.

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.

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

PubMed

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

2012-07-06

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

Sensitive determination of polycyclic aromatic hydrocarbons in water samples by HPLC coupled with SPE based on graphene functionalized with triethoxysilane.

PubMed

Huang, Ke-Jing; Li, Jing; Liu, Yan-Ming; Wang, Lan

2013-02-01

The graphene functionalized with (3-aminopropyl) triethoxysilane was synthesized by a simple hydrothermal reaction and applied as SPE sorbents to extract trace polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. These sorbents possess high adsorption capacity and extraction efficiency due to strong adsorption ability of carbon materials and large specific surface area of nanoparticles, and only 10 mg of sorbents are required to extract PAHs from 100 mL water samples. Several condition parameters, such as eluent and its volume, adsorbent amount, sample volume, sample pH, and sample flow rate, were optimized to achieve good sensitivity and precision. Under the optimized extraction conditions, the method showed good linearity in the range of 1-100 μg/L, repeatability of the extraction (the RSDs were between 1.8 and 2.9%, n = 6), and satisfactory detection limits of 0.029-0.1 μg/L. The recoveries of PAHs spiked in environmental water samples ranged from 84.6 to 109.5%. All these results demonstrated that this new SPE technique was a viable alternative to conventional enrichment techniques for the extraction and analysis of PAHs in complex samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Application of solvent floatation to separation and determination of triazine herbicides in honey by high-performance liquid chromatography.

PubMed

Wang, Kun; Jiang, Jia; Lv, Xinping; Zang, Shuang; Tian, Sizhu; Zhang, Hanqi; Yu, Aimin; Zhang, Ziwei; Yu, Yong

2018-03-01

Based on the foaming property of the honey, a rapid, simple, and effective method solvent floatation (SF) was developed and firstly applied to the extraction and separation of triazine herbicides in honey. The analytes were determined by high-performance liquid chromatography. Some parameters affecting the extraction efficiencies, such as the type and volume of extraction solvent, type of salt, amount of (NH 4 ) 2 SO 4 , pH value of sample solution, gas flow rate, and floatation time, were investigated and optimized. The limits of detection for analytes are in the range of 0.16-0.56 μg kg -1 . The recoveries and relative standard deviations for determining triazines in five real honey samples are in the range of 78.2-112.9 and 0.2-9.2%, respectively.

Measurement of formaldehyde in clean air

NASA Astrophysics Data System (ADS)

Neitzert, Volker; Seiler, Wolfgang

1981-01-01

A method for the measurement of small amounts of formaldehyde in air has been developed. The method is based on the derivatization of HCHO with 2.4-Dinitrophenylhydrazine, forming 2.4-Dinitrophenylhydrazone, measured with GC-ECD-technique. HCHO is preconcentrated using a cryogenic sampling technique. The detection limit is 0.05 ppbv for a sampling volume of 200 liter. The method has been applied for measurements in continental and marine air masses showing HCHO mixing ratios of 0.4 - 5.0 ppbv and 0.2 - 1.0 ppbv, respectively. HCHO mixing ratios show diurnal variations with maximum values during the early afternoon and minimum values during the early morning. In continental air, HCHO mixing ratios are positively correlated with CO and SO2, indicating anthropogenic HCHO sources which are estimated to be 6-11 × 1012g/year-1 on a global scale.

Iraq liquid radioactive waste tanks maintenance and monitoring program plan.

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

Dennis, Matthew L.; Cochran, John Russell; Sol Shamsaldin, Emad

2011-10-01

The purpose of this report is to develop a project management plan for maintaining and monitoring liquid radioactive waste tanks at Iraq's Al-Tuwaitha Nuclear Research Center. Based on information from several sources, the Al-Tuwaitha site has approximately 30 waste tanks that contain varying amounts of liquid or sludge radioactive waste. All of the tanks have been non-operational for over 20 years and most have limited characterization. The program plan embodied in this document provides guidance on conducting radiological surveys, posting radiation control areas and controlling access, performing tank hazard assessments to remove debris and gain access, and conducting routine tankmore » inspections. This program plan provides general advice on how to sample and characterize tank contents, and how to prioritize tanks for soil sampling and borehole monitoring.« less

A future, intense source of negative hydrogen ions

NASA Technical Reports Server (NTRS)

Siefken, Hugh; Stein, Charles

1994-01-01

By directly heating lithium hydride in a vacuum, up to 18 micro-A/sq cm of negative hydrogen has been obtained from the crystal lattice. The amount of ion current extracted and analyzed is closely related to the temperature of the sample and to the rate at which the temperature is changed. The ion current appears to be emission limited and saturates with extraction voltage. For a fixed extraction voltage, the ion current could be maximized by placing a grid between the sample surface and the extraction electrode. Electrons accompanying the negative ions were removed by a magnetic trap. A Wein velocity filter was designed and built to provide definitive mass analysis of the extracted ion species. This technique when applied to other alkali hydrides may produce even higher intensity beams possessing low values of emittance.

Effect of purity on adsorption capacities of a Mars-like clay mineral at different pressures

NASA Technical Reports Server (NTRS)

Jenkins, Traci; Mcdoniel, Bridgett; Bustin, Roberta; Allton, Judith H.

1992-01-01

There has been considerable interest in adsorption of carbon dioxide on Marslike clay minerals. Some estimates of the carbon dioxide reservoir capacity of the martian regolith were calculated from the amount of carbon dioxide adsorbed on the ironrich smectite nontronite under martian conditions. The adsorption capacity of pure nontronite could place upper limits on the regolith carbon dioxide reservoir, both at present martian atmospheric pressure and at the postulated higher pressures required to permit liquid water on the surface. Adsorption of carbon dioxide on a Clay Mineral Society standard containing nontronite was studied over a wide range of pressures in the absence of water. Similar experiments were conducted on the pure nontronite extracted from the natural sample. Heating curves were obtained to help characterize and determine the purity of the clay sample.

A new derivatization approach with D-cysteine for the sensitive and simple analysis of acrylamide in foods by liquid chromatography-tandem mass spectrometry.

PubMed

Lim, Hyun-Hee; Shin, Ho-Sang

2014-09-26

A liquid chromatography-tandem mass spectrometry method (LC-MS/MS) was developed in order to determine the amount of acrylamide in foods after derivatization with d-cysteine. The sulfhydryl group of d-cysteine was added at the β-site double bond of acrylamide to form 2-amino-3-(3-amino-3-oxo-propyl)sulfanyl-propanoic acid. Deuterated acrylamide (acrylamide-d3) was chosen as the internal standard (IS) for analyzing the food samples. Acrylamide was extracted from 2.0 g of food sample with 6 mL of methylene chloride, and the organic extract was diluted with 3 mL of hexane, and then the analyte was back-extracted with 0.5 mL of pure water. The derivatization of acrylamide was performed in the water extract. The best reaction conditions (3.0mg of d-cysteine, a pH 6.5, a reaction temperature of 90°C, and a heating time of 50 min) were established by the variation of parameters. The formed derivative was injected into the LC-MS/MS without further extraction or purification procedures. Separation and detection were improved with the use of an ion-pairing reagent of perfluorooctanoic acid. Under the established conditions, the limits of detection and the limits of quantification were 0.04 μg/kg and 0.14 μg/kg, respectively, and the inter-day relative standard deviation was less than 8% at concentrations of 20 and 100 μg/kg. The method was successfully applied to determine the amount of acrylamide in potato chips, French fries, and coffee. Copyright © 2014 Elsevier B.V. All rights reserved.

Label-free quantitation of peptide release from neurons in a microfluidic device with mass spectrometry imaging

PubMed Central

Zhong, Ming; Lee, Chang Young; Croushore, Callie A.; Sweedler, Jonathan V.

2013-01-01

Microfluidic technology allows the manipulation of mass-limited samples and when used with cultured cells, enables control of the extracellular microenvironment, making it well suited for studying neurons and their response to environmental perturbations. While matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS) provides for off-line coupling to microfluidic devices for characterizing small-volume extracellular releasates, performing quantitative studies with MALDI is challenging. Here we describe a label-free absolute quantitation approach for microfluidic devices. We optimize device fabrication to prevent analyte losses before measurement and then incorporate a substrate that collects the analytes as they flow through a collection channel. Following collection, the channel is interrogated using MS imaging. Rather than quantifying the sample present via MS peak height, the length of the channel containing appreciable analyte signal is used as a measure of analyte amount. A linear relationship between peptide amount and band length is suggested by modeling the adsorption process and this relationship is validated using two neuropeptides, acidic peptide (AP) and α-bag cell peptide [1-9] (αBCP). The variance of length measurement, defined as the ratio of standard error to mean value, is as low as 3% between devices. The limit of detection (LOD) of our system is 600 fmol for AP and 400 fmol for αBCP. Using appropriate calibrations, we determined that an individual Aplysia bag cell neuron secretes 0.15 ± 0.03 pmol of AP and 0.13 ± 0.06 pmol of αBCP after being stimulated with elevated KCl. This quantitation approach is robust, does not require labeling, and is well suited for miniaturized off-line characterization from microfluidic devices. PMID:22508372

Mycorrhizal symbiosis effects on growth of chalk false-brome (Brachypodium pinnatum) are dependent on the environmental light regime.

PubMed

Füzy, Anna; Bothe, Hermann; Molnár, Edit; Biró, Borbála

2014-03-01

AMF (arbuscular mycorrhizal fungi) colonization of the grass chalk false-brome (Brachypodium pinnatum (L.) P. B.) was studied in selected habitats under spatially different light regimes: (a) shade condition under oak trees, (b) half shade in a shrubby area and (c) full-sun conditions on unshaded grassland. This study assessed the variations in AMF colonization of the grass dependent on the light supply in field habitats. Soil, root and shoot samples were collected four times during the vegetation period (in June, July, September and October). Root colonization, root and shoot biomass as well as soil water content were determined. The highest rate of AMF colonization was detected in June under half-sun and full-sun conditions, where about 50% of the roots were colonized. The average amount of arbuscules was less than 20% in the roots at the three sites, with the highest number of arbuscules in June, under half-sun and full-sun conditions, however, not under the trees. Overall, best mycorrhizal colonization occurred during summer, and its rate decreased in autumn. This tendency inversely correlated with the amount of precipitation, and thus with the water content of soils. The high colonization rate of the examined root samples, and also its seasonal fluctuation, might reflect the importance of the symbiosis where inorganic nutrients and water are the growth-limiting factors. The marginal AMF colonization of chalk false-brome under shade conditions indicates that plants do not use AMF under all stress conditions. When low light limits photosynthesis and thus growth of the plants, they dispense with the colonization of AMF in order to save the expenditure of organic carbon. Copyright © 2013 Elsevier GmbH. All rights reserved.

Chemical-mineralogical characterization of C and D waste recycled aggregates from Sao Paulo, Brazil

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

Angulo, S.C.; Ulsen, C.; John, V.M.

2009-02-15

This study presents a methodology for the characterization of construction and demolition (C and D) waste recycled aggregates based on a combination of analytical techniques (X-ray fluorescence (XRF), soluble ions, semi-quantitative X-ray diffraction (XRD), thermogravimetric analysis (TGA-DTG) and hydrochloric acid (HCl) selective dissolution). These combined analytical techniques allow for the estimation of the amount of cement paste, its most important hydrated and carbonated phases, as well as the amount of clay and micas. Details of the methodology are presented here and the results of three representative C and D samples taken from the Sao Paulo region in Brazil are discussed.more » Chemical compositions of mixed C and D aggregate samples have mostly been influenced by particle size rather than the visual classification of C and D into red or grey and geographical origin. The amount of measured soluble salts in C and D aggregates (0.15-25.4 mm) is lower than the usual limits for mortar and concrete production. The content of porous cement paste in the C and D aggregates is around 19.3% (w/w). However, this content is significantly lower than the 43% detected for the C and D powders (<0.15 mm). The clay content of the powders was also high, potentially resulting from soil intermixed with the C and D waste, as well as poorly burnt red ceramic. Since only about 50% of the measured CaO is combined with CO{sub 2}, the powders have potential use as raw materials for the cement industry.« less

A solid-phase extraction method using Transcarpathian clinoptilolite for preconcentration of trace amounts of terbium in water samples.

PubMed

Vasylechko, Volodymyr O; Gryshchouk, Galyna V; Zakordonskiy, Victor P; Vyviurska, Olga; Pashuk, Andriy V

2015-01-01

In spite of the fact that terbium is one of the rarest elements in the Earth's crust, it is frequently used for the production of high technological materials. At the result, an effective combination of sample preparation procedure and detection method for terbium ions in different matrices is highly required. The solid-phase extraction procedure with natural Transcarpathian clinoptilolite thermally activated at 350 °C was used to preconcentrate trace amounts of terbium ions in aqueous solutions for a final spectrophotometric determination with arsenazo III. Thermogravimetric investigations confirmed the existence of relations between changes that appeared during dehydratation of calcined zeolite and its sorption affinity. Since the maximum of sorption capacity towards terbium was observed at pH 8.25, a borate buffer medium (2.5 · 10(-4) М) was used to maintain ionic force and solution acidity. Terbium was quantitatively removed from the solid-phase extraction column with a 1.0 M solution of sodium chloride (pH 2.5). The linearity of the proposed method was evaluated in the range of 2.5-200 ng · mL(-1) with detection limit 0.75 ng · mL(-1). Due to acceptable recoveries (93.3-102.0 %) and RSD values (6-7.1) from spiked tap water, the developed method can be successfully applied for the determination of trace amounts of terbium ions in the presence of major components of water. Graphical abstractSorption of terbium(III) ions on clinoptilolite.

Development and validation of a single LC-MS/MS assay following SPE for simultaneous hair analysis of amphetamines, opiates, cocaine and metabolites.

PubMed

Imbert, L; Dulaurent, S; Mercerolle, M; Morichon, J; Lachâtre, G; Gaulier, J-M

2014-01-01

The two major challenges in hair analysis are the limited amount of samples usually available and the low targeted concentrations. To overcome these limitations, a liquid chromatography-electrospray-tandem mass spectrometry method (LC-ESI-MS/MS) allowing the simultaneous analysis of 17 amphetamines (amphetamine, BDB, m-CPP, dexfenfluramine, DOB, DOM, ephedrine, MBDB, MDA, MDEA, MDMA, methamphetamine, methylphenidate, 4-MTA, norephedrine, norfenfluramine and PMA), 5 opiates (morphine, codeine, heroin, ethylmorphine, and 6AM), cocaine and 5 metabolites [ecgonine methyl ester (EME), benzoylecgonine (BZE), anhydroecgonine methyl ester (AME), cocaethylene, and norcocaine] has been developed. The validation procedure included linearity, intra-day and inter-day variability and accuracy for 5 days (5 replicates at 3 concentration levels). Proficiency studies were used to check the accuracy of the method. As a result, all amphetamines, opiates and cocaine derivatives were satisfactory identified by 2 MRM transitions in 15 min. Calibration curves were performed by a quadratic 1/X weighted regression. The calibration model fits from 0.05 to 10 ng/mg. The limits of detection (LODs) range between 0.005 and 0.030 ng/mg. Precision has been checked by intra-day and inter-day RSD, and associated relative bias, which were lower than 25% for the limits of quantifications (LOQs) and lower than 20% for the other levels tested. This method was routinely applied to hair samples: two positive results of adult drug addicts are presented. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

Iron species determination by task-specific ionic liquid-based in situ solvent formation dispersive liquid-liquid microextraction combined with flame atomic absorption spectrometry.

PubMed

Sadeghi, Susan; Ashoori, Vahid

2017-10-01

The task-specific ionic liquid (TSIL) of 1-ethyl-3-methylimidazolium bromide functionalized with 8-hydroxyquinoline was used as a chelating agent and extracting solvent for dispersive liquid-liquid microextraction and subsequent determination of Fe(III) by flame atomic absorption spectrometry. The in situ solvent formation of TSIL using KPF 6 provided the desired water-immiscible ionic liquid. The total Fe concentration could be determined after pre-oxidation of Fe(II) to Fe(III). Various factors affecting the proposed extraction procedure were optimized. The proposed analytical conditions were: sample pH 5, TSIL amount 0.3% (w/v), KPF 6 amount 0.15% (w/v), anti-sticking 0.1% (w/v) and salt concentration 5% (w/v). Under optimal conditions, the linear dynamic ranges for Fe(III) and total Fe were 20-80 and 20-110 ng mL -1 , respectively, with a detection limit of 6.9 ng mL -1 for Fe(III) and relative standard deviation of 2.2%. The proposed method was successfully applied to the determination of trace Fe(III) in water (underground, tap, refined water and artificial sea water) and beverage (apple, tomato, and tea) samples. The developed method offers advantages such as simplicity, ease of operation, and extraction of Fe(III) from aqueous solutions without the use of organic solvent. It was successfully applied for iron speciation in different real samples. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Dioxin analysis in water by using a passive sampler and CALUX bioassay.

PubMed

Addeck, Amr; Croes, Kim; Van Langenhove, Kersten; Denison, Michael; Elskens, Marc; Baeyens, Willy

2012-01-15

Passive sampling of organic pollutants is a new trend in environmental monitoring and analysis. Passive samplers are being developed to overcome the drawbacks of the conventional snapshot sampling approach. The ceramic toximeter is a promising passive sampler for monitoring dioxin-contaminated surface and ground waters. It consists of an alumina cylinder lined with a thin coating of titania and a pore diameter of 0.05 μm. The cylinder serves as a diffusion barrier limiting the analyte transport to molecular diffusion only, as well as a container for a selective trapping material of a high capacity and affinity towards the chemical(s) of concern. The cylinder is closed from both sides with PTFE caps. The ceramic toximeter was filled with activated carbon as the trapping material and has been tested in vitro for the sampling of dioxin-contaminated water. In addition, the utilization of the CALUX bioassay technique for analyzing the trapped dioxin has greatly reduced the time and costs for dioxin scanning in aqueous media. Exposure times varied between 1 and 7 days in a solution of 1.35 ng-TCDDL(-1) (TCDD is 2,3,7,8-tetrachlorodibenzodioxin). The mean effective molecular diffusion coefficient of TCDD in the toximeter amounts to 11.9×10(-6)m(2)d(-1) while the minimum concentration detectable in an aquatic system after 30 days of exposure amounts to 0.89 pg-TCDDL(-1). Copyright © 2011 Elsevier B.V. All rights reserved.

Simultaneous determination of estrogenic odorant alkylphenols, chlorophenols, and their derivatives in water using online headspace solid phase microextraction coupled with gas chromatography-mass spectrometry.

PubMed

Yuan, Su-Fen; Liu, Ze-Hua; Lian, Hai-Xian; Yang, Chuangtao; Lin, Qing; Yin, Hua; Dang, Zhi

2016-10-01

A simple online headspace solid-phase microextraction (HS-SPME) coupled with the gas chromatography-mass spectrometry (GC-MS) method was developed for simultaneous determination of trace amounts of nine estrogenic odorant alkylphenols and chlorophenols and their derivatives in water samples. The extraction conditions of HS-SPME were optimized including fiber selection, extraction temperature, extraction time, and salt concentration. Results showed that divinylbenzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber was the most appropriate one among the three selected commercial fibers, and the optimal extraction temperature, time, and salt concentration were 70 °C, 30 min, and 0.25 g/mL, respectively. The developed method was validated and showed good linearity (R (2) > 0.989), low limit of detection (LOD, 0.002-0.5 μg/L), and excellent recoveries (76-126 %) with low relative standard deviation (RSD, 0.7-12.9 %). The developed method was finally applied to two surface water samples and some of these target compounds were detected. All these detected compounds were below their odor thresholds, except for 2,4,6-TCAS and 2,4,6-TBAS wherein their concentrations were near their odor thresholds. However, in the two surface water samples, these detected compounds contributed to a certain amount of estrogenicity, which seemed to suggest that more attention should be paid to the issue of estrogenicity rather than to the odor problem.

Analysis of (210)Pb in water samples with plastic scintillation resins.

PubMed

Lluch, E; Barrera, J; Tarancón, A; Bagán, H; García, J F

2016-10-12

(210)Pb is a radioactive lead isotope present in the environment as member of the (238)U decay chain. Since it is a relatively long-lived radionuclide (T1/2 = 22.2 years), its analysis is of interest in radiation protection and the geochronology of sediments and artwork. Here, we present a method for analysing (210)Pb using plastic scintillation resins (PSresins) packaged in solid-phase extraction columns (SPE cartridge). The advantages of this method are its selectivity, the low limit of detection, as well as reductions in the amount of time and reagents required for analysis and the quantity of waste generated. The PSresins used in this study were composed of a selective extractant (4',4″(5″)-Di-tert-butyldicyclohexano-18-crown-6 in 1-octanol) covering the surface of plastic scintillation microspheres. Once the amount of extractant (1:1/4) and medium of separation (2 M HNO3) were optimised, PSresins in SPE cartridges were calibrated with a standard solution of (210)Pb. (210)Pb could be fully separated from its daughters, (210)Bi and (210)Po, with a recovery value of 91(3)% and detection efficiency of 44(3)%. Three spiked water samples (one underground and two river water samples) were analysed in triplicates with deviations lower than 10%, demonstrating the validity of the PS resin method for (210)Pb analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

The effect of limited availability of N or water on C allocation to fine roots and annual fine root turnover in Alnus incana and Salix viminalis.

PubMed

Rytter, Rose-Marie

2013-09-01

The effect of limited nitrogen (N) or water availability on fine root growth and turnover was examined in two deciduous species, Alnus incana L. and Salix viminalis L., grown under three different regimes: (i) supply of N and water in amounts which would not hamper growth, (ii) limited N supply and (iii) limited water supply. Plants were grown outdoors during three seasons in covered and buried lysimeters placed in a stand structure and filled with quartz sand. Computer-controlled irrigation and fertilization were supplied through drip tubes. Production and turnover of fine roots were estimated by combining minirhizotron observations and core sampling, or by sequential core sampling. Annual turnover rates of fine roots <1 mm (5-6 year(-1)) and 1-2 mm (0.9-2.8 year(-1)) were not affected by changes in N or water availability. Fine root production (<1 mm) differed between Alnus and Salix, and between treatments in Salix; i.e., absolute length and biomass production increased in the order: water limited < unlimited < N limited. Few treatment effects were detected for fine roots 1-2 mm. Proportionally more C was allocated to fine roots (≤2 mm) in N or water-limited Salix; 2.7 and 2.3 times the allocation to fine roots in the unlimited regime, respectively. Estimated input to soil organic carbon increased by ca. 20% at N limitation in Salix. However, future studies on fine root decomposition under various environmental conditions are required. Fine root growth responses to N or water limitation were less pronounced in Alnus, thus indicating species differences caused by N-fixing capacity and slower initial growth in Alnus, or higher fine root plasticity in Salix. A similar seasonal growth pattern across species and treatments suggested the influence of outer stimuli, such as temperature and light.

A novel thermometric biosensor for fast surveillance of β-lactamase activity in milk.

PubMed

Zhou, Shuang; Zhao, Yunfeng; Mecklenburg, Michael; Yang, Dajin; Xie, Bin

2013-11-15

Regulatory restrictions on antibiotic residues in dairy products have resulted in the illegal addition of β-lactamase to lower antibiotic levels in milk in China. Here we demonstrate a fast, sensitive and convenient method based on enzyme thermistor (ET) for the surveillance of β-lactamase in milk. A fixed amount of penicillin G, which is a specific substrate of β-lactamase, was incubated with the milk sample, and an aliquot of the mixture was directly injected into the ET system to give a temperature change corresponding to the remained penicillin G. The amount of β-lactamase present in sample was deduced by the penicillin G consumed during incubation. This method was successfully applied to quantify β-lactamase in milk with the linear range of 1.1-20 UmL(-1) and the detection limit of 1.1 UmL(-1). The recoveries ranged from 93% to 105%, with relative standard deviations (RSDs) below 8%. The stability of the column equipped in ET was also studied, and only 5% decrease of activity was observed after 60 days of use. Compared with the conventional culture-based assay, the advantages of high throughput, timesaving and accurate quantification have made this method an ideal alternative for routine use. Copyright © 2013 Elsevier B.V. All rights reserved.

[Determination of olive oil content in olive blend oil by headspace gas chromatography-mass spectrometry].

PubMed

Jiang, Wanfeng; Zhang, Ning; Zhang, Fengyan; Yang, Zhao

2017-07-08

A method for the determination of the content of olive oil in olive blend oil by headspace gas chromatography-mass spectrometry (SH-GC/MS) was established. The amount of the sample, the heating temperature, the heating time, the amount of injection, the injection mode and the chromatographic column were optimized. The characteristic compounds of olive oil were found by chemometric method. A sample of 1.0 g was placed in a 20 mL headspace flask, and heated at 180℃ for 2700 s. Then, 1.0 mL headspace gas was taken into the instrument. An HP-88 chromatographic column was used for the separation and the analysis was performed by GC/MS. The results showed that the linear range was 0-100%(olive oil content). The linear correlation coefficient ( r 2 ) was more than 0.995, and the limits of detection were 1.26%-2.13%. The deviations of olive oil contents in the olive blend oil were from -0.65% to 1.02%, with the relative deviations from -1.3% to 6.8% and the relative standard deviations from 1.18% to 4.26% ( n =6). The method is simple, rapid, environment friendly, sensitive and accurate. It is suitable for the determination of the content of olive oil in olive blend oil.

New method for determination of epichlorohydrin in epoxy-coated cans by oxolane derivatization and gas chromatography-mass spectrometry.

PubMed

Sung, Jun Hyun; Lee, Young Ja; Park, Hyun Jin

2008-08-01

A new method was developed for the determination of epichlorohydrin (ECH) in food contact surface of epoxy-coated cans. The oxolane derivative, which produced by reaction of epoxy moiety in ECH with cyclopentanone in the presence of borontrifluoride-diethyletherate, was analyzed by gas chromatography (GC)/mass spectrometry (MS). 1,2-Epoxyhexane was used as internal standard (IS), which produced an oxolane derivative under the same reaction mechanism as ECH. The developed method was validated with 1 ng ml(-1) of limit of detection (LOD, surface area related 20 ng dm(-2)), >0.999 of linearity. Good precision, which was tested both in terms of intra-day repeatability and inter-day reproducibility, and 97.3-102.7% of good recoveries were obtained on three spiked levels of 5.2, 40.3 and 149.1 ng ml(-1). The excellent validation data suggests that this method is more simple, quick and effective than the official method in European Committee for Standardization (CEN) to determine the residual amount of ECH in food contact materials for food law compliance test. The residual amount of ECH for 13 epoxy-coated can samples was analyzed, and none of the samples was found to be detectable levels of ECH in epoxy-coated cans.

Multigen-2 Pre-Flight Testing: Science Testing Unit (STU) and Stowage Conditions

NASA Astrophysics Data System (ADS)

Kittang, A.-I.; Kvaloy, B.; Berg, C.; Rakvaag, G.; Iversen, T.-H.

2008-06-01

The Multigen-2 experiment Science Testing Unit (STU) proved to be a useful tool in optimizing experiment environment settings for cultivation of Arabidopsis thaliana (Col-0) in the European Modular Cultivation System (EMCS). By using the EMCS Experiment Reference Model (ERM); light, temperature and air flow regimes for optimal growth could be tested. Healthy seedlings were obtained using the STU#2 and STU#3 in the EMCS ERM. It was concluded that the Experiment Container Development Kit (ECDK) is unsuitable for the Multigen-2 testing due to limitation in the ECDK temperature control. The results from the stowage condition tests showed that the selected growth medium (agar) can be used after 3 months at +4°C. The seeds show a germination rate of ≥80% after sterilisation and stowed for 5 months. The Multigen-2 plant samples will be fixed in RNA later and stored at - 80 °C. Three methods with different RNA isolation kits showed that the Qiagen kit (#74904) gave the highest amount and the best quality of Total RNA from RNA Later and frozen samples. The amount of plant material from one cultivation chamber gives two RNA isolations. Each of the isolations gives Total RNA sufficient for at least two microarray analyses.