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Sample records for air sample extract

  1. CLEANLINESS OF COMMON AIR SAMPLING SORBENTS FOR APPLICATION TO PHENOLIC COMPOUNDS MEASUREMENT USING SUPERCRITICAL FLUID EXTRACTION

    Science.gov (United States)

    The trace-level measurement of phenolic compounds in the ambient air is complicated by the acidic and polar nature of the compounds especially during recovery from the sampling medium. ecently, supercritical fluid extraction (SFE) has been proposed as an alternative extraction me...

  2. Automated Sampling and Extraction of Krypton from Small Air Samples for Kr-85 Measurement Using Atom Trap Trace Analysis

    International Nuclear Information System (INIS)

    Atom-Trap-Trace-Analysis (ATTA) provides the capability of measuring the Krypton-85 concentration in microlitre amounts of krypton extracted from air samples of about 1 litre. This sample size is sufficiently small to allow for a range of applications, including on-site spot sampling and continuous sampling over periods of several hours. All samples can be easily handled and transported to an off-site laboratory for ATTA measurement, or stored and analyzed on demand. Bayesian sampling methodologies can be applied by blending samples for bulk measurement and performing in-depth analysis as required. Prerequisite for measurement is the extraction of a pure krypton fraction from the sample. This paper introduces an extraction unit able to isolate the krypton in small ambient air samples with high speed, high efficiency and in a fully automated manner using a combination of cryogenic distillation and gas chromatography. Air samples are collected using an automated smart sampler developed in-house to achieve a constant sampling rate over adjustable time periods ranging from 5 minutes to 3 hours per sample. The smart sampler can be deployed in the field and operate on battery for one week to take up to 60 air samples. This high flexibility of sampling and the fast, robust sample preparation are a valuable tool for research and the application of Kr-85 measurements to novel Safeguards procedures. (author)

  3. Hot methanol extraction for the analysis of volatile organic chemicals in subsurface core samples from Dover Air Force Base, Delaware

    Energy Technology Data Exchange (ETDEWEB)

    Ball, W.P.; Xia, G.; Durfee, D.P.; Wilson, R.D.; Brown, M.J.; Mackay, D.M.

    1997-06-01

    The evaluation of contaminant concentrations in ground water and soil is an essential aspect of most hazardous waste remedial investigations. This paper describes methods applied toward obtaining, preserving, and analyzing subsurface samples for the determination of VOC concentration in the saturated region of an unconfined coastal plain aquifer at Dover Air Force Base (DAFB), Delaware. The described protocol involved headspace-free subsampling of cores, field preservation of subsamples in methanol, and overnight extraction of the VOCs at elevated temperature (70 C). Methanol-extracted compounds were subsequently transferred to hexane and analyzed by gas chromatography. The method was found to achieve quantitative extraction from the aquifer sands in a single step, although extraction from fine-grained and more strongly sorbing aquitard samples required multiple methanol extractions to achieve comparable recovery. An extensive set of DAFB results is presented as an indication of how these methods can be applied toward characterizing field-scale contamination with a high degree of resolution and accuracy.

  4. Radioactive air sampling methods

    CERN Document Server

    Maiello, Mark L

    2010-01-01

    Although the field of radioactive air sampling has matured and evolved over decades, it has lacked a single resource that assimilates technical and background information on its many facets. Edited by experts and with contributions from top practitioners and researchers, Radioactive Air Sampling Methods provides authoritative guidance on measuring airborne radioactivity from industrial, research, and nuclear power operations, as well as naturally occuring radioactivity in the environment. Designed for industrial hygienists, air quality experts, and heath physicists, the book delves into the applied research advancing and transforming practice with improvements to measurement equipment, human dose modeling of inhaled radioactivity, and radiation safety regulations. To present a wide picture of the field, it covers the international and national standards that guide the quality of air sampling measurements and equipment. It discusses emergency response issues, including radioactive fallout and the assets used ...

  5. Trace Analysis in End-Exhaled Air Using Direct Solvent Extraction in Gas Sampling Tubes: Tetrachloroethene in Workers as an Example

    Directory of Open Access Journals (Sweden)

    Chris-Elmo Ziener

    2014-01-01

    Full Text Available Simple and cost-effective analytical methods are required to overcome the barriers preventing the use of exhaled air in routine occupational biological monitoring. Against this background, a new method is proposed that simplifies the automation and calibration of the analytical measurements. End-exhaled air is sampled using valveless gas sampling tubes made of glass. Gaseous analytes are transferred to a liquid phase using a microscale solvent extraction performed directly inside the gas sampling tubes. The liquid extracts are analysed using a gas chromatograph equipped, as usual, with a liquid autosampler, and liquid standards are used for calibration. For demonstration purposes, the method’s concept was applied to the determination of tetrachloroethene in end-exhaled air, which is a biomarker for occupational tetrachloroethene exposure. The method’s performance was investigated in the concentration range 2 to 20 μg tetrachloroethene/L, which corresponds to today’s exposure levels. The calibration curve was linear, and the intra-assay repeatability and recovery rate were sufficient. Analysis of real samples from dry-cleaning workers occupationally exposed to tetrachloroethene and from nonexposed subjects demonstrated the method’s utility. In the case of tetrachloroethene, the method can be deployed quickly, requires no previous experiences in gas analysis, provides sufficient analytical reliability, and addresses typical end-exhaled air concentrations from exposed workers.

  6. Air sampling in the workplace

    International Nuclear Information System (INIS)

    This report provides technical information on air sampling that will be useful for facilities following the recommendations in the NRC's Regulatory Guide 8.25, Revision 1, ''Air sampling in the Workplace.'' That guide addresses air sampling to meet the requirements in NRC's regulations on radiation protection, 10 CFR Part 20. This report describes how to determine the need for air sampling based on the amount of material in process modified by the type of material, release potential, and confinement of the material. The purposes of air sampling and how the purposes affect the types of air sampling provided are discussed. The report discusses how to locate air samplers to accurately determine the concentrations of airborne radioactive materials that workers will be exposed to. The need for and the methods of performing airflow pattern studies to improve the accuracy of air sampling results are included. The report presents and gives examples of several techniques that can be used to evaluate whether the airborne concentrations of material are representative of the air inhaled by workers. Methods to adjust derived air concentrations for particle size are described. Methods to calibrate for volume of air sampled and estimate the uncertainty in the volume of air sampled are described. Statistical tests for determining minimum detectable concentrations are presented. How to perform an annual evaluation of the adequacy of the air sampling is also discussed

  7. Simultaneous analysis of organochlorine pesticides and polychlorinated biphenyls in air samples by using accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) coupled to gas chromatography dual electron capture detection.

    Science.gov (United States)

    Mokbel, Haifaa; Al Dine, Enaam Jamal; Elmoll, Ahmad; Liaud, Céline; Millet, Maurice

    2016-04-01

    An analytical method associating accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) in immersion mode combined with gas chromatography dual electrons capture detectors (SPME-GC-2ECD) has been developed and studied for the simultaneous determination of 19 organochlorine pesticides (OCPs) and 22 polychlorinated biphenyls (PCBs) in air samples (active and XAD-2 passive samplers). Samples were extracted with ASE with acetonitrile using the following conditions: temperature, 150 °C; pressure, 1500 psi; static, 15 min; cycles, 3; purge, 300 s; flush, 100 %. Extracts were reduced to 1 mL, and 500 μL of this extract, filled with deionised water, was subject to SPME extraction. Experimental results indicated that the proposed method attained the best extraction efficiency under the optimised conditions: extraction of PCB-OCP mixture using 100-μm PDMS fibre at 80 °C for 40 min with no addition of salt. The performance of the proposed ASE-SPME-GC-2ECD methodology with respect to linearity, limit of quantification and detection was evaluated by spiking of XAD-2 resin with target compounds. The regression coefficient (R (2)) of most compounds was found to be high of 0.99. limits of detection (LODs) are between 0.02 and 4.90 ng m(-3), and limits of quantification (LOQs) are between 0.05 and 9.12 ng m(-3) and between 0.2 and 49 ng/sampler and 0.52 and 91 ng/sampler, respectively, for XAD-2 passive samplers. Finally, a developed procedure was applied to determine selected PCBs and OCPs in the atmosphere. PMID:26780048

  8. Temporal-spatial analysis of U.S.-Mexico border environmental fine and coarse PM air sample extract activity in human bronchial epithelial cells

    International Nuclear Information System (INIS)

    Particulate matter less than 10 μm (PM10) has been shown to be associated with aggravation of asthma and respiratory and cardiopulmonary morbidity. There is also great interest in the potential health effects of PM2.5. Particulate matter (PM) varies in composition both spatially and temporally depending on the source, location and seasonal condition. El Paso County which lies in the Paso del Norte airshed is a unique location to study ambient air pollution due to three major points: the geological land formation, the relatively large population and the various sources of PM. In this study, dichotomous filters were collected from various sites in El Paso County every 7 days for a period of 1 year. The sampling sites were both distant and near border crossings, which are near heavily populated areas with high traffic volume. Fine (PM2.5) and Coarse (PM10-2.5) PM filter samples were extracted using dichloromethane and were assessed for biologic activity and polycyclic aromatic (PAH) content. Three sets of marker genes human BEAS2B bronchial epithelial cells were utilized to assess the effects of airborne PAHs on biologic activities associated with specific biological pathways associated with airway diseases. These pathways included in inflammatory cytokine production (IL-6, IL-8), oxidative stress (HMOX-1, NQO-1, ALDH3A1, AKR1C1), and aryl hydrocarbon receptor (AhR)-dependent signaling (CYP1A1). Results demonstrated interesting temporal and spatial patterns of gene induction for all pathways, particularly those associated with oxidative stress, and significant differences in the PAHs detected in the PM10-2.5 and PM2.5 fractions. Temporally, the greatest effects on gene induction were observed in winter months, which appeared to correlate with inversions that are common in the air basin. Spatially, the greatest gene expression increases were seen in extracts collected from the central most areas of El Paso which are also closest to highways and border crossings.

  9. Phenol extraction of DNA samples

    OpenAIRE

    sprotocols

    2014-01-01

    Typically, an equal volume of TE-saturated phenol is added to an aqueous DNA sample in a microcentrifuge tube. The mixture is vigorously vortexed, and then centrifuged to enact phase separation. The upper, aqueous layer carefully is removed to a new tube, avoiding the phenol interface and then is subjected to two ether extractions to remove residual phenol. An equal volume of water-saturated ether is added to the tube, the mixture is vortexed, and the tube is centrifuged to allow phase separa...

  10. Air sampling in the workplace. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Hickey, E.E.; Stoetzel, G.A.; Strom, D.J.; Cicotte, G.R. [Pacific Northwest Lab., Richland, WA (United States); Wiblin, C.M. [Advanced Systems Technology, Inc., Atlanta, GA (United States); McGuire, S.A. [Nuclear Regulatory Commission, Washington, DC (United States). Div. of Regulatory Applications

    1993-09-01

    This report provides technical information on air sampling that will be useful for facilities following the recommendations in the NRC`s Regulatory Guide 8.25, Revision 1, ``Air sampling in the Workplace.`` That guide addresses air sampling to meet the requirements in NRC`s regulations on radiation protection, 10 CFR Part 20. This report describes how to determine the need for air sampling based on the amount of material in process modified by the type of material, release potential, and confinement of the material. The purposes of air sampling and how the purposes affect the types of air sampling provided are discussed. The report discusses how to locate air samplers to accurately determine the concentrations of airborne radioactive materials that workers will be exposed to. The need for and the methods of performing airflow pattern studies to improve the accuracy of air sampling results are included. The report presents and gives examples of several techniques that can be used to evaluate whether the airborne concentrations of material are representative of the air inhaled by workers. Methods to adjust derived air concentrations for particle size are described. Methods to calibrate for volume of air sampled and estimate the uncertainty in the volume of air sampled are described. Statistical tests for determining minimum detectable concentrations are presented. How to perform an annual evaluation of the adequacy of the air sampling is also discussed.

  11. Guidance for air sampling at nuclear facilities

    International Nuclear Information System (INIS)

    The principal uses of air sampling at nuclear facilities are to monitor general levels of radioactive air contamination, identify sources of air contamination, and evaluate the effectiveness of contaminant control equipment, determine exposures of individual workers, and provide automatic warning of hazardous concentrations of radioactivity. These applications of air sampling are discussed with respect to standards of occupational exposure, instrumentation, sample analysis, sampling protocol, and statistical treatment of concentration data. Emphasis is given to the influence of spacial and temporal variations of radionuclide concentration on the location, duration, and frequency of air sampling

  12. Cabin Air Sampling Study Functionality Test.

    OpenAIRE

    Muir, Helen; Walton, Christopher; McKeown, Rebecca

    2008-01-01

    The Department for Transport (DFT), on behalf of the Government’s Aviation Health Working Group (AHWG), commissioned Cranfield University to organise, manage and deliver a functionality test of a variety of air sampling devices capable of detecting a wide range of compounds in a cabin air environment. The functionality test was to be the preliminary stage of a major monitoring study of the cabin air environment, which the Department intends to conduct. Report prepared for the Department f...

  13. Reduced bleed air extraction for DC-10 cabin air conditioning

    Science.gov (United States)

    Newman, W. H.; Viele, M. R.; Hrach, F. J.

    1980-01-01

    It is noted that a significant fuel savings can be achieved by reducing bleed air used for cabin air conditioning. Air in the cabin can be recirculated to maintain comfortable ventilation rates but the quality of the air tends to decrease due to entrainment of smoke and odors. Attention is given to a development system designed and fabricated under the NASA Engine Component Improvement Program to define the recirculation limit for the DC-10. It is shown that with the system, a wide range of bleed air reductions and recirculation rates is possible. A goal of 0.8% fuel savings has been achieved which results from a 50% reduction in bleed extraction from the engine.

  14. East Mountain Area 1995 air sampling results

    Energy Technology Data Exchange (ETDEWEB)

    Deola, R.A. [Sandia National Labs., Albuquerque, NM (United States). Air Quality Dept.

    1996-09-01

    Ambient air samples were taken at two locations in the East Mountain Area in conjunction with thermal testing at the Lurance Canyon Burn Site (LCBS). The samples were taken to provide measurements of particulate matter with a diameter less than or equal to 10 micrometers (PM{sub 10}) and volatile organic compounds (VOCs). This report summarizes the results of the sampling performed in 1995. The results from small-scale testing performed to determine the potentially produced air pollutants in the thermal tests are included in this report. Analytical results indicate few samples produced measurable concentrations of pollutants believed to be produced by thermal testing. Recommendations for future air sampling in the East Mountain Area are also noted.

  15. East Mountain Area 1995 air sampling results

    International Nuclear Information System (INIS)

    Ambient air samples were taken at two locations in the East Mountain Area in conjunction with thermal testing at the Lurance Canyon Burn Site (LCBS). The samples were taken to provide measurements of particulate matter with a diameter less than or equal to 10 micrometers (PM10) and volatile organic compounds (VOCs). This report summarizes the results of the sampling performed in 1995. The results from small-scale testing performed to determine the potentially produced air pollutants in the thermal tests are included in this report. Analytical results indicate few samples produced measurable concentrations of pollutants believed to be produced by thermal testing. Recommendations for future air sampling in the East Mountain Area are also noted

  16. Air sampling system for airborne surveys

    International Nuclear Information System (INIS)

    An air sampling system has been designed for installation on the Beechcraft King Air A-100 aircraft as a part of the Aerial Radiological Measuring System (ARMS). It is intended for both particle and whole gas sampling. The sampling probe is designed for isokinetic sampling and is mounted on a removable modified escape hatch cover, behind the co-pilot's seat, and extends about two feet forward of the hatch cover in the air stream lines. Directly behind the sampling probe inside the modified hatch cover is an expansion chamber, space for a 5-inch diameter filter paper cassette, and an optional four-stage cascade impactor for particle size distribution measurements. A pair of motors and blower pumps provide the necessary 0.5 atmosphere pressure across the type MSA 1106 B glass fiber filter paper to allow a flow rate of 50 cfm. The MSA 1106 B filter paper is designed to trap sub-micrometer particles with a high efficiency; it was chosen to enable a quantitative measurement of airborne radon daughters, one of the principal sources of background signals when radiological surveys are being performed. A venturi section and pressure gauges allow air flow rate measurements so that airborne contaminant concentrations may be quantified. A whole gas sampler capable of sampling a cubic meter of air is mounted inside the aircraft cabin. A nuclear counting system on board the aircraft provides capability for α, β and γ counting of filter paper samples. Design data are presented and types of survey missions which may be served by this system are described

  17. An analytical method coupling accelerated solvent extraction and HPLC-fluorescence for the quantification of particle-bound PAHs in indoor air sampled with a 3-stages cascade impactor.

    Science.gov (United States)

    Liaud, Céline; Millet, Maurice; Le Calvé, Stéphane

    2015-01-01

    Most of Polycyclic Aromatic Hydrocarbons (PAHs) are associated to airborne particles and their health impact depends on the particle size where they are bound. This work aims to develop a high sensitive analytical technique to quantify particulate PAHs sampled with a 3-stages cascade impactor in order to derive simultaneously their individual concentration in PM1, PM2.5 and PM10. Three key steps of the method were evaluated separately in order to avoid any PAHs loss during the global sample preparation procedure: (1) the accelerated solvent extraction of PAHs from the filter; (2) the primary concentration of the extract until 1 mL by means of a rotary evaporator at 45°C and 220 mbar and (3) the final concentration of the pre-concentrated extract to about 100-150 µL under a gentle nitrogen stream. Each recovery experiment was realized in triplicates. All these steps evaluated independently show that the overall PAHs loss, even for those with a low molecular weight, should not exceed more than a few percent. Extracts were then analyzed by using a HPLC coupled to fluorescence and Diode Array Detectors with the external standard method. The resulting calibration curves containing between 9 and 12 points were plotted in the concentration range of 0.05-45 µg L(-1) for most of the 16 US-EPA priority PAHs and were fully linear (R(2)>0.999). Limits Of Quantification were in the range 0.05-0.47 µg L(-1) corresponding to 0.75-7.05 pg m(-3) for 20 m(3) of pumped air. Finally, taking into account the average PAHs concentrations previously reported in typical European indoor environments, and considering the use of a 3-stages cascade impactor to collect simultaneously PM>10 µm, 2.5 µmsampling duration was estimated to 20-40 h for a sampling flow fixed to 0.5m(3)h(-1). PMID:25281119

  18. Leaf tissue sampling and DNA extraction protocols.

    Science.gov (United States)

    Semagn, Kassa

    2014-01-01

    Taxonomists must be familiar with a number of issues in collecting and transporting samples using freezing methods (liquid nitrogen and dry ice), desiccants (silica gel and blotter paper), and preservatives (CTAB, ethanol, and isopropanol), with each method having its own merits and limitations. For most molecular studies, a reasonably good quality and quantity of DNA is required, which can only be obtained using standard DNA extraction protocols. There are many DNA extraction protocols that vary from simple and quick ones that yield low-quality DNA but good enough for routine analyses to the laborious and time-consuming standard methods that usually produce high quality and quantities of DNA. The protocol to be chosen will depend on the quality and quantity of DNA needed, the nature of samples, and the presence of natural substances that may interfere with the extraction and subsequent analysis. The protocol described in this chapter has been tested for extracting DNA from eight species and provided very good quality and quantity of DNA for different applications, including those genotyping methods that use restriction enzymes. PMID:24415469

  19. Air Sampling Instruments for Evaluation of Atmospheric Contaminants. Fourth Edition.

    Science.gov (United States)

    American Conference of Governmental Industrial Hygienists, Cincinnati, OH.

    This text, a revision and extension of the first three editions, consists of papers discussing the basic considerations in sampling air for specific purposes, sampler calibration, systems components, sample collectors, and descriptions of air-sampling instruments. (BT)

  20. Improvement of the equipment for air sampling and enriching air samples with radionuclides

    International Nuclear Information System (INIS)

    The air liquefaction and cryogenic distillation methods were used to inverse the concentration of gaseous radionuclides in the air samples. For this purpose the air liquefaction equipment ZIF-1002 was applied. Gaseous radionuclides which liquefy at the temperature higher than -200 degrees Celsius are concentrated in liquid oxygen. In the work an equipment model allowing to increase the volume of pumping and the liquefied air 2-3 times by ZIF is proposed. For this purpose an air drying and preliminary cooling equipment were constructed, and a pump was applied. Having shortened the sampling time, it became possible to measure the volumetric activity of short-lived radionuclides in the environment of their sources. The activity of 131J, 41Ar, krypton and xenon radioisotope is measured in liquid oxygen in a special disk. For determining tritium volumetric activity, samples of air humidity (water) or a mixture of hydrogen and other undissolved gases are taken and finally prepared in the laboratory. For 14C sampling, a special equipment allowing to obtain about 60 I of CO2 gas per day was constructed. The ZIF-1002 equipment with supplements was installed in a car and in a container. Using the refrigerating unit MVT-20-1-0, a fresh water cooling system of the ZIF was constructed. The equipment was tested on land and sea. (author)

  1. Phenolic-Compound-Extraction Systems for Fruit and Vegetable Samples

    Directory of Open Access Journals (Sweden)

    Antonio Segura-Carretero

    2010-12-01

    Full Text Available This paper reviews the phenolic-compound-extraction systems used to analyse fruit and vegetable samples over the last 10 years. Phenolic compounds are naturally occurring antioxidants, usually found in fruits and vegetables. Sample preparation for analytical studies is necessary to determine the polyphenolic composition in these matrices. The most widely used extraction system is liquid-liquid extraction (LLE, which is an inexpensive method since it involves the use of organic solvents, but it requires long extraction times, giving rise to possible extract degradation. Likewise, solid-phase extraction (SPE can be used in liquid samples. Modern techniques, which have been replacing conventional ones, include: supercritical fluid extraction (SFE, pressurized liquid extraction (PLE, microwave-assisted extraction (MAE and ultrasound-assisted extraction (UAE. These alternative techniques reduce considerably the use of solvents and accelerate the extraction process.

  2. A RAPID DNA EXTRACTION METHOD FOR PCR IDENTIFICATION OF FUNGAL INDOOR AIR CONTAMINANTS

    Science.gov (United States)

    Following air sampling, fungal DNA needs to be extracted and purified to a state suitable for laboratory use. Our laboratory has developed a simple method of extraction and purification of fungal DNA appropriate for enzymatic manipulation and polymerase chain reaction (PCR) appli...

  3. Antimicrobial potentials of different solvent extracted samples from Physalis ixocarpa.

    Science.gov (United States)

    Khan, Wajid; Bakht, Jehan; Shafi, Mohammad

    2016-03-01

    The present study investigates the antimicrobial activities of different solvent extracted samples isolated from different parts of Physalis ixocarpa through disc diffusion assay using three different concentrations. Statistical analysis of the data revealed that different parts of the plant showed varying degree of inhibition against different bacteria at different concentrations. Different solvent extracted samples from the calyx showed inhibitory activity against most of the bacteria under study. Extracts from leaf and fruit samples showed activity against S. aureus and K. pneumoniae and extracts from the stem tissues were effective to control the growth of E. coli and K. pneumoniae. Crude methanolic extract from the stem and n-butanol extracted samples from fruit exhibited strong inhibitory activity against Klebsiella pneumoniae at highest concentrations. Antifungal activity was observed only in crude methanol extract from the leaf against Rhizopus stolinifer, Aspergillus niger and Penicillium chrysogenum. PMID:27087074

  4. Fatal venous air embolism in a cat undergoing dental extractions.

    Science.gov (United States)

    Gunew, M; Marshall, R; Lui, M; Astley, C

    2008-11-01

    A five-year-old domestic shorthair cat underwent general anaesthesia and tooth extractions. Immediately after use of a high-speed, air-driven, water-cooled dental drill, the cat suffered cardiac arrest and attempted resuscitation was unsuccessful. Post-mortem radiographs showed air in the vena cava, right atrium, right auricle and right ventricle, hepatic and renal veins. These findings were confirmed at post-mortem examination. The cause of death was massive air embolism. There are reports of fatal venous air embolism in the human literature from the use of high-speed, air-driven, water-cooled dental drills. In this case, we believe that the air jet from the cooling system provided an enormous pressure gradient allowing air entry through an alveolar bone fracture or the inflamed gingival tissues. This is the first report of fatal venous air embolism associated with the use of a high-speed dental drill in the veterinary literature. PMID:19006491

  5. 40 CFR 761.292 - Chemical extraction and analysis of individual samples and composite samples.

    Science.gov (United States)

    2010-07-01

    ....61(a)(6) § 761.292 Chemical extraction and analysis of individual samples and composite samples. Use... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Chemical extraction and analysis of individual samples and composite samples. 761.292 Section 761.292 Protection of Environment...

  6. UNLABELED SELECTED SAMPLES IN FEATURE EXTRACTION FOR CLASSIFICATION OF HYPERSPECTRAL IMAGES WITH LIMITED TRAINING SAMPLES

    Directory of Open Access Journals (Sweden)

    A. Kianisarkaleh

    2015-12-01

    Full Text Available Feature extraction plays a key role in hyperspectral images classification. Using unlabeled samples, often unlimitedly available, unsupervised and semisupervised feature extraction methods show better performance when limited number of training samples exists. This paper illustrates the importance of selecting appropriate unlabeled samples that used in feature extraction methods. Also proposes a new method for unlabeled samples selection using spectral and spatial information. The proposed method has four parts including: PCA, prior classification, posterior classification and sample selection. As hyperspectral image passes these parts, selected unlabeled samples can be used in arbitrary feature extraction methods. The effectiveness of the proposed unlabeled selected samples in unsupervised and semisupervised feature extraction is demonstrated using two real hyperspectral datasets. Results show that through selecting appropriate unlabeled samples, the proposed method can improve the performance of feature extraction methods and increase classification accuracy.

  7. Phenolic-Compound-Extraction Systems for Fruit and Vegetable Samples

    OpenAIRE

    Antonio Segura-Carretero; Alberto Fernández-Gutiérrez; Patricia Garcia-Salas; Aranzazu Morales-Soto

    2010-01-01

    This paper reviews the phenolic-compound-extraction systems used to analyse fruit and vegetable samples over the last 10 years. Phenolic compounds are naturally occurring antioxidants, usually found in fruits and vegetables. Sample preparation for analytical studies is necessary to determine the polyphenolic composition in these matrices. The most widely used extraction system is liquid-liquid extraction (LLE), which is an inexpensive method since it involves the use of organic solvents, but ...

  8. Air sparging and soil vapor extraction to remediate ground water

    International Nuclear Information System (INIS)

    An Air Sparging and Soil Vapor Extraction System was chosen to remediate petroleum impacted ground water over traditional remedial alternatives, such as ''pump and treat'', to expedite site closure. Field pilot testing, computer modeling and cost benefit analyses performed for several alternatives. Air Sparging and Soil Vapor Extraction pilot studies proved this technology to be the most effective with respect to remedial and economic concerns. Underground Storage Tanks (USTs) were closed at the facility located in North Eastern North Carolina in August of 1992. During UST closure, petroleum impacted ground water and soils were encountered. ATEC performed a Comprehensive Site assessment to delineate the impacted soil and ground water plume. Following completion of the site assessment, a Corrective Action Plan was prepared. As part of the Corrective Action Plan preparation, field pilot testing was performed to evaluate remedial alternatives and provide information for full scale design. The full scale treatment system was installed and started in January 1994. This effective Remedial System was selected over other options due to successful pilot testing results with site closure petitioning scheduled within 12 to 14 months after start up. The Air Sparging System, properly applied, is an effective and ''quick'' remedial option with no generation of ground water for disposal and permitting. This paper concentrates on the Air Sparging application applied at this North Carolina site. Although Vapor extraction was also implemented, this presentation does not elaborate on vapor extraction design or implementation and only discusses vapor extraction where it is directly related to the Air Sparging System

  9. Structural effects of sample ageing in hydrocracked coal liquefaction extracts

    Energy Technology Data Exchange (ETDEWEB)

    Begon, V.; Suelves, I.; Herod, A.A.; Dugwell, D.R.; Kandiyoti, R. [Imperial College, London (United Kingdom). Dept. of Chemical Engineering and Chemical Technology

    2000-10-01

    A sample of Point of Ayr coal extract has been hydrocracked in a microbomb reactor with NiMo on alumina catalyst in tetralin as solvent and hydrogen donor and under hydrogen pressure. The product was separated from solvent and catalyst and then split into equal parts and stored either under nitrogen atmosphere in a freezer or in air at room temperature. Samples of the products were examined at 2 h frequencies for a day, then daily for a week, then at less frequent intervals for a year. Methods used for examination were size exclusion chromatography (SEC) and UV fluorescence spectroscopy (UV-F), both using 1-methyl-2-pyrrolidinone as solvent. Aging was assessed in terms of shifts to shorter elution times in SEC and parallel changes in UV-F spectra. Both stored products showed significant structural evidence of aging over the first week of storage. After that time, changes observed were within the range of variability of the chromatography method based on polystyrene standards. The aging was attributed to the presence of low-reactivity free radicals species, which underwent recombination reactions during storage. These changes are likely to affect the viscosity and combustion characteristics of the hydrocracked product. 30 refs., 6 figs., 1 tab.

  10. Solubility testing of actinides on breathing-zone and area air samples

    Energy Technology Data Exchange (ETDEWEB)

    Metzger, R.L.; Jessop, B.H.; McDowell, B.L. [Radiation Safety Engineering, Inc., Chandler, AZ (United States)

    1996-02-01

    A solubility testing method for several common actinides has been developed with sufficient sensitivity to allow profiles to be determined from routine breathing zone and area air samples in the workplace. Air samples are covered with a clean filter to form a filter-sample-filter sandwich which is immersed in an extracellular lung serum simulant solution. The sample is moved to a fresh beaker of the lung fluid simulant each day for one week, and then weekly until the end of the 28 day test period. The soak solutions are wet ashed with nitric acid and hydrogen peroxide to destroy the organic components of the lung simulant solution prior to extraction of the nuclides of interest directly into an extractive scintillator for subsequent counting on a Photon-Electron Rejecting Alpha Liquid Scintillation (PERALS{reg_sign}) spectrometer. Solvent extraction methods utilizing the extractive scintillators have been developed for the isotopes of uranium, plutonium, and curium. The procedures normally produce an isotopic recovery greater than 95% and have been used to develop solubility profiles from air samples with 40 pCi or less of U{sub 3}O{sub 8}. Profiles developed for U{sub 3}O{sub 8} samples show good agreement with in vitro and in vivo tests performed by other investigators on samples from the same uranium mills.

  11. Solubility testing of actinides on breathing-zone and area air samples

    International Nuclear Information System (INIS)

    A solubility testing method for several common actinides has been developed with sufficient sensitivity to allow profiles to be determined from routine breathing zone and area air samples in the workplace. Air samples are covered with a clean filter to form a filter-sample-filter sandwich which is immersed in an extracellular lung serum simulant solution. The sample is moved to a fresh beaker of the lung fluid simulant each day for one week, and then weekly until the end of the 28 day test period. The soak solutions are wet ashed with nitric acid and hydrogen peroxide to destroy the organic components of the lung simulant solution prior to extraction of the nuclides of interest directly into an extractive scintillator for subsequent counting on a Photon-Electron Rejecting Alpha Liquid Scintillation (PERALS reg-sign) spectrometer. Solvent extraction methods utilizing the extractive scintillators have been developed for the isotopes of uranium, plutonium, and curium. The procedures normally produce an isotopic recovery greater than 95% and have been used to develop solubility profiles from air samples with 40 pCi or less of U3O8. Profiles developed for U3O8 samples show good agreement with in vitro and in vivo tests performed by other investigators on samples from the same uranium mills

  12. Acid Release from an Acid Sulfate Soil Sample Under Successive Extractions with Different Extractants

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    An acid sulfate soil sample was successively extracted with deionized water, 1 mol L-1 KCI and 0.000 5 mol L-1 Ca(OH)2 solutions. The results showed that only very small amounts of acidity were extracted by deionized water, possibly through slow jarosite hydrolysis. Acid release through jarosite hydrolysis was greatly enhanced by Ca(OH)2 extraction at the expense of the added OH- being neutralized by the acid released. Successive extraction of the sample with KCI removed the largest amounts of acidity from the sample. However, it is likely that the major form of acidity released by KC1 extraction was exchangeable acidity. The results also show the occurrence of low or non charged A1 and Fe species in water and Ca(OH)2 extracts after first a few extractions. It appears that such a phenomenon was related to a decreasing EC value with increasing number of extractions.

  13. Workplace air monitoring and sampling practices at DOE facilities

    International Nuclear Information System (INIS)

    The Pacific Northwest Laboratory (PNL) surveyed the current air monitoring and sampling practices at U.S. Department of Energy (DOE) facilities as a part of an air monitoring upgrade task. A comprehensive questionnaire was developed and distributed to DOE contractors through the DOE field offices. Twenty-six facilities returned a completed questionnaire. Questionnaire replies indicate a large diversity in air sampling and monitoring practices among DOE facilities. The differences among the facilities exist in monitoring and sampling instrumentation, procedures, calibration, analytical methods, detection levels, and action levels. Many of these differences could be attributed to different operational needs. 5 references, 2 figures, 2 tables

  14. Preparation of protein samples for gel electrophoresis by sequential extraction

    Institute of Scientific and Technical Information of China (English)

    钟伯雄; 翁宏飚; 等

    2002-01-01

    Since preparation and solubilization of protein samples are crucial factors in proteome research,the authors established a sequential extraction technique to prepare protein samples from the body wall of the 5th instar larvae of silkworm.Bombyx mori.Two kinds of protein samples were obtained from the body wall using the method.Between the two types of samples only about 15% proteins were identical;the majority were different,indicating that more species of proteins could be obtained with the sequential extraction method;which will be useful for preparation of protein samples for proteome study.

  15. EML Surface Air Sampling Program, 1990--1993 data

    International Nuclear Information System (INIS)

    Measurements of the concentrations of specific atmospheric radionuclides in air filter samples collected for the Environmental Measurements Laboratory's Surface Air Sampling Program (SASP) during 1990--1993, with the exception of April 1993, indicate that anthropogenic radionuclides, in both hemispheres, were at or below the lower limits of detection for the sampling and analytical techniques that were used to collect and measure them. The occasional detection of 137Cs in some air filter samples may have resulted from resuspension of previously deposited debris. Following the April 6, 1993 accident and release of radionuclides into the atmosphere at a reprocessing plant in the Tomsk-7 military nuclear complex located 16 km north of the Siberian city of Tomsk, Russia, weekly air filter samples from Barrow, Alaska; Thule, Greenland and Moosonee, Canada were selected for special analyses. The naturally occurring radioisotopes that the authors measure, 7Be and 210Pb, continue to be detected in most air filter samples. Variations in the annual mean concentrations of 7Be at many of the sites appear to result primarily from changes in the atmospheric production rate of this cosmogenic radionuclide. Short-term variations in the concentrations of 7Be and 210Pb continued to be observed at many sites at which weekly air filter samples were analyzed. The monthly gross gamma-ray activity and the monthly mean surface air concentrations of 7Be, 95Zr, 137Cs, 144Ce, and 210Pb measured at sampling sites in SASP during 1990--1993 are presented. The weekly mean surface air concentrations of 7Be, 95Zr, 137Cs, 144Ce, and 210Pb for samples collected during 1990--1993 are given for 17 sites

  16. EML Surface Air Sampling Program, 1990--1993 data

    Energy Technology Data Exchange (ETDEWEB)

    Larsen, R.J.; Sanderson, C.G.; Kada, J.

    1995-11-01

    Measurements of the concentrations of specific atmospheric radionuclides in air filter samples collected for the Environmental Measurements Laboratory`s Surface Air Sampling Program (SASP) during 1990--1993, with the exception of April 1993, indicate that anthropogenic radionuclides, in both hemispheres, were at or below the lower limits of detection for the sampling and analytical techniques that were used to collect and measure them. The occasional detection of {sup 137}Cs in some air filter samples may have resulted from resuspension of previously deposited debris. Following the April 6, 1993 accident and release of radionuclides into the atmosphere at a reprocessing plant in the Tomsk-7 military nuclear complex located 16 km north of the Siberian city of Tomsk, Russia, weekly air filter samples from Barrow, Alaska; Thule, Greenland and Moosonee, Canada were selected for special analyses. The naturally occurring radioisotopes that the authors measure, {sup 7}Be and {sup 210}Pb, continue to be detected in most air filter samples. Variations in the annual mean concentrations of {sup 7}Be at many of the sites appear to result primarily from changes in the atmospheric production rate of this cosmogenic radionuclide. Short-term variations in the concentrations of {sup 7}Be and {sup 210}Pb continued to be observed at many sites at which weekly air filter samples were analyzed. The monthly gross gamma-ray activity and the monthly mean surface air concentrations of {sup 7}Be, {sup 95}Zr, {sup 137}Cs, {sup 144}Ce, and {sup 210}Pb measured at sampling sites in SASP during 1990--1993 are presented. The weekly mean surface air concentrations of {sup 7}Be, {sup 95}Zr, {sup 137}Cs, {sup 144}Ce, and {sup 210}Pb for samples collected during 1990--1993 are given for 17 sites.

  17. Tritium monitoring in air, optimization of a sampling method

    International Nuclear Information System (INIS)

    An air humidity sampling method using dry silica gel and its application to tritium activity concentration monitoring in air humidity are described. The method was used to monitor tritium in the surroundings of Czech nuclear power plants. The problem of elimination of cross-contamination is discussed

  18. Droplet-Based Segregation and Extraction of Concentrated Samples

    Energy Technology Data Exchange (ETDEWEB)

    Buie, C R; Buckley, P; Hamilton, J; Ness, K D; Rose, K A

    2007-02-23

    Microfluidic analysis often requires sample concentration and separation techniques to isolate and detect analytes of interest. Complex or scarce samples may also require an orthogonal separation and detection method or off-chip analysis to confirm results. To perform these additional steps, the concentrated sample plug must be extracted from the primary microfluidic channel with minimal sample loss and dilution. We investigated two extraction techniques; injection of immiscible fluid droplets into the sample stream (''capping'''') and injection of the sample into an immiscible fluid stream (''extraction''). From our results we conclude that capping is the more effective partitioning technique. Furthermore, this functionality enables additional off-chip post-processing procedures such as DNA/RNA microarray analysis, realtime polymerase chain reaction (RT-PCR), and culture growth to validate chip performance.

  19. Solid waste transuranic storage and assay facility indoor air sampling

    Energy Technology Data Exchange (ETDEWEB)

    Pingel, L.A., Westinghouse Hanford

    1996-08-20

    The purpose of the study is to collect and analyze samples of the indoor air at the Transuranic Storage and Assay Facility (TRUSAF), Westinghouse Hanford. A modified US EPA TO-14 methodology, using gas chromatography/mass spectrography, may be used for the collection and analysis of the samples. The information obtained will be used to estimate the total release of volatile organic compounds from TRUSAF to determine the need for air emmission permits.

  20. Presence of organophosphorus pesticide oxygen analogs in air samples

    OpenAIRE

    Armstrong, Jenna L.; Fenske, Richard A; Yost, Michael G.; Galvin, Kit; Tchong-French, Maria; Yu, Jianbo

    2013-01-01

    A number of recent toxicity studies have highlighted the increased potency of oxygen analogs (oxons) of several organophosphorus (OP) pesticides. These findings were a major concern after environmental oxons were identified in environmental samples from air and surfaces following agricultural spray applications in California and Washington State. This paper reports on the validity of oxygen analog measurements in air samples for the OP pesticide, chlorpyrifos. Controlled environmental and lab...

  1. Efficiency of dust sampling inlets in calm air.

    Science.gov (United States)

    Breslin, J A; Stein, R L

    1975-08-01

    Measurement of airborne dust concentrations usually involves drawing a sample of the dust-laden air into the measuring instrument through an inlet. Even if the surrounding air is calm, theoretical calculations predict that large particles may not be sampled accurately due to the combined effects of gravity and inertia on the particles near the sampling inlet. Tests were conducted to determine the conditions of particle size, inlet radius, and flow rare necessary for accurate dust sampling. A coal-dust aerosol was sampled simultaneously through inlets of different diameters at the same volume flow-rate and collected on filters. The dust was removed from the filters and the particles were counted and sized with a Coulter counter. Results showed that published criteria for inlet conditions for correct sampling are overly restrictive and that respirable-size particles are sampled correctly in the normal range or operation of most dust sampling instruments. PMID:1227283

  2. Recent development in uranium mining air sampling programs

    International Nuclear Information System (INIS)

    Licensees planning to operate in-situ uranium mining facilities must demonstrate compliance with USNRC Regulatory Guide 4.14 regarding the facility's impact on the local ambient air quality. Regulatory compliance includes a pre-operational baseline study with a subsequent operational air monitoring program. Compliance with the air monitoring requirements is being aided by utilization of advanced-technology AC/DC air sampling systems operable from batteries charged by solar power or wind turbine systems. These modern air sampling systems employ low power brushless motors, automatic flow control, in addition to normalization of flow rates and volumes to a standard temperature and pressure. These high tech features enable a licensee to demonstrate more accurately compliance with the MDA requirements of Req. Guide 4.14 for specific isotopes of Th, Ra, Pb and U.

  3. The comparison of pollen abundance in air and honey samples

    Directory of Open Access Journals (Sweden)

    Ingrida Šaulienė

    2015-12-01

    Full Text Available Honey as a food has long been used in human nutrition and is still popular. Honey is important because of its therapeutic, prophylactic and strengthening value. Pollen is one of the most decisive components that ensure the quality and type of honey. Modern society becomes more and more sensitive to airborne pollen. Therefore, it is crucial to determine the composition of allergenic plant pollen in natural honey. For this purpose, we studied and compared pollen abundance in honey and air samples collected in Lithuania. Standard methods for pollen investigation in air and honey were used in this study. The botanical diversity of pollen identified in honey and air samples indicates 10 morphotypes: 8 of woody plants and 2 of herbaceous plants, in both the honey and air samples. Salix pollen counts in the honey were found to be highest among airborne pollen from May to September. The anemophilous allergenic pollen constituted 44 % of the total pollen detected in the honey.

  4. Determination of radiocarbon in stratospheric CO2, obtained through AirCore sampling.

    Science.gov (United States)

    Paul, Dipayan; Chen, Huilin; Been, Henk A.; Kivi, Rigel; Meijer, Harro A. J.

    2016-04-01

    The concentration of Greenhouse Gases (GHG), with carbon dioxide as the most prominent example, has been and still is increasing, predominantly due to emissions from fossil fuel combustion. CO2 is also the most important component of the global carbon cycle. Among other tracers, radiocarbon (Carbon-14) is a unique and an important atmospheric tracer used in the understanding of the global carbon cycle. Radiocarbon is a naturally occurring isotope (radioactive, t 1/2 = 5730 ± 40 years) of carbon produced through the interaction of thermalized neutrons and nitrogen in the upper atmosphere. Generally, for performing atmospheric radiocarbon measurements in the higher atmosphere, large samples (few liters of air) were collected using aircrafts and balloons. However, collecting stratospheric samples on a regular basis for radiocarbon analysis is extremely expensive. Here we describe the determination of radiocarbon concentrations in stratospheric CO2, collected using AirCore sampling. AirCore is an innovative sampling technique for obtaining vertical atmospheric profiles and, in Europe, is done on a regular basis at Sodankylä, Finland for CO2, CH4 and CO. The stratospheric parts of two such AirCore profiles were used in this study as a proof-of-principle. CO2 from the stratospheric air samples were extracted and converted to elemental carbon, which were then measured at the Accelerator Mass Spectrometric (AMS) facility of the Centre for Isotope Research (CIO) at the University of Groningen. The stratospheric part of the AirCore profile was divided into six sections, each contained approximately 10 μg C. A detailed description of the extraction, graphitization, AMS analysis and the derivation of the stratospheric radiocarbon profile will be the main focus. Through our results, we will show that AirCore is a viable sampling method for performing high-precision radiocarbon measurements of stratospheric CO2 with reasonably good spatial resolution on a regular basis

  5. CARBONIZED FIBROUS RESIN AS A NEW SORBENT FOR SAMPLING POLYCYCLIC AROMATIC HYDROCARBONS (PAHS) IN AMBIENT AIR

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    A new sampling method of ambient air analysis using carbonized fibrous resin as asorbent for polycyclic aromatic hydrocarbons (PAHs) was reported.The physical and chemical properties of the carbonized fibrous resins were measured. Thesample pretreatment with ultrasonic extraction and subsequent clean-up ehition through a silica gelcolumn was optimized. The suitable ultrasonic extraction conditions were selected as follows: resinweight was 1.5 g, ultrasonic extraction time 20 min, volume of extraction solvent 100 mi andextraction operation times 2~3. The concentrated extractable organic matter was submitted to nextstep of clean-up procedure of adsorption chromatography on silica gel column/n-hexane and amixture of dichloromethene:n-hexane solution 2:3 (v/v). The PAHs fractions in the real samplesfrom Changzhou, China were particularly analyzed using GC-MS data system and the data of massspectra, retention times and scan numbers of the real samples were compared with that of thestandards of 16 PAHs listed by the US EPA as "priority pollutants" of the environment. Theanalysis of the real samples indicates that the carbonized fibrous resin is a good sorbent. Thepretreatment of samples of ambient air with carbonized fibrous resin as a sorbent for P,AHs isproved to be reliable and might be used for the procedure of the determination of PAHs inatmospheric environment.

  6. Passive sampling of polychlorinated biphenyls (PCB) in indoor air

    DEFF Research Database (Denmark)

    Vorkamp, Katrin; Mayer, Philipp

    PCBs were widely used in construction materials in the 1906s and 1970s, a period of high building activity in Denmark. The objective of this study was therefore to use passive sampling techniques to develop a simple and cost-effective screening tool for PCBs in indoor air. The study proceeded in...... three phases combining a literature review, laboratory experiments and measurements in buildings potentially containing PCBs in indoor air. The laboratory experiments showed a strong influence of air velocity on the PCB partitioning between air and the passive sampler. Based on the results of the first...... two phases and comments from experts in the field of PCB containing construction materials, a kinetic sampler (petri dish with silicone) and a potential equilibrium sampler (silicone-coated paper) were tested in buildings. Calibration and validation were based on conventional active sampling, for both...

  7. Direct analysis of air filter samples for alpha emitting isotopes

    International Nuclear Information System (INIS)

    The traditional method for determination of alpha emitting isotopes on air filters has been to process the samples by radiochemical methods. However, this method is too slow for cases of incidents involving radioactive materials where the determination of personnel received dose is urgent. A method is developed to directly analyze the air filters taken from personal and area air monitors. The site knowledge is used in combination with alpha spectral information to identify isotopes. A mathematical function is developed to estimate the activity for each isotope. The strengths and weaknesses of the method are discussed

  8. Air Monitoring: New Advances in Sampling and Detection

    Directory of Open Access Journals (Sweden)

    Nicola Watson

    2011-01-01

    Full Text Available As the harmful effects of low-level exposure to hazardous organic air pollutants become more evident, there is constant pressure to improve the detection limits of indoor and ambient air monitoring methods, for example, by collecting larger air volumes and by optimising the sensitivity of the analytical detector. However, at the other end of the scale, rapid industrialisation in the developing world and growing pressure to reclaim derelict industrial land for house building is driving the need for air monitoring methods that can reliably accommodate very-high-concentration samples in potentially aggressive matrices. This paper investigates the potential of a combination of two powerful gas chromatography—based analytical enhancements—sample preconcentration/thermal desorption and time-of-flight mass spectrometry—to improve quantitative and qualitative measurement of very-low-(ppt level organic chemicals, even in the most complex air samples. It also describes new, practical monitoring options for addressing equally challenging high-concentration industrial samples.

  9. Sampling density for the quantitative evaluation of air trapping

    Energy Technology Data Exchange (ETDEWEB)

    Goris, Michael L. [Stanford University School of Medicine, Division of Nuclear Medicine, Stanford, CA (United States); Robinson, Terry E. [Stanford University School of Medicine, Center of Excellence in Pulmonary Biology, Pulmonary Division, Department of Pediatrics, Stanford, CA (United States)

    2009-03-15

    Concerns have been expressed recently about the radiation burden on patient populations, especially children, undergoing serial radiological testing. To reduce the dose one can change the CT acquisition settings or decrease the sampling density. In this study we determined the minimum desirable sampling density to ascertain the degree of air trapping in children with cystic fibrosis. Ten children with cystic fibrosis in stable condition underwent a volumetric spiral CT scan. The degree of air trapping was determined by an automated algorithm for all slices in the volume, and then for 1/2, 1/4, to 1/128 of all slices, or a sampling density ranging from 100% to 1% of the total volume. The variation around the true value derived from 100% sampling was determined for all other sampling densities. The precision of the measurement remained stable down to a 10% sampling density, but decreased markedly below 3.4%. For a disease marker with the regional variability of air trapping in cystic fibrosis, regardless of observer variability, a sampling density below 10% and even more so, below 3.4%, apparently decreases the precision of the evaluation. (orig.)

  10. Sampling density for the quantitative evaluation of air trapping

    International Nuclear Information System (INIS)

    Concerns have been expressed recently about the radiation burden on patient populations, especially children, undergoing serial radiological testing. To reduce the dose one can change the CT acquisition settings or decrease the sampling density. In this study we determined the minimum desirable sampling density to ascertain the degree of air trapping in children with cystic fibrosis. Ten children with cystic fibrosis in stable condition underwent a volumetric spiral CT scan. The degree of air trapping was determined by an automated algorithm for all slices in the volume, and then for 1/2, 1/4, to 1/128 of all slices, or a sampling density ranging from 100% to 1% of the total volume. The variation around the true value derived from 100% sampling was determined for all other sampling densities. The precision of the measurement remained stable down to a 10% sampling density, but decreased markedly below 3.4%. For a disease marker with the regional variability of air trapping in cystic fibrosis, regardless of observer variability, a sampling density below 10% and even more so, below 3.4%, apparently decreases the precision of the evaluation. (orig.)

  11. Sampling frequency guidance for ambient air toxics monitoring.

    Science.gov (United States)

    Bortnick, Steven M; Stetzer, Shannon L

    2002-07-01

    The U.S. Environmental Protection Agency (EPA) is in the process of designing a national network to monitor hazardous air pollutants (HAPs), also known as air toxics. The purposes of the expanded monitoring are to (1) characterize ambient concentrations in representative areas; (2) provide data to support and evaluate dispersion and receptor models; and (3) establish trends and evaluate the effectiveness of HAP emission reduction strategies. Existing air toxics data, in the form of an archive compiled by EPA's Office of Air Quality Planning and Standards (OAQPS), are used in this paper to examine the relationship between estimated annual average (AA) HAP concentrations and their associated variability. The goal is to assess the accuracy, or bias and precision, with which the AA can be estimated as a function of ambient concentration levels and sampling frequency. The results suggest that, for several air toxics, a sampling schedule of 1 in 3 days (1:3) or 1:6 days maybe appropriate for meeting some of the general objectives of the national network, with the more intense sampling rate being recommended for areas expected to exhibit relatively high ambient levels. PMID:12139351

  12. Extraction of Eleven Polycyclic Aromatic Hydrocarbons in Water Samples

    Directory of Open Access Journals (Sweden)

    W. Kanchanamayoon

    2009-01-01

    Full Text Available Eleven polycyclic aromatic hydrocarbons namely; naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[b]fluoranthene, benzo[a]pyrene and benzo[ghi]perylene were extracted simultaneously by solid phase and analysis by gas chromatograph. The LC-18 solid phase showed good recoveries for extraction of 11 PAHs by using 3 mL of the mixture of (1:1:1 dichloromethane: cyclohexane: hexane as eluent, the percentage recoveries were in the ranges of 84.31-97.38 with the standard deviation of 1.56-5.36. The detection limits for solid phase extraction were in the ranges of 0.06-0.55 ppm. Application for analysis of water samples were done by this technique. The concentration of PAHs in water samples were found slightly varied from the location. The advantages of solid phase are solvent consumption, reuse in several times and pre-concentration.

  13. Some observations on the results of personal air samples

    International Nuclear Information System (INIS)

    Results of personal air samples taken in plutonium and uranium handling areas at Harwell Laboratory during 1986 were examined on a statistical basis. The distribution of concentrations shown by samples is of log-normal form, and similar in all plutonium handling areas in having a median concentration of 0.026 DAC and a geometric standard deviation of ∼6.0. A computer program was used to demonstrate large variation in sample results could be wholly due to statistics of sampling radioactive particles at very low concentration. This variation would mask all but the largest changes due to other causes (e.g. different work methods or ventilation patterns). In uranium handling areas particle sampling statistics do not play an important part in variation between samples as the concentration of particles is high. The geometric standard deviation of the samples was 3.5 and attributable to changes in work, work methods or ventilation patterns. Radiometric analysis of the personal air samples is discussed. Errors due to counting statistics are considered to be relatively small compared with other sources of sample variation. (author)

  14. Polycyclic aromatic hydrocarbons in air samples of meat smokehouses

    DEFF Research Database (Denmark)

    Hansen, Åse Marie; Olsen, I L; Poulsen, O M

    In a screening programme nine Danish meat smokehouses were randomly selected for measurements on concentration of airborne polycyclic aromatic hydrocarbons (PAH). A total of 23 stationary air samples were collected during the entire working period of the kiln either above the kiln doors or...

  15. Optimal Media for Use in Air Sampling To Detect Cultivable Bacteria and Fungi in the Pharmacy

    OpenAIRE

    Weissfeld, Alice S.; Joseph, Riya Augustin; Le, Theresa V.; Trevino, Ernest A.; Schaeffer, M. Frances; Vance, Paula H.

    2013-01-01

    Current guidelines for air sampling for bacteria and fungi in compounding pharmacies require the use of a medium for each type of organism. U.S. Pharmacopeia (USP) chapter (http://www.pbm.va.gov/linksotherresources/docs/USP797PharmaceuticalCompoundingSterileCompounding.pdf) calls for tryptic soy agar with polysorbate and lecithin (TSApl) for bacteria and malt extract agar (MEA) for fungi. In contrast, the Controlled Environment Testing Association (CETA), the professional organization for in...

  16. Development and calibration of real-time PCR for quantification of airborne microorganisms in air samples

    Science.gov (United States)

    An, Hey Reoun; Mainelis, Gediminas; White, Lori

    This manuscript describes the coupling of bioaerosol collection and the use of real-time PCR (RT-PCR) to quantify the airborne bacteria. The quantity of collected bacteria determined by RT-PCR is compared with conventional quantification techniques, such as culturing, microscopy and airborne microorganism counting by using optical particle counter (OPC). Our data show that an experimental approach used to develop standard curves for use with RT-PCR is critical for accurate sample quantification. Using universal primers we generated 12 different standard curves which were used to quantify model organism Escherichia coli (Migula) Catellani from air samples. Standard curves prepared using a traditional approach, where serially diluted genomic DNA extracted from pure cultured bacteria were used in PCR reaction as a template DNA yielded significant underestimation of sample quantities compared to airborne microorganism concentration as measured by an OPC. The underestimation was especially pronounced when standard curves were built using colony forming units (CFUs). In contrast, the estimate of cell concentration in an air sample by RT-PCR was more accurate (˜60% compared to the airborne microorganism concentration) when the standard curve was built using aerosolized E. coli. The accuracy improved even further (˜100%) when air samples used to build the standard curves were diluted first, then the DNA extracted from each dilution was amplified by the RT-PCR—to mimic the handling of air samples with unknown and possibly low concentration. Therefore, our data show that standard curves used for quantification by RT-PCR needs to be prepared using the same environmental matrix and procedures as handling of the environmental sample in question. Reliance on the standard curves generated with cultured bacterial suspension (a traditional approach) may lead to substantial underestimation of microorganism quantities in environmental samples.

  17. Methods for Sampling and Measurement of Compressed Air Contaminants

    Energy Technology Data Exchange (ETDEWEB)

    Stroem, L.

    1976-10-15

    In order to improve the technique for measuring oil and water entrained in a compressed air stream, a laboratory study has been made of some methods for sampling and measurement. For this purpose water or oil as artificial contaminants were injected in thin streams into a test loop, carrying dry compressed air. Sampling was performed in a vertical run, down-stream of the injection point. Wall attached liquid, coarse droplet flow, and fine droplet flow were sampled separately. The results were compared with two-phase flow theory and direct observation of liquid behaviour. In a study of sample transport through narrow tubes, it was observed that, below a certain liquid loading, the sample did not move, the liquid remaining stationary on the tubing wall. The basic analysis of the collected samples was made by gravimetric methods. Adsorption tubes were used with success to measure water vapour. A humidity meter with a sensor of the aluminium oxide type was found to be unreliable. Oil could be measured selectively by a flame ionization detector, the sample being pretreated in an evaporation- condensation unit

  18. In-air micro-pixe analysis of tissue samples

    International Nuclear Information System (INIS)

    Micro-PIXE is capable of providing spatial distributions of elements in the micro-meter scale and its application to biology is useful to elucidate the cellular metabolism. Since, in this method, a sample target is usually irradiated with proton or α-particle beams in vacuum, beam heating results in evaporation of volatile elements an shrinking of the sample. In order to avoid these side effects, we previously developed a technique of in-air micro-PIXE analysis for samples of cultured cells. In addition to these, analysis of exposed tissue samples from living subjects is highly desirable in biological and medical research. Here, we describe a technique of in-air micro-PIXE analysis of such tissue samples. The target samples of exposed tissue slices from a Donryu rat, in which a tumor had been transplanted, were analyzed with proton micro-beams of 2.6 MeV. We report that the shape of cells and the distribution of volatile elements in the tissue sample remain uncharged when using a target preparation based on a freeze-drying method. (author)

  19. Methods for Sampling and Measurement of Compressed Air Contaminants

    International Nuclear Information System (INIS)

    In order to improve the technique for measuring oil and water entrained in a compressed air stream, a laboratory study has been made of some methods for sampling and measurement. For this purpose water or oil as artificial contaminants were injected in thin streams into a test loop, carrying dry compressed air. Sampling was performed in a vertical run, down-stream of the injection point. Wall attached liquid, coarse droplet flow, and fine droplet flow were sampled separately. The results were compared with two-phase flow theory and direct observation of liquid behaviour. In a study of sample transport through narrow tubes, it was observed that, below a certain liquid loading, the sample did not move, the liquid remaining stationary on the tubing wall. The basic analysis of the collected samples was made by gravimetric methods. Adsorption tubes were used with success to measure water vapour. A humidity meter with a sensor of the aluminium oxide type was found to be unreliable. Oil could be measured selectively by a flame ionization detector, the sample being pretreated in an evaporation- condensation unit

  20. Genotoxicity, inflammation and physico-chemical properties of fine particle samples from an incineration energy plant and urban air

    DEFF Research Database (Denmark)

    Sharma, Anoop Kumar; Jensen, Keld Alstrup; Rank, Jette;

    2007-01-01

    Airborne particulate matter (PM) was sampled by use of an electrostatic sampler in an oven hall and a receiving hall in a waste-incineration energy plant, and from urban air in a heavy-traffic street and from background air in Copenhagen. PM was sampled for 1-2 weeks, four samples at each site. The......), but the distribution was completely different in the oven hall (maximum mode at about 150 nm). Also chemically, the samples from the oven hall were highly different from the other samples. PM extracts from the receiving hall, street and background air were more mutagenic than the PM extracts from the...... locations in particle size distribution, chemical composition and the resulting biological effects when A549 cells were incubated with the PM. These characteristics and observations in the oven hall indicated that the PM source was oven exhaust, which was well combusted. (c) 2007 Elsevier B.V. All rights...

  1. Validation of analysis results of ground air samples - using different sampling and analysis methods

    International Nuclear Information System (INIS)

    In the laboratory different techniques for ground air sampling were compared to each other. For this purpose constant mixtures of gases were produced with gas mixing systems and the samples were taken using different sampling techniques in the same way as usually done in situ. A mixture of different chlorinated hydrocarbons in three different concentrations was analysed. It resulted that all sampling methods testes can be considered as equally suited with regard to the quality of the measuring results. But with regard to other evaluation criteria such as e.g. the limit of determination or sample volume they differ considerably. (orig.)

  2. Design of an online spot air sampling system

    International Nuclear Information System (INIS)

    In all the alpha handling facilities spot air sampling is essential while clearing a lab consequent to week end ventilation shut down or subsequent to completion of work/operations goes inside the facility. The sampling head is designed for 5 micron particles. Following pints are noticed over a period of such operational activities: Health Physicist goes inside a lab with a half face mask whose protection factor is 10, thereby useful for lab air activity up to ten DACs. Many times HP goes inside the lab when activity is more which is highly unsafe. On many occasions simultaneously a number of samples have to be taken by HP from a large number of laboratories inside the facility or for any special job where continuous radiological protection is required. Based on this it is proposed to design a sampling system which will overcome the above limitations. The design of the sampling head has been carried out which is for 5 micron particle size. The pump which is available in the existing facilities can be utilized. An innovative way of counting for large number of samples is fabricated in the RHC wing, RMD which can count ten samples at a time. Removal and counting of the sample may be carried out in a similar sampling carousel which is being used in RHC Unit, Radiometallurgy wing successfully with a little modification. In the proposed system, three samples can be operated in-line such that health physics intervention during the active operation would be minimum and during alarm situations (i.e. on the DAC level) proper protective equipment shall be advised by health physicist or he may suggest any other protective action. This type of online monitors will help in establishing the airborne activity inside the lab where special jobs are being carried out which will provide maximum protection to the lab personnel as well as to the health physicist who supervises the entire operation

  3. Solubility testing of actinides on breathing-zone and area air samples

    Science.gov (United States)

    Metzger, Robert Lawrence

    The solubility of inhaled radionuclides in the human lung is an important characteristic of the compounds needed to perform internal dosimetry assessments for exposed workers. A solubility testing method for uranium and several common actinides has been developed with sufficient sensitivity to allow profiles to be determined from routine breathing zone and area air samples in the workplace. Air samples are covered with a clean filter to form a filter-sample-filter sandwich which is immersed in an extracellular lung serum simulant solution. The sample is moved to a fresh beaker of the lung fluid simulant each day for one week, and then weekly until the end of the 28 day test period. The soak solutions are wet ashed with nitric acid and hydrogen peroxide to destroy the organic components of the lung simulant solution prior to extraction of the nuclides of interest directly into an extractive scintillator for subsequent counting on a Photon-Electron Rejecting Alpha Liquid Scintillation (PERALSsp°ler ) spectrometer. Solvent extraction methods utilizing the extractive scintillators have been developed for the isotopes of uranium, plutonium, and curium. The procedures normally produce an isotopic recovery greater than 95% and have been used to develop solubility profiles from air samples with 40 pCi or less of Usb3Osb8. This makes it possible to characterize solubility profiles in every section of operating facilities where airborne nuclides are found using common breathing zone air samples. The new method was evaluated by analyzing uranium compounds from two uranium mills whose product had been previously analyzed by in vitro solubility testing in the laboratory and in vivo solubility testing in rodents. The new technique compared well with the in vivo rodent solubility profiles. The method was then used to evaluate the solubility profiles in all process sections of an operating in situ uranium plant using breathing zone and area air samples collected during routine

  4. BMAA extraction of cyanobacteria samples: which method to choose?

    Science.gov (United States)

    Lage, Sandra; Burian, Alfred; Rasmussen, Ulla; Costa, Pedro Reis; Annadotter, Heléne; Godhe, Anna; Rydberg, Sara

    2016-01-01

    β-N-Methylamino-L-alanine (BMAA), a neurotoxin reportedly produced by cyanobacteria, diatoms and dinoflagellates, is proposed to be linked to the development of neurological diseases. BMAA has been found in aquatic and terrestrial ecosystems worldwide, both in its phytoplankton producers and in several invertebrate and vertebrate organisms that bioaccumulate it. LC-MS/MS is the most frequently used analytical technique in BMAA research due to its high selectivity, though consensus is lacking as to the best extraction method to apply. This study accordingly surveys the efficiency of three extraction methods regularly used in BMAA research to extract BMAA from cyanobacteria samples. The results obtained provide insights into possible reasons for the BMAA concentration discrepancies in previous publications. In addition and according to the method validation guidelines for analysing cyanotoxins, the TCA protein precipitation method, followed by AQC derivatization and LC-MS/MS analysis, is now validated for extracting protein-bound (after protein hydrolysis) and free BMAA from cyanobacteria matrix. BMAA biological variability was also tested through the extraction of diatom and cyanobacteria species, revealing a high variance in BMAA levels (0.0080-2.5797 μg g(-1) DW). PMID:26304815

  5. RAPID SEPARATION METHOD FOR ACTINIDES IN EMERGENCY AIR FILTER SAMPLES

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S.; Noyes, G.; Culligan, B.

    2010-02-03

    A new rapid method for the determination of actinides and strontium in air filter samples has been developed at the Savannah River Site Environmental Lab (Aiken, SC, USA) that can be used in emergency response situations. The actinides and strontium in air filter method utilizes a rapid acid digestion method and a streamlined column separation process with stacked TEVA, TRU and Sr Resin cartridges. Vacuum box technology and rapid flow rates are used to reduce analytical time. Alpha emitters are prepared using cerium fluoride microprecipitation for counting by alpha spectrometry. The purified {sup 90}Sr fractions are mounted directly on planchets and counted by gas flow proportional counting. The method showed high chemical recoveries and effective removal of interferences. This new procedure was applied to emergency air filter samples received in the NRIP Emergency Response exercise administered by the National Institute for Standards and Technology (NIST) in April, 2009. The actinide and {sup 90}Sr in air filter results were reported in {approx}4 hours with excellent quality.

  6. Compression test of masonry core samples extracted from existing brickwork

    OpenAIRE

    Pelà, Luca; Canella, Elisa; Aprile, Alessandra; Roca Fabregat, Pedro

    2016-01-01

    This research is focused on the experimental characterisation of the compressive behaviour of masonry in existing buildings. The proposed technique is based on in situ core drilling of masonry members. Two walls were built making use of terracotta handmade bricks and lime mortar, without cement, to reproduce a low-strength historical masonry. Core samples were extracted from the walls and then regularized to perform a non-standard compression test in the laboratory. Stack-bonded prisms were a...

  7. Extraction DNA from Activated Sludge-Comparing with Soil Sample

    Institute of Scientific and Technical Information of China (English)

    谢冰; 奚旦立; 陈季华

    2003-01-01

    DNA directly extraction from activated sludge and soil sample with enzyme lyses methods was investigated in this paper. DNA yield from activated sludge was 3.0 mg/g. VLSS, and 28.2-43.8 μg/g soil respectively. The resulting DNA is suitable for PCR.By studied methods, higher quality and quantity of sludge DNA could be obtained rapidly and inexpensively from large number of samples, and the PCR product obtained from this protocol was not affected by contaminated higher concentration of heavy metals.

  8. The comparison of pollen abundance in air and honey samples

    OpenAIRE

    Ingrida Šaulienė; Laura Šukienė; Auste Noreikaite-Merkeliene; Vidmantas Pileckas

    2015-01-01

    Honey as a food has long been used in human nutrition and is still popular. Honey is important because of its therapeutic, prophylactic and strengthening value. Pollen is one of the most decisive components that ensure the quality and type of honey. Modern society becomes more and more sensitive to airborne pollen. Therefore, it is crucial to determine the composition of allergenic plant pollen in natural honey. For this purpose, we studied and compared pollen abundance in honey and air sampl...

  9. Bioaerosol DNA Extraction Technique from Air Filters Collected from Marine and Freshwater Locations

    Science.gov (United States)

    Beckwith, M.; Crandall, S. G.; Barnes, A.; Paytan, A.

    2015-12-01

    Bioaerosols are composed of microorganisms suspended in air. Among these organisms include bacteria, fungi, virus, and protists. Microbes introduced into the atmosphere can drift, primarily by wind, into natural environments different from their point of origin. Although bioaerosols can impact atmospheric dynamics as well as the ecology and biogeochemistry of terrestrial systems, very little is known about the composition of bioaerosols collected from marine and freshwater environments. The first step to determine composition of airborne microbes is to successfully extract environmental DNA from air filters. We asked 1) can DNA be extracted from quartz (SiO2) air filters? and 2) how can we optimize the DNA yield for downstream metagenomic sequencing? Aerosol filters were collected and archived on a weekly basis from aquatic sites (USA, Bermuda, Israel) over the course of 10 years. We successfully extracted DNA from a subsample of ~ 20 filters. We modified a DNA extraction protocol (Qiagen) by adding a beadbeating step to mechanically shear cell walls in order to optimize our DNA product. We quantified our DNA yield using a spectrophotometer (Nanodrop 1000). Results indicate that DNA can indeed be extracted from quartz filters. The additional beadbeating step helped increase our yield - up to twice as much DNA product was obtained compared to when this step was omitted. Moreover, bioaerosol DNA content does vary across time. For instance, the DNA extracted from filters from Lake Tahoe, USA collected near the end of June decreased from 9.9 ng/μL in 2007 to 3.8 ng/μL in 2008. Further next-generation sequencing analysis of our extracted DNA will be performed to determine the composition of these microbes. We will also model the meteorological and chemical factors that are good predictors for microbial composition for our samples over time and space.

  10. Sample extraction and injection with a microscale preconcentrator.

    Energy Technology Data Exchange (ETDEWEB)

    Robinson, Alex Lockwood (Advanced Sensor Technologies, Albuquerque, NM); Chan, Helena Kai Lun

    2007-09-01

    This report details the development of a microfabricated preconcentrator that functions as a fully integrated chemical extractor-injector for a microscale gas chromatograph (GC). The device enables parts-per-billion detection and quantitative analysis of volatile organic compounds (VOCs) in indoor air with size and power advantages over macro-scale systems. The 44 mm{sup 3} preconcentrator extracts VOCs using highly adsorptive, granular forms of graphitized carbon black and carbon molecular sieves. The micron-sized silicon cavities have integrated heating and temperature sensing allowing low power, yet rapid heating to thermally desorb the collected VOCs (GC injection). The keys to device construction are a new adsorbent-solvent filling technique and solvent-tolerant wafer-level silicon-gold eutectic bonding technology. The product is the first granular adsorbent preconcentrator integrated at the wafer level. Other advantages include exhaustive VOC extraction and injection peak widths an order of magnitude narrower than predecessor prototypes. A mass transfer model, the first for any microscale preconcentrator, is developed to describe both adsorption and desorption behaviors. The physically intuitive model uses implicit and explicit finite differences to numerically solve the required partial differential equations. The model is applied to the adsorption and desorption of decane at various concentrations to extract Langmuir adsorption isotherm parameters from effluent curve measurements where properties are unknown a priori.

  11. EXTRACT: interactive extraction of environment metadata and term suggestion for metagenomic sample annotation.

    Science.gov (United States)

    Pafilis, Evangelos; Buttigieg, Pier Luigi; Ferrell, Barbra; Pereira, Emiliano; Schnetzer, Julia; Arvanitidis, Christos; Jensen, Lars Juhl

    2016-01-01

    The microbial and molecular ecology research communities have made substantial progress on developing standards for annotating samples with environment metadata. However, sample manual annotation is a highly labor intensive process and requires familiarity with the terminologies used. We have therefore developed an interactive annotation tool, EXTRACT, which helps curators identify and extract standard-compliant terms for annotation of metagenomic records and other samples. Behind its web-based user interface, the system combines published methods for named entity recognition of environment, organism, tissue and disease terms. The evaluators in the BioCreative V Interactive Annotation Task found the system to be intuitive, useful, well documented and sufficiently accurate to be helpful in spotting relevant text passages and extracting organism and environment terms. Comparison of fully manual and text-mining-assisted curation revealed that EXTRACT speeds up annotation by 15-25% and helps curators to detect terms that would otherwise have been missed. Database URL: https://extract.hcmr.gr/. PMID:26896844

  12. Comparative Study of the Effect of Sample Pretreatment and Extraction on the Determination of Flavonoids from Lemon (Citrus limon.

    Directory of Open Access Journals (Sweden)

    Carlos A Ledesma-Escobar

    Full Text Available Flavonoids have shown to exert multiple beneficial effects on human health, being also appreciated by both food and pharmaceutical industries. Citrus fruits are a key source of flavonoids, thus promoting studies to obtain them. Characteristics of these studies are the discrepancies among sample pretreatments and among extraction methods, and also the scant number of comparative studies developed so far.Evaluate the effect of both the sample pretreatment and the extraction method on the profile of flavonoids isolated from lemon.Extracts from fresh, lyophilized and air-dried samples obtained by shaking extraction (SE, ultrasound-assisted extraction (USAE, microwave-assisted extraction (MAE and superheated liquid extraction (SHLE were analyzed by LC-QTOF MS/MS, and 32 flavonoids were tentatively identified using MS/MS information. ANOVA applied to the data from fresh and dehydrated samples and from extraction by the different methods revealed that 26 and 32 flavonoids, respectively, were significant (p≤0.01. The pairwise comparison (Tukey HSD; p≤0.01 showed that lyophilized samples are more different from fresh samples than from air-dried samples; also, principal component analysis (PCA showed a clear discrimination among sample pretreatment strategies and suggested that such differences are mainly created by the abundance of major flavonoids. On the other hand, pairwise comparison of extraction methods revealed that USAE and MAE provided quite similar extracts, being SHLE extracts different from the other two. In this case, PCA showed a clear discrimination among extraction methods, and their position in the scores plot suggests a lower abundance of flavonoids in the extracts from SHLE. In the two PCA the loadings plots revealed a trend to forming groups according to flavonoid aglycones.The present study shows clear discrimination caused by both sample pretreatments and extraction methods. Under the studied conditions, liophilization provides

  13. Passive air sampling of gaseous elemental mercury: a critical review

    Science.gov (United States)

    McLagan, David S.; Mazur, Maxwell E. E.; Mitchell, Carl P. J.; Wania, Frank

    2016-03-01

    Because gaseous elemental mercury (GEM) is distributed globally through the atmosphere, reliable means of measuring its concentrations in air are important. Passive air samplers (PASs), designed to be cheap, simple to operate, and to work without electricity, could provide an alternative to established active sampling techniques in applications such as (1) long-term monitoring of atmospheric GEM levels in remote regions and in developing countries, (2) atmospheric mercury source identification and characterization through finely resolved spatial mapping, and (3) the recording of personal exposure to GEM. An effective GEM PAS requires a tightly constrained sampling rate, a large and stable uptake capacity, and a sensitive analytical technique. None of the GEM PASs developed to date achieve levels of accuracy and precision sufficient for the reliable determination of background concentrations over extended deployments. This is due to (1) sampling rates that vary due to meteorological factors and manufacturing inconsistencies, and/or (2) an often low, irreproducible and/or unstable uptake capacity of the employed sorbents. While we identify shortcomings of existing GEM PAS, we also reveal potential routes to overcome those difficulties. Activated carbon and nanostructured metal surfaces hold promise as effective sorbents. Sampler designs incorporating diffusive barriers should be able to notably reduce the influence of wind on sampling rates.

  14. ANALYSIS OF VAPORS FROM METHYLENE CHLORIDE EXTRACTS OF NUCLEAR GRADE HEPA FILTER FIBERGLASS SAMPLES

    Energy Technology Data Exchange (ETDEWEB)

    FRYE JM; ANASTOS HL; GUTIERREZ FC

    2012-06-07

    While several organic compounds were detected in the vapor samples used in the reenactment of the preparation of mounts from the extracts of nuclear grade high-efficiency particulate air filter fiberglass samples, the most significant species present in the samples were methylene chloride, phenol, phenol-d6, and 2-fluorophenol. These species were all known to be present in the extracts, but were expected to have evaporated during the preparation of the mounts, as the mounts appeared to be dry before any vapor was collected. These species were present at the following percentages of their respective occupational exposure limits: methylene chloride, 2%; phenol, 0.4%; and phenol-d6, 0.6%. However, there is no established limit for 2-fluorophenol. Several other compounds were detected at low levels for which, as in the case of 2-fluorophenol, there are no established permissible exposure limits. These compounds include 2-chlorophenol; N-nitroso-1-propanamine; 2-fluoro-1,1{prime}-biphenyl; 1,2-dihydroacenaphthylene; 2,5-cyclohexadiene-1,4-dione,2,6-bis(1,1-dimethylethyl); trimethyl oxirane; n-propylpropanamine; 2-(Propylamino)ethanol; 4-methoxy-1-butene; 6-methyl-5-hepten-2-one; and 3,4-dimethylpyridine. Some of these were among those added as surrogates or spike standards as part ofthe Advanced Technologies and Laboratories International, Inc. preparation ofthe extract of the HEPA filter media and are indicated as such in the data tables in Section 2, Results; other compounds found were not previously known to be present. The main inorganic species detected (sulfate, sodium, and sulfur) are also consistent with species added in the preparation of the methylene chloride extract of the high-efficiency particulate air sample.

  15. Evaluating the mutagenicity of the water-soluble fraction of air particulate matter: A comparison of two extraction strategies.

    Science.gov (United States)

    Palacio, Isabel C; Oliveira, Ivo F; Franklin, Robson L; Barros, Silvia B M; Roubicek, Deborah A

    2016-09-01

    Many studies have focused on assessing the genotoxic potential of the organic fraction of airborne particulate matter. However, the determination of water-soluble compounds, and the evaluation of the toxic effects of these elements can also provide valuable information for the development of novel strategies to control atmospheric air pollution. To determine an appropriate extraction method for assessing the mutagenicity of the water-soluble fraction of PM, we performed microwave assisted (MW) and ultrasonic bath (US) extractions, using water as solvent, in eight different air samples (TSP and PM10). Mutagenicity and extraction performances were evaluated using the Salmonella/microsome assay with strains TA98 and TA100, followed by chemical determination of water-soluble metals. Additionally, we evaluated the chemical and biological stability of the extracts testing their mutagenic potential and chemically determining elements present in the samples along several periods after extraction. Reference material SRM 1648a was used. The comparison of MW and US extractions did not show differences on the metals concentrations, however positive mutagenic responses were detected with TA98 strain in all samples extracted using the MW method, but not with the US bath extraction. The recovery, using reference material was better in samples extracted with MW. We concluded that the MW extraction is more efficient to assess the mutagenic activity of the soluble fraction of airborne PM. We also observed that the extract freezing and storage over 60 days has a significant effect on the mutagenic and analytical results on PM samples, and should be avoided. PMID:27258903

  16. Radioiodine deposition losses from sample air containing particulate and gaseous iodine in nuclear reactor sample lines

    International Nuclear Information System (INIS)

    Mechanisms of radioiodine deposition from sample air containing both gaseous and particulate radioiodine in reactor sample lines are studied, and experimental methods are developed. A short half-lived radioiodine tracer, 128I (t1/2 = 25 min), is used in the chemical forms of molecular iodine and methyl iodide. An effort is made to investigate the type of particles for particulate iodine. Of the various types of particles tested, only tobacco smoke particles have a sufficiently high iodination rate to be used in these studies. The 609.6-cm (20-ft)-long sample lines of Types 316 and 304 stainless steel tube (2.29 cm i.d.) were tested for the sample flow rates of 28.3 ell/min (1 ft3/min) and 56.6 ell/min (2 ft3/min). In-tube measurements using a calibrated thin-walled Geiger tube are conducted to determine the penetration factor and space-dependent deposition velocity profile of radioiodine. Methyl iodide is not reactive for either the tube surfaces or aerosol particles. The overall deposition velocity of the mixture of the smoke particles and molecular iodine is higher than that of molecular iodine alone for similar sampling conditions. It is concluded that the high deposition rate of radioiodine in the sample air mixed with smoke particles and molecular iodine is caused by the different sample line surfaces that are contaminated with smoke particles

  17. Electromembrane extraction for the determination of parabens in water samples.

    Science.gov (United States)

    Villar-Navarro, Mercedes; Moreno-Carballo, María Del Carmen; Fernández-Torres, Rut; Callejón-Mochón, Manuel; Bello-López, Miguel Ángel

    2016-02-01

    To our knowledge, for the first time an electromembrane extraction combined with a high-performance liquid chromatography procedure using diode-array detection has been developed for the determination of five of the most widely used parabens: ethyl 4-hydroxybenzoate, propyl 4-hydroxybenzoate, butyl 4-hydroxybenzoate, isobutyl 4-hydroxybenzoate, and benzyl 4-hydroxybenzoate. Parabens were extracted from pH 4 aqueous sample solutions with use of an Accurel® S6/2 polypropylene hollow fiber that supports a liquid membrane of 1-octanol to a pH 12 aqueous acceptor solution placed inside the lumen of the hollow fiber. An electric current of 30 V was applied over the supported liquid membrane by means of platinum wires placed in the donor and acceptor phases. Parabens were extracted in 40 min with enrichment factors in the 30-49 range. The procedure has detection limits between 0.98 and 1.43 μg L(-1). The method was applied to the determination of parabens in surface environmental waters with excellent results. PMID:26753971

  18. Biomimetic air sampling for detection of low concentrations of molecules and bioagents : LDRD 52744 final report.

    Energy Technology Data Exchange (ETDEWEB)

    Hughes, Robert Clark

    2003-12-01

    Present methods of air sampling for low concentrations of chemicals like explosives and bioagents involve noisy and power hungry collectors with mechanical parts for moving large volumes of air. However there are biological systems that are capable of detecting very low concentrations of molecules with no mechanical moving parts. An example is the silkworm moth antenna which is a highly branched structure where each of 100 branches contains about 200 sensory 'hairs' which have dimensions of 2 microns wide by 100 microns long. The hairs contain about 3000 pores which is where the gas phase molecules enter the aqueous (lymph) phase for detection. Simulations of diffusion of molecules indicate that this 'forest' of hairs is 'designed' to maximize the extraction of the vapor phase molecules. Since typical molecules lose about 4 decades in diffusion constant upon entering the liquid phase, it is important to allow air diffusion to bring the molecule as close to the 'sensor' as possible. The moth acts on concentrations as low as 1000 molecules per cubic cm. (one part in 1e16). A 3-D collection system of these dimensions could be fabricated by micromachining techniques available at Sandia. This LDRD addresses the issues involved with extracting molecules from air onto micromachined structures and then delivering those molecules to microsensors for detection.

  19. Oxygen Isotopic Analyses of Water Extracted from Lunar Samples

    Science.gov (United States)

    Nunn Martinez, M.; Thiemens, M. H.

    2014-12-01

    Oxygen exists in lunar materials in distinct phases having unique sources and equilibration histories. The oxygen isotopic composition (δ17O, δ18O) of various components of lunar materials has been studied extensively, but analyses of water in these samples are relatively sparse [1-3]. Samples collected on the lunar surface reflect not only the composition of their source reservoirs but also contributions from asteroidal and cometary impacts, interactions with solar wind and cosmic radiation, among other surface processes. Isotopic characterization of oxygen in lunar water could help resolve the major source of water in the Earth-Moon system by revealing if lunar water is primordial, asteroidal, or cometary in origin [1]. Methods: A lunar rock/soil sample is pumped to high vacuum to remove physisorbed water before heating step-wise to 50, 150, and 1000°C to extract extraterrestrial water without terrestrial contamination. The temperature at which water is evolved is proportional to the strength with which the water is bound in the sample and the relative difficulty of exchanging oxygen atoms in that water. This allows for the isolated extraction of water bound in different phases, which could have different source reservoirs and/or histories, as evidenced by the mass (in)dependence of oxygen compositions. A low blank procedure was developed to accommodate the low water content of lunar material [4]. Results: Oxygen isotopic analyses of lunar water extracted by stepwise heating lunar basalts and breccias with a range of compositions, petrologic types, and surface exposure ages will be presented. The cosmic ray exposure age of these samples varies by two orders of magnitude, and we will consider this in discussing the effects of solar wind and cosmic radiation on the oxygen isotopic composition (Δ17O). I will examine the implications of our water analyses for the composition of the oxygen-bearing reservoir from which that water formed, the effects of surface

  20. Sorbent-based sampling methods for volatile and semi-volatile organic compounds in air Part 1: Sorbent-based air monitoring options.

    Science.gov (United States)

    Woolfenden, Elizabeth

    2010-04-16

    Sorbent tubes/traps are widely used in combination with gas chromatographic (GC) analytical methods to monitor the vapour-phase fraction of organic compounds in air. Target compounds range in volatility from acetylene and freons to phthalates and PCBs and include apolar, polar and reactive species. Airborne vapour concentrations will vary depending on the nature of the location, nearby pollution sources, weather conditions, etc. Levels can range from low percent concentrations in stack and vent emissions to low part per trillion (ppt) levels in ultra-clean outdoor locations. Hundreds, even thousands of different compounds may be present in any given atmosphere. GC is commonly used in combination with mass spectrometry (MS) detection especially for environmental monitoring or for screening uncharacterised workplace atmospheres. Given the complexity and variability of organic vapours in air, no one sampling approach suits every monitoring scenario. A variety of different sampling strategies and sorbent media have been developed to address specific applications. Key sorbent-based examples include: active (pumped) sampling onto tubes packed with one or more sorbents held at ambient temperature; diffusive (passive) sampling onto sorbent tubes/cartridges; on-line sampling of air/gas streams into cooled sorbent traps; and transfer of air samples from containers (canisters, Tedlar) bags, etc.) into cooled sorbent focusing traps. Whichever sampling approach is selected, subsequent analysis almost always involves either solvent extraction or thermal desorption (TD) prior to GC(/MS) analysis. The overall performance of the air monitoring method will depend heavily on appropriate selection of key sampling and analytical parameters. This comprehensive review of air monitoring using sorbent tubes/traps is divided into 2 parts. (1) Sorbent-based air sampling option. (2) Sorbent selection and other aspects of optimizing sorbent-based air monitoring methods. The paper presents

  1. Measurements of an ion beam diameter extracted into air through a glass capillary

    International Nuclear Information System (INIS)

    To establish techniques for in-air materials analysis using a glass capillary, we studied the beam distribution extracted in air as a function of the distance between the exit of the capillary and the target. We measured three-dimensional intensity distributions of the extracted beams, and compared the observed results with the model calculation. The comparison showed that the glass capillary technique is designed to reduce a divergence of the beam extracted into the air by a beam-focusing effect

  2. Progress in field-assisted extraction and its application to solid sample analysis.

    Science.gov (United States)

    He, Yuanyuan; Xiao, Xiaohua; Cheng, Yingyi; Li, Gongke

    2016-01-01

    Sample preparation is the most time-consuming and laborious procedure during analysis. The rapid and effective extraction of solid and semi-solid samples is much more difficult than that of gas and liquid samples. In the present review, various extraction methods for solid and semi-solid samples such as supercritical fluid extraction, ultrasound-assisted extraction, microwave-assisted extraction, etc. are summarized based on the principles of field and field synergy effects. The expected trends of field-assisted extraction methods are discussed and proposed to encourage further development on the rapid and effective extraction for solid and semi-solid samples. PMID:26390199

  3. CARBONIZED FIBROUS RESIN AS A NEW SORBENT FOR SAMPLING POLYCYCLIC AROMATIC HYDROCARBONS (PAHS)IN AMBIENT AIR

    Institute of Scientific and Technical Information of China (English)

    LINGDaren; LIUBing; 等

    2002-01-01

    A new sampling method of ambient air analysis using carbonized fibrous resin as a sorbent for polycyclic aromatic hydrocarbons(PAHs) was reported.The physical and chemical properties of the carbonized fibrous resins were measured.The sample pretreatment with ultrasonic extraction and subsequent clean-up elution through a silica gel column was optimized.The suitable ultrasonic extraction conditions were selected as follows:resin weight was 1.5g,ultrasonic extraction time 20min,volume of extraction solvent 100 ml and extraction operation times 2-3.The concentrated extractable organic matter was submitted to next step of clean-up procedure of adsorption chromatography on silica gel column/n-hexane and a mixture of dichloromethene:n-hexane solution 2:3(v/v).The PAHs fractions in the real samples from Changzhou,China were particularly analyzed using GC-MS data system and the data of mass spectra,retention times and scan numbers of the real samples were compared with that of the standards of 16 PAHs listed by the US EPA as “priority pollutants” of the environment. The pretreatment of samples of ambient air with carbonized fibrous resin as a sorbent for PAHs is proved to be reliable and might be used for the procedure of the determination of PAHs in atmospheric environment.

  4. Extraction of Plutonium From Spiked INEEL Soil Samples Using the Ligand-Assisted Supercritical Fluid Extraction (LA-SFE) Technique

    International Nuclear Information System (INIS)

    In order to investigate the effectiveness of ligand-assisted supercritical fluid extraction for the removal of transuranic contaminations from soils an Idaho National Engineering and Environmental Laboratory (INEEL) silty-clay soil sample was obtained from near the Radioactive Waste Management Complex area and subjected to three different chemical preparations before being spiked with plutonium. The spiked INEEL soil samples were subjected to a sequential aqueous extraction procedure to determine radionuclide portioning in each sample. Results from those extractions demonstrate that plutonium consistently partitioned into the residual fraction across all three INEEL soil preparations whereas americium partitioned 73% into the iron/manganese fraction for soil preparation A, with the balance partitioning into the residual fraction. Plutonium and americium were extracted from the INEEL soil samples using a ligand-assisted supercritical fluid extraction technique. Initial supercritical fluid extraction runs produced plutonium extraction technique. Initial supercritical fluid extraction runs produced plutonium extraction efficiencies ranging from 14% to 19%. After a second round wherein the initial extraction parameters were changed, the plutonium extraction efficiencies increased to 60% and as high as 80% with the americium level in the post-extracted soil samples dropping near to the detection limits. The third round of experiments are currently underway. These results demonstrate that the ligand-assisted supercritical fluid extraction technique can effectively extract plutonium from the spiked INEEL soil preparations

  5. Modifier free supercritical fluid extraction of uranium from sintered UO2, soil and ore samples

    International Nuclear Information System (INIS)

    Direct extraction of uranium from different samples viz. sintered UO2, soil and ores was carried out by modifier free supercritical fluid using tri-n-butyl phosphate-nitric acid (TBP-HNO3) adduct as extractant. These studies showed that pre-equilibration with more concentrated nitric acid helps in better dissolution and extraction of uranium from sintered UO2 samples. Modifier free supercritical fluid extraction appears attractive with respect to minimization of secondary wastes. This method resulted 80-100% extraction of uranium from different soil/ore samples. The results were confirmed by performing neutron activation analysis of original (before extraction) and residue (after extraction) samples. (author)

  6. Recent developments on field gas extraction and sample preparation methods for radiokrypton dating of groundwater

    Science.gov (United States)

    Yokochi, Reika

    2016-09-01

    Current and foreseen population growths will lead to an increased demand in freshwater, large quantities of which is stored as groundwater. The ventilation age is crucial to the assessment of groundwater resources, complementing the hydrological model approach based on hydrogeological parameters. Ultra-trace radioactive isotopes of Kr (81 Kr and 85 Kr) possess the ideal physical and chemical properties for groundwater dating. The recent advent of atom trap trace analyses (ATTA) has enabled determination of ultra-trace noble gas radioisotope abundances using 5-10 μ L of pure Kr. Anticipated developments will enable ATTA to analyze radiokrypton isotope abundances at high sample throughput, which necessitates simple and efficient sample preparation techniques that are adaptable to various sample chemistries. Recent developments of field gas extraction devices and simple and rapid Kr separation method at the University of Chicago are presented herein. Two field gas extraction devices optimized for different sampling conditions were recently designed and constructed, aiming at operational simplicity and portability. A newly developed Kr purification system enriches Kr by flowing a sample gas through a moderately cooled (138 K) activated charcoal column, followed by a gentle fractionating desorption. This simple process uses a single adsorbent and separates 99% of the bulk atmospheric gases from Kr without significant loss. The subsequent two stages of gas chromatographic separation and a hot Ti sponge getter further purify the Kr-enriched gas. Abundant CH4 necessitates multiple passages through one of the gas chromatographic separation columns. The presented Kr separation system has a demonstrated capability of extracting Kr with > 90% yield and 99% purity within 75 min from 1.2 to 26.8 L STP of atmospheric air with various concentrations of CH4. The apparatuses have successfully been deployed for sampling in the field and purification of groundwater samples.

  7. Interlaboratory evaluation of cellulosic acid-soluble internal air sampling capsules for multi-element analysis.

    Science.gov (United States)

    Andrews, Ronnee N; Feng, H Amy; Ashley, Kevin

    2016-01-01

    An interlaboratory study was carried out to evaluate the use of acid-soluble cellulosic air sampling capsules for their suitability in the measurement of trace elements in workplace atmospheric samples. These capsules are used as inserts to perform closed-face cassette sample collection for occupational exposure monitoring. The interlaboratory study was performed in accordance with NIOSH guidelines that describe statistical procedures for evaluating measurement accuracy of air monitoring methods. The performance evaluation materials used consisted of cellulose acetate capsules melded to mixed-cellulose ester filters that were dosed with multiple elements from commercial standard aqueous solutions. The cellulosic capsules were spiked with the following 33 elements of interest in workplace air monitoring: Ag, Al, As, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe, In, K, La, Li, Mg, Mn, Mo, Ni, P, Pb, Sb, Se, Sn, Sr, Te, Ti, Tl, V, W, Y, Zn, Zr. The elemental loading levels were certified by an accredited provider of certified reference materials. Triplicates of media blanks and multielement-spiked capsules at three different elemental loadings were sent to each participating laboratory; the elemental loading levels were not revealed to the laboratories. The volunteer participating laboratories were asked to prepare the samples by acid dissolution and to analyze aliquots of extracted samples by inductively coupled plasma atomic emission spectrometry in accordance with NIOSH methods. It was requested that the study participants report their analytical results in units of μg of each target element per internal capsule sample. For the majority of the elements investigated (30 out of 33), the study accuracy estimates obtained satisfied the NIOSH accuracy criterion (A < 25%). This investigation demonstrates the utility of acid-soluble internal sampling capsules for multielement analysis by atomic spectrometry. PMID:26308974

  8. Passive Samplers for Investigations of Air Quality: Method Description, Implementation, and Comparison to Alternative Sampling Methods

    Science.gov (United States)

    This Paper covers the basics of passive sampler design, compares passive samplers to conventional methods of air sampling, and discusses considerations when implementing a passive sampling program. The Paper also discusses field sampling and sample analysis considerations to ensu...

  9. Dispersion modeling of selected PAHs in urban air: A new approach combining dispersion model with GIS and passive air sampling

    Czech Academy of Sciences Publication Activity Database

    Sáňka, O.; Melymuk, L.; Čupr, P.; Dvorská, Alice; Klánová, J.

    2014-01-01

    Roč. 90, oct (2014), s. 88-95. ISSN 1352-2310 Institutional support: RVO:67179843 Keywords : passive air sampling * air dispersion modeling * GIS * polycyclic aromatic hydrocarbons * emission inventories Subject RIV: DI - Air Pollution ; Quality Impact factor: 3.281, year: 2014

  10. Inter-laboratory comparison study on measuring semi-volatile organic chemicals in standards and air samples

    Energy Technology Data Exchange (ETDEWEB)

    Su Yushan, E-mail: yushan.su@ec.gc.c [Air Quality Research Division, Science and Technology Branch, Environment Canada, 4905 Dufferin Street, Toronto, Ontario M3H 5T4 (Canada); Hung, Hayley, E-mail: hayley.hung@ec.gc.c [Air Quality Research Division, Science and Technology Branch, Environment Canada, 4905 Dufferin Street, Toronto, Ontario M3H 5T4 (Canada)

    2010-11-15

    Measurements of semi-volatile organic chemicals (SVOCs) were compared among 21 laboratories from 7 countries through the analysis of standards, a blind sample, an air extract, and an atmospheric dust sample. Measurement accuracy strongly depended on analytes, laboratories, and types of standards and samples. Intra-laboratory precision was generally good with relative standard deviations (RSDs) of triplicate injections <10% and with median differences of duplicate samples between 2.1 and 22%. Inter-laboratory variability, measured by RSDs of all measurements, was in the range of 2.8-58% in analyzing standards, and 6.9-190% in analyzing blind sample and air extract. Inter-laboratory precision was poorer when samples were subject to cleanup processes, or when SVOCs were quantified at low concentrations. In general, inter-laboratory differences up to a factor of 2 can be expected to analyze atmospheric SVOCs. When comparing air measurements from different laboratories, caution should be exercised if the data variability is less than the inter-laboratory differences. - Inter-laboratory differences up to a factor of 2 can be expected for air measurements of semi-volatile organic chemicals.

  11. Inter-laboratory comparison study on measuring semi-volatile organic chemicals in standards and air samples

    International Nuclear Information System (INIS)

    Measurements of semi-volatile organic chemicals (SVOCs) were compared among 21 laboratories from 7 countries through the analysis of standards, a blind sample, an air extract, and an atmospheric dust sample. Measurement accuracy strongly depended on analytes, laboratories, and types of standards and samples. Intra-laboratory precision was generally good with relative standard deviations (RSDs) of triplicate injections <10% and with median differences of duplicate samples between 2.1 and 22%. Inter-laboratory variability, measured by RSDs of all measurements, was in the range of 2.8-58% in analyzing standards, and 6.9-190% in analyzing blind sample and air extract. Inter-laboratory precision was poorer when samples were subject to cleanup processes, or when SVOCs were quantified at low concentrations. In general, inter-laboratory differences up to a factor of 2 can be expected to analyze atmospheric SVOCs. When comparing air measurements from different laboratories, caution should be exercised if the data variability is less than the inter-laboratory differences. - Inter-laboratory differences up to a factor of 2 can be expected for air measurements of semi-volatile organic chemicals.

  12. Stachybotrys mycotoxins: from culture extracts to dust samples.

    Science.gov (United States)

    Došen, Ina; Andersen, Birgitte; Phippen, Christopher B W; Clausen, Geo; Nielsen, Kristian Fog

    2016-08-01

    The filamentous fungus Stachybotrys chartarum is known for its toxic metabolites and has been associated with serious health problems, including mycotoxicosis, among occupants of contaminated buildings. Here, we present results from a case study, where an ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed for known and tentatively identified compounds characterized via UHPLC-quadruple time-of-flight (QTOF) screening of fungal culture extracts, wall scrapings and reference standards. The UHPLC-MS/MS method was able to identify 12 Stachybotrys metabolites, of which four could be quantified based on authentic standards and a further six estimated based on similarity to authentic standards. Samples collected from walls contaminated by S. chartarum in a water-damaged building showed that the two known chemotypes, S and A, coexisted. More importantly, a link between mycotoxin concentrations found on contaminated surfaces and in settled dust was made. One dust sample, collected from a water-damaged room, contained 10 pg/cm(2) macrocyclic trichothecenes (roridin E). For the first time, more than one spirocyclic drimane was detected in dust. Spirocyclic drimanes were detected in all 11 analysed dust samples and in total amounted to 600 pg/cm(2) in the water-damaged room and 340 pg/cm(2) in rooms adjacent to the water-damaged area. Their wide distribution in detectable amounts in dust suggested they could be good candidates for exposure biomarkers. Graphical abstract Stachybotrys growing on a gypsum board, and some of the compounds it produces. PMID:27255106

  13. Low-cost monitoring of campylobacter in poultry houses by air sampling and quantitative PCR

    DEFF Research Database (Denmark)

    Søndergaard, Mette Sofie Rousing; Josefsen, Mathilde Hasseldam; Löfström, Charlotta;

    2014-01-01

    approximately 10(4) and 10(5) CCE per sample for boot swabs and air, respectively. In conclusion, using air samples combined with quantitative real-time PCR, Campylobacter contamination could be detected earlier than by boot swabs and was found to be a more convenient technique for monitoring and/or to obtain......The present study describes the evaluation of a method for the quantification of Campylobacter by air sampling in poultry houses. Sampling was carried out in conventional chicken houses in Poland, in addition to a preliminary sampling in Denmark. Each measurement consisted of three air samples, two...... standard boot swab fecal samples, and one airborne particle count. Sampling was conducted over an 8-week period in three flocks, assessing the presence and levels of Campylobacter in boot swabs and air samples using quantitative real-time PCR. The detection limit for air sampling was approximately 100...

  14. Rapid extraction of PCDD/Fs from soil and fly ash samples. Pressurized fluid extraction (PFE) and microwave-assisted extraction (MAE)

    Energy Technology Data Exchange (ETDEWEB)

    Sanz, P.; Fabrellas, B. [Centro de Investigaciones Energeticas Medioambientales y Tecnologicas (CIEMAT), Madrid (Spain)

    2004-09-15

    The main reference extraction method in the analysis of polychlorinated dibenzop- dioxins and dibenzofurans (PCDD/Fs) is still the Soxhlet extraction. But it requires long extraction times (up to 24 hs), large volumes of hazardous organic solvents (100-300 ml) and its automation is limited. Pressurized Fluid Extraction (PFE) and Microwave-Assisted Extraction (MAE) are two relatively new extraction techniques that reduce the time and the volume of solvent required for extraction. However, very different PFE extraction conditions are found for the same enviromental matrices in the literature. MAE is not a extraction technique very applied for the analysis of PCDD/Fs yet, although it is used for the determination of other organic compounds, such as PCBs and PAHs. In this study, PFE and MAE extraction conditions were optimized to determine PCDDs y PCDFs in fly ash and soil/sediment samples. Conventional Soxhlet extraction with toluene was used to compare the extraction efficiency of both techniques.

  15. Improved Butanol-Methanol (BUME) Method by Replacing Acetic Acid for Lipid Extraction of Biological Samples.

    Science.gov (United States)

    Cruz, Mutya; Wang, Miao; Frisch-Daiello, Jessica; Han, Xianlin

    2016-07-01

    Extraction of lipids from biological samples is a critical step in lipidomics, especially for shotgun lipidomics where lipid extracts are directly infused into a mass spectrometer. The butanol-methanol (BUME) extraction method was originally developed to extract lipids from plasma samples with 1 % acetic acid. Considering some lipids are sensitive to acidic environments, we modified this protocol by replacing acetic acid with lithium chloride solution and extended the modified extraction to tissue samples. Although no significant reduction of plasmalogen levels in the acidic BUME extracts of rat heart samples was found, the modified method was established to extract various tissue samples, including rat liver, heart, and plasma. Essentially identical profiles of the majority of lipid classes were obtained from the extracts of the modified BUME and traditional Bligh-Dyer methods. However, it was found that neither the original, nor the modified BUME method was suitable for 4-hydroxyalkenal species measurement in biological samples. PMID:27245345

  16. Are extracted materials truly representative of original samples? Impact of C18 extraction on CDOM optical and chemical properties

    Directory of Open Access Journals (Sweden)

    Andrea A Andrew

    2016-02-01

    Full Text Available Some properties of dissolved organic matter (DOM and chromophoric dissolved organic matter (CDOM can be easily measured directly on whole waters, while others require sample concentration and removal of natural salts. To increase CDOM content and eliminate salts, solid phase extraction is often employed. Biases following extraction and elution are inevitable, thus raising the question of how truly representative the extracted material is of the original. In this context, we investigated the wavelength dependence of extraction efficiency for C18 cartridges with respect to CDOM optical properties using samples obtained from the Middle Atlantic Bight (MAB and the Equatorial Atlantic Ocean (EAO. Further, we compared the optical changes of C18 extracts and the corresponding whole water following chemical reduction with sodium borohydride (NaBH4.C18 cartridges preferentially extracted long-wavelength absorbing/emitting material for samples impacted by riverine input. Extraction efficiency overall decreased with offshore distance away from riverine input. Spectral slopes of C18-OM samples were also almost always lower than those of their corresponding CDOM samples supporting the preferential extraction of higher molecular weight absorbing material. The wavelength dependence of the optical properties (absorption, fluorescence emission and quantum yield of the original water samples and their corresponding extracted material were very similar. C18 extracts and corresponding water samples further exhibited comparable optical changes following NaBH4 reduction, thus suggesting a similarity in nature (structure of the optically active extracted material, independent of geographical locale. Altogether, these data suggested a strong similarity between C18 extracts and corresponding whole waters, thus indicating that extracts are representative of the CDOM content of original waters.

  17. Composition of extractable organic matter of air particles from malaysia: Initial study

    Science.gov (United States)

    Bin Abas, M. Radzi; Simoneit, Bernd R. T.

    The solvent extractable compounds of airborne particulate samples, which were collected on two occasions in a suburb of Kuala Lumpur, Malaysia, with a standard high-volume air sampler, were investigated to determine the distributions of homologous and biomarker compounds. These preliminary results show that both samples contain n-alkanes, n-alkanoic acids and n-alkanols as the dominant solvent-extractable components, with minor amounts of n-alkanedioic acids, n-alkanones, terpenoids, sterols, and phthalate contaminants, derived from biogenic sources (vascular plant wax) and from anthropogenic utilization of fossil fuel products (lubricating oil, vehicle fuels, etc.). Some compositional differences are observed in the two samples and greater atmospheric concentrations were found for almost all organic components in the sample collected under hazy conditions. This is interpreted to be due to the local build-up of organic contaminants as a result of atmospheric stability during the haze episode, to atmospheric photochemical reactions, and to some unidentified anthropogenic activities which are peculiar to the city. Some of the organic components are also suspected to be brought in from areas outside the region.

  18. The Sappanwood Extract Drying With Carrier Agent Under Air Dehumidification

    OpenAIRE

    Mohamad Djaeni; Meilya Suzan Triyastuti; Febiani Utari; Arianti Nuur Annisa; Dewi Ayu Novita

    2016-01-01

    The sappanwood extract enriched by brazilin can be used for natural colouring agent in food and beverages. The extract is produced in form of dry powder for consummer convenience as well as prolonging storage life. Currently, the sappanwood extract drying still deals with the product sticky that inhibit water transport in drying. As a result, the drying process needs long time to get moisture content below 10%. The extract drying with carrier agent is an option to break the product sticky and...

  19. The effect of air temperature on the sappan wood extract drying

    Science.gov (United States)

    Djaeni, M.; Triyastuti, M. S.; Asiah, N.; Annisa, A. N.; Novita, D. A.

    2015-12-01

    The sappan wood extract contain natural colour called brazilin that can be used as a food colouring and antioxidant. The product is commonly found as a dry extract powder for consummer convenience. The spray dryer with air dehumidification can be an option to retain the colour and antioxidant agent. This paper discusses the effect of air temperature on sappan wood extract drying that was mixed with maltodextrin. As responses, the particle size, final moisture content, and extract solubility degradation were observed. In all cases, the process conducted in temperature ranging 90 - 110°C can retain the brazilin quality as seen in solubility and particle size. In addition, the sappan wood extract can be fully dried with moisture content below 2%. Moreover, with the increase of air temperature, the particle size of dry extract can be smaller.

  20. Microbial diversity in fecal samples depends on DNA extraction method

    DEFF Research Database (Denmark)

    Mirsepasi, Hengameh; Persson, Søren; Struve, Carsten;

    2014-01-01

    was to evaluate two different DNA extraction methods in order to choose the most efficient method for studying intestinal bacterial diversity using Denaturing Gradient Gel Electrophoresis (DGGE). FINDINGS: In this study, a semi-automatic DNA extraction system (easyMag®, BioMérieux, Marcy I'Etoile, France...

  1. Fractionation of natural radionuclides from soil and sediment samples with sequential extractions

    International Nuclear Information System (INIS)

    Sequential extractions are used to evaluate the mobility and bioavailability of natural radionuclides in the environment as well as their binding and origin in soil. However, as extractions results are dependent on the extraction conditions, it is not possible to find out the exact chemical forms of the radionuclides or their sorption to certain geochemical phases. In sequential extractions the same solid sample is extracted several times with stronger extraction conditions each time. There are many extraction methods but their fractionation is mostly same. Easily exchanged cations are extracted in the first step. In the second step acid-soluble materials are dissolved and in the third step reducible manganese and iron oxyhydroxides are dissolved. In the fourth step the sample is extracted with oxidizing reagent to decompose the oxidisable materials. In the last extraction step the remnant sample is decomposed with strong acids. This study focuses on sequential extractions of Olkiluoto soil samples. Five-step extractions were carried out to find out more information about the sorption of uranium, thorium, radium and lead in the soil. The concentrations of uranium, thorium and stable lead in extraction fractions were determined with inductively coupled plasma mass spectrometry. 210Pb activity concentration was determined by alpha spectrometry through its daughter nuclide 210Po. Fractionation of the radionuclides was found to be dependent on the sample depth and particle size. The largest concentrations of uranium, thorium and lead were found in the smallest particle size samples. (orig.)

  2. Measurement of radon daughters in air samples by alpha spectroscopy

    International Nuclear Information System (INIS)

    The concentration of radon progeny in air has been determined by alpha spectrometry measurement of polonium 214 and polonium 218. A known volume of air was passed through a filter, then the alpha activity was directly measured on this filter (Author)

  3. Extraction of Thermal Performance Values from Samples in the Lunar Dust Adhesion Bell Jar

    Science.gov (United States)

    Gaier, James R.; Siamidis, John; Larkin, Elizabeth M. G.

    2010-01-01

    A simulation chamber has been developed to test the performance of thermal control surfaces under dusty lunar conditions. The lunar dust adhesion bell jar (LDAB) is a diffusion pumped vacuum chamber (10(exp -8) Torr) built to test material samples less than about 7 cm in diameter. The LDAB has the following lunar dust simulant processing capabilities: heating and cooling while stirring in order to degas and remove adsorbed water; RF air-plasma for activating the dust and for organic contaminant removal; RF H/He-plasma to simulate solar wind; dust sieving system for controlling particle sizes; and a controlled means of introducing the activated dust to the samples under study. The LDAB is also fitted with an in situ Xe arc lamp solar simulator, and a cold box that can reach 30 K. Samples of thermal control surfaces (2.5 cm diameter) are introduced into the chamber for calorimetric evaluation using thermocouple instrumentation. The object of this paper is to present a thermal model of the samples under test conditions and to outline the procedure to extract the absorptance, emittance, and thermal efficiency from the pristine and sub-monolayer dust covered samples.

  4. Evaluation of Soxhlet extraction, accelerated solvent extraction and microwave-assisted extraction for the determination of polychlorinated biphenyls and polybrominated diphenyl ethers in soil and fish samples

    International Nuclear Information System (INIS)

    Three commonly applied extraction techniques for persistent organic chemicals, Soxhlet extraction (SE), accelerated solvent extraction (ASE) and microwave-assisted extraction (MAE), were applied on soil and fish samples in order to evaluate their performances. For both PCBs and PBDEs, the two more recent developed techniques (ASE and MAE) were in general capable of producing comparable extraction results as the classical SE, and even higher extraction recoveries were obtained for some PCB congeners with large octanol-water partitioning coefficients (Kow). This relatively uniform extraction results from ASE and MAE indicated that elevated temperature and pressure are favorable to the efficient extraction of PCBs from the solid matrices. For PBDEs, difference between the results from MAE and ASE (or SE) suggests that the MAE extraction condition needs to be carefully optimized according to the characteristics of the matrix and analyte to avoid degradation of higher brominated BDE congeners and improve the extraction yields.

  5. Evaluation of Soxhlet extraction, accelerated solvent extraction and microwave-assisted extraction for the determination of polychlorinated biphenyls and polybrominated diphenyl ethers in soil and fish samples

    Energy Technology Data Exchange (ETDEWEB)

    Wang Pu [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, 18 Shuangqing Road, Beijing 100085 (China); Zhang Qinghua, E-mail: qhzhang@rcees.ac.cn [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, 18 Shuangqing Road, Beijing 100085 (China); Wang Yawei; Wang Thanh; Li Xiaomin; Ding Lei; Jiang Guibin [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, 18 Shuangqing Road, Beijing 100085 (China)

    2010-03-17

    Three commonly applied extraction techniques for persistent organic chemicals, Soxhlet extraction (SE), accelerated solvent extraction (ASE) and microwave-assisted extraction (MAE), were applied on soil and fish samples in order to evaluate their performances. For both PCBs and PBDEs, the two more recent developed techniques (ASE and MAE) were in general capable of producing comparable extraction results as the classical SE, and even higher extraction recoveries were obtained for some PCB congeners with large octanol-water partitioning coefficients (K{sub ow}). This relatively uniform extraction results from ASE and MAE indicated that elevated temperature and pressure are favorable to the efficient extraction of PCBs from the solid matrices. For PBDEs, difference between the results from MAE and ASE (or SE) suggests that the MAE extraction condition needs to be carefully optimized according to the characteristics of the matrix and analyte to avoid degradation of higher brominated BDE congeners and improve the extraction yields.

  6. HPLC-UV-FL PAH analysis in air particulates. Application to La Coruna (Spain) air samples

    Energy Technology Data Exchange (ETDEWEB)

    Pineiro Iglesias, M.; Vasquez Blanco, E.; Lopez Mahia, P.; Muniategui Lorenzo, S.; Prada Rodriguez, D. [A Coruna Univ., A Coruna (Spain). Dept. of Analytical Chemistry

    2000-06-01

    In this paper, a procedure for the determination of airborne polycyclic aromatic hydrocarbons (PAHs) is described. Airborne particulate samples were collected on glass fiber filters which were microwave assisted extracted using hexane/acetone (1:1). The extractable organic matter was submitted to several steps of clean-up procedure by solid phase extraction. The PAH fraction was analyzed by high performance liquid chromatography with ultraviolet (UV) at two fixed wavelengths (254 and 300 nm) and wavelength programmable fluorescence (FL) detection. Analytical method detection limits were in the range from 0.30 to 9.5 pg/m{sup 3} with ultraviolet detection ({lambda}=254 nm) and from 0.035 to 0.86 pg/m{sup 3} with fluorescence detection. Also, the effect of the temperature on the retention of the PAHs is described. [Italian] In questo lavoro e' descritta una procedura per la determinazione degli idrocarburi policiclici aromatici (PAHs) nel particolato atmosferico. I campioni sono stati raccolti su filtri di fibra di vetro dai quali sono stati estratti con l'impiego delle microonde utilizzando esano-acetone (1:1). La materia organica estraibile e' stata sottoposta a vari stadi di una procedura di pulizia mediante cromatografia liquida ad elevata pressione e rivelazione ultravioletta a due lunghezze d'onda fisse (254 e 300 nm) e di fluorescenza a lunghezza d'onda programmabile. I limiti di rivelabilita' del metodo analitico sono nell'intervallo di 0.30-9.5 pg/m{sup 3} per la rilevazione UV (254 nm) e di 0.035-0.86 pg/m{sup 3} per la rivelazione in fluorescenza. E' inoltre descritto l'effetto della temperatura sul trattenimento dei PAHs.

  7. Application of Solid Phase Microextraction followed by Chromatograph-Flame Ionization Detector for Sampling and Analysis of Acetonitrile in Air

    OpenAIRE

    NEMATULLAH KURD; ABDULRAHMAN BAHRAMI; FARSHID GHORBANI-SHAHNA; MAHMOUD HEIDARI

    2015-01-01

    Acetonitrile used as a solvent in manufactures and affects to central nervous system from inhalation exposure. The aim of this study was to develop a micro-solid phase extraction method for the determination of acetonitrile in the air matrix. The sampling was performed with a small diameter fused silica fiber coated with a thin film of stationary phase and was subsequently desorbed and analyzed by gas chromatograph equipped with a flame ionization detector (GC/FID). The effects of laboratory ...

  8. CO2 isotope analyses using large air samples collected on intercontinental flights by the CARIBIC Boeing 767.

    Science.gov (United States)

    Assonov, S S; Brenninkmeijer, C A M; Koeppel, C; Röckmann, T

    2009-03-01

    Analytical details for 13C and 18O isotope analyses of atmospheric CO2 in large air samples are given. The large air samples of nominally 300 L were collected during the passenger aircraft-based atmospheric chemistry research project CARIBIC and analyzed for a large number of trace gases and isotopic composition. In the laboratory, an ultra-pure and high efficiency extraction system and high-quality isotope ratio mass spectrometry were used. Because direct comparison with other laboratories was practically impossible, the extraction and measurement procedures were tested in considerable detail. Extracted CO2 was measured twice vs. two different working reference CO2 gases of different isotopic composition. The two data sets agree well and their distributions can be used to evaluate analytical errors due to isotope measurement, ion corrections, internal calibration consistency, etc. The calibration itself is based on NBS-19 and also verified using isotope analyses on pure CO2 gases (NIST Reference Materials (RMs) and NARCIS CO2 gases). The major problem encountered could be attributed to CO2-water exchange in the air sampling cylinders. This exchange decreased over the years. To exclude artefacts due to such isotopic exchange, the data were filtered to reject negative delta18O(CO2) values. Examples of the results are given. PMID:19219897

  9. Application of air-lifting pump in standard spray-sieve-plates pulsed extraction column

    International Nuclear Information System (INIS)

    The present research aims to determine the application of air-lifting pump in 100 mm diameter standard spray-sieve-plates pulsed extraction column for 30%TRPO/ kerosene solution-1 mol/L HNO3 solution. The liquid flow rate of air-lifting pump, designed for aqueous phase feeding, organic phase feeding and aqueous phase discharging, increases linearly with air flow rate within experimental range, and the submerged ratio of the air-lifting pump for aqueous phase discharging is linear with the holdup of the pulsed extraction column. By combining above results with the online measurement of air-purge method, the steady state of pulsed extraction column is easily controlled. (authors)

  10. On the Methodology of Nematode Extraction from Field Samples: Comparison of Methods for Soil Extraction

    OpenAIRE

    Viglierchio, David R.; Schmitt, Richard V.

    1983-01-01

    The commonly used nematode extraction methods were compared using three soil types and four nematode species. The comparison was repeated in three trials by the same operator to estimate operator reproducibility. Extraction efficiency was dependent upon method, soil type, and nematode species, and reproducibility was not particularly satisfactory for routine analyses. Extraction by any method tested was less than 50% efficient. Quantitative nematode extraction methodology needs serious attent...

  11. AFM fluid delivery/liquid extraction surface sampling/electrostatic spray cantilever probe

    Science.gov (United States)

    Van Berkel, Gary J.

    2015-06-23

    An electrospray system comprises a liquid extraction surface sampling probe. The probe comprises a probe body having a liquid inlet and a liquid outlet, and having a liquid extraction tip. A solvent delivery conduit is provided for receiving solvent liquid from the liquid inlet and delivering the solvent liquid to the liquid extraction tip. An open liquid extraction channel extends across an exterior surface of the probe body from the liquid extraction tip to the liquid outlet. An electrospray emitter tip is in liquid communication with the liquid outlet of the liquid extraction surface sampling probe. A system for analyzing samples, a liquid junction surface sampling system, and a method of analyzing samples are also disclosed.

  12. Extraction of polycyclic aromatic nitrogen heterocycles from spiked soil samples

    Czech Academy of Sciences Publication Activity Database

    Kočí, K.; Petrovská, H.; Šimek, Z.; Varaďová-Ostrá, Elena; Syslová, A.

    2007-01-01

    Roč. 87, č. 2 (2007), s. 111-123. ISSN 0306-7319 Institutional research plan: CEZ:AV0Z40310501 Keywords : polycyclic aromatic nitrogen heterocycle * supercritical fluid extraction * Soxhlet Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 1.026, year: 2007

  13. 32 CFR 806.27 - Samples of Air Force FOIA processing documents.

    Science.gov (United States)

    2010-07-01

    ... review will require policy determinations from different Air Force elements; records describe law... 32 National Defense 6 2010-07-01 2010-07-01 false Samples of Air Force FOIA processing documents. 806.27 Section 806.27 National Defense Department of Defense (Continued) DEPARTMENT OF THE AIR...

  14. Comparative study of modern extraction techniques for the determination of environmental samples (M14)

    International Nuclear Information System (INIS)

    Full text: The aim of any extraction method in analytical chemistry is, to effectively separate the analytes from the matrix. The whole step should be fast and quantitative with minimal solvent and time required. The classical Soxhlet extraction usually requires large volumes (up to 200 ml) of solvent to be refluxed through the solid samples for several hours. Therefore, in the last decades, alternatives for this extraction method have been presented and investigated such as ultrasonic extraction (UE), supercritical fluid extraction (SFE), accelerated solvent extraction (ASE), microwave-assisted extraction (MAE) and fluidized-bed extraction (FBE). The actual choice for analytical application is frequently the initial capital cost, operating costs, simplicity of operation, amount of organic solvent required and sample throughput. Since sample preparation is a critical step in the analytical cycle, special care has to be taken for an accurate choice and optimization of extraction techniques and clean-up procedures. Therefore, MAE and FBE were investigated for their influential extraction parameters and these parameters were optimized for the extraction of organochlorine biocides, polychlorinated biphenyls and polycyclic aromatic hydrocarbons from environmental matrices like soil, sediment and sewage sludge. The extraction yields were compared with those obtained by Soxhlet extraction performed following DIN-methods. Finally, the optimized modern methods were validated by systematic experiments with certified reference materials. Refs. 3 (author)

  15. Practical Method for Extraction of PCR-Quality DNA from Environmental Soil Samples ▿ †

    OpenAIRE

    Kelly A Fitzpatrick; Kersh, Gilbert J.; Massung, Robert F.

    2010-01-01

    Methods for the extraction of PCR-quality DNA from environmental soil samples by using pairs of commercially available kits were evaluated. Coxiella burnetii DNA was detected in spiked soil samples at

  16. HCI Treatment Followed by Bligh and Dyer Extraction Extract More Fatty Acids than Stoldt Fat Extraction in Feed and Fecal Samples

    DEFF Research Database (Denmark)

    Jensen, Søren Krogh; Lauridsen, Charlotte

    HCl Treatment Followed By Bligh and Dyer Extraction Extract More Fatty Acids than Stoldt Fat Extraction in Feed and Fecal Samples., S.K. Jensen, C. Lauridsen, Aarhus University, Faculty of Agricultural Sciences, Tjele, Denmark. The official EU method for fatty acid analysis in feed is based......-15% more total fatty acids and a 30-50% increase in some of the PUFA compared with the official EU method. Thus, besides being much more efficient for extraction of fatty acids, the HCl-Bligh and Dyer method is much faster, and allows inclusion of an internal standard from the beginning of the sample...

  17. Electromembrane extraction as a rapid and selective miniaturized sample preparation technique for biological fluids

    DEFF Research Database (Denmark)

    Gjelstad, Astrid; Pedersen-Bjergaard, Stig; Seip, Knut Fredrik

    2015-01-01

    organic solvent, and into an aqueous receiver solution. The extraction is promoted by application of an electrical field, causing electrokinetic migration of the charged analytes. The method has shown to perform excellent clean-up and selectivity from complicated aqueous matrices like biological fluids......This special report discusses the sample preparation method electromembrane extraction, which was introduced in 2006 as a rapid and selective miniaturized extraction method. The extraction principle is based on isolation of charged analytes extracted from an aqueous sample, across a thin film of....... Technical aspects of electromembrane extraction, important extraction parameters as well as a handful of examples of applications from different biological samples and bioanalytical areas are discussed in the paper....

  18. Sampling strategies for the analysis of reactive low-molecular weight compounds in air

    OpenAIRE

    Henneken, Hartmut

    2006-01-01

    Within this thesis, new sampling and analysis strategies for the determination of airborne workplace contaminants have been developed. Special focus has been directed towards the development of air sampling methods that involve diffusive sampling. In an introductory overview, the current state-of-the-art of sampling and analysis of airborne isocyanates is reviewed. The most important derivatization reagents are introduced, and their application for air analysis with special emphasis on sampli...

  19. Metal Extraction From Soil Samples By chelation in a Microwave System

    OpenAIRE

    Chatreewongsin, Urai

    2000-01-01

    This work involves the combination of chelation and microwave extraction as a technique for extracting adsorbed metals in soil. It has been termed in this work, Chelate Assisted Microwave Extraction (CAME). Unlike other extraction methods, CAME is able to differentiate between anthropological and geological trace metals. The method has been applied to major sample matrices included three types of soils (Bertie Sandy Loam, Davidson Silty Clay, and Davidson Clayey Loam) as well as se...

  20. Technical assessment of compliance with work place air sampling requirements at T Plant. Revision No. 1

    International Nuclear Information System (INIS)

    The US DOE requires its contractors to conduct air sampling to detect and evaluate airborne radioactive material in the workplace. Hanford Reservation T Plant compliance with workplace air sampling requirements has been assessed. Requirements, basis for determining compliance and recommendations are included

  1. Low-cost monitoring of Campylobacter in poultry houses by air sampling and quantitative PCR.

    Science.gov (United States)

    Søndergaard, M S R; Josefsen, M H; Löfström, C; Christensen, L S; Wieczorek, K; Osek, J; Hoorfar, J

    2014-02-01

    The present study describes the evaluation of a method for the quantification of Campylobacter by air sampling in poultry houses. Sampling was carried out in conventional chicken houses in Poland, in addition to a preliminary sampling in Denmark. Each measurement consisted of three air samples, two standard boot swab fecal samples, and one airborne particle count. Sampling was conducted over an 8-week period in three flocks, assessing the presence and levels of Campylobacter in boot swabs and air samples using quantitative real-time PCR. The detection limit for air sampling was approximately 100 Campylobacter cell equivalents (CCE)/m3. Airborne particle counts were used to analyze the size distribution of airborne particles (0.3 to 10 μm) in the chicken houses in relation to the level of airborne Campylobacter. No correlation was found. Using air sampling, Campylobacter was detected in the flocks right away, while boot swab samples were positive after 2 weeks. All samples collected were positive for Campylobacter from week 2 through the rest of the rearing period for both sampling techniques, although levels 1- to 2-log CCE higher were found with air sampling. At week 8, the levels were approximately 10(4) and 10(5) CCE per sample for boot swabs and air, respectively. In conclusion, using air samples combined with quantitative real-time PCR, Campylobacter contamination could be detected earlier than by boot swabs and was found to be a more convenient technique for monitoring and/or to obtain enumeration data useful for quantitative risk assessment of Campylobacter. PMID:24490929

  2. A comparative study of extraction and purification methods for environmental DNA from soil and sludge samples

    OpenAIRE

    Roh, Changhyun; Villatte, Francois; Kim, Byung-Gee; Schmid, Rolf D.

    2006-01-01

    An important prerequisite for a successful metagenome library construction is an efficient extraction procedure for DNA out of environmental samples. In this study we compared three indirect and four direct extraction methods, including a commercial kit, in terms of DNA yield, purity and time requirement. A special focus was set on methods which are appropriate for the extraction of environmental DNA (eDNA) from very limited sample sizes (0.1 g) to enable a highly parallel approach. Direct ex...

  3. Speciation of Pb, Cu and Zn determined by sequential extraction for identification of air pollution sources in Syria

    Science.gov (United States)

    Al-Masri, M. S.; Al-Kharfan, K.; Al-Shamali, K.

    Speciation of three trace elements (Zn, Pb, Cu) in air particulates of two Syrian cities (Tartous and Darya) with different climate conditions and industrial emissions has been studied. Air filters were collected during 2000-2001 and extracted chemically using different selective fluids in an attempt to identify the different forms of trace elements. Approximately 60% of lead in air particulates of both cities was found to be associated with organic materials produced by incomplete burning of vehicles fuels and residential heating; the remaining 40% of lead was as lead oxides and mineral acids soluble compounds. Zinc was found in oxides (28-65%) samples collected in Tartous city, indicating that the Tartous cement factory and phosphate loading cargoes are the main source of emissions. In the Darya filters, zinc associated with organic materials (28-49%) was related to the presence of plastic molding industries and corroding car tires. In addition, copper was also found to be in the form of oxides (19-46%) in both cities in the summer periods, while 13-25% and 35% are associated with organic materials and silicates, respectively. Differences in chemical forms of the studied trace elements in air particulates were found to be related to differences in air pollution sources and differences in human behaviour throughout the year. Therefore, chemical fractionation of trace elements in air particulates using sequential leaching can be used for identification of air pollutions sources in urban and industrial areas.

  4. A modular method for the extraction of DNA and RNA, and the separation of DNA pools from diverse environmental sample types

    DEFF Research Database (Denmark)

    Lever, Mark; Torti, Andrea; Eickenbusch, Philip;

    2015-01-01

    A method for the extraction of nucleic acids from a wide range of environmental samples was developed. This method consists of several modules, which can be individually modified to maximize yields in extractions of DNA and RNA or separations of DNA pools. Modules were designed based on elaborate...... tests, in which permutations of all nucleic acid extraction steps were compared. The final modular protocol is suitable for extractions from igneous rock, air, water, and sediments. Sediments range from high-biomass, organic rich coastal samples to samples from the most oligotrophic region of the world...... DNA pools without cell lysis from intracellular and particle-complexed DNA pools may enable new insights into the cycling and preservation of DNA in environmental samples in the future. A general protocol is outlined, along with recommendations for optimizing this general protocol for specific sample...

  5. Subcritical extraction as sample treatment method for antioxidant screening of various plant extracts

    OpenAIRE

    Hohnová, B. (Barbora); Šťavíková, L. (Lenka); Karásek, P. (Pavel); Roth, M

    2014-01-01

    Pressurized Hot Water Extraction performed in both static and dynamic modes followed by HPLC with UV-ViS detection was employed for fast and efficient determination of rutin and quercetin from various berries. Moreover, the antioxidant power of subcritical extracts applying •DPPH was evaluated.

  6. The analysis of uranium prospecting, mining and extraction plant samples

    International Nuclear Information System (INIS)

    The physical methods for the determination of uranium, such as x-ray fluorescence spectrometry, radiometric analysis, fluorimetric analysis, emission spectrographic analysis, and neutron activation analysis, are discussed as well as the chemical methods for the determination of uranium such as decomposition, spectrophotometric methods and the volumetric determination of U3O8 in ammonium diuranate slurries. The general methods of analysis for plant control is discussed, especially regarding the determination of cobalt, manganese, iron, free acids, chlorides, nitrates, silica, amines, isodecanol, thiocyanates and tetrathionates in uranium solvent extraction and leaching processes

  7. Feasibility of analyzing fine particulate matter in air using solid-phase extraction membranes and dynamic subcritical water extraction.

    Science.gov (United States)

    Tollbäck, Johanna; Bigatá, María Blasco; Crescenzi, Carlo; Ström, Johan

    2008-05-01

    We have evaluated the feasibility of using Empore solid-phase extraction (SPE) membranes as an alternative to conventional techniques for sampling fine airborne particulate matter (PM), including nanoparticles, utilizing a scanning mobility particle sizer (SMPS) and a condensation particle counter to evaluate their efficiency for trapping fine particles in the 10-800 nm size range. The results demonstrate that the membranes can efficiently trap these particles and can then be conveniently packed into an extraction cell and extracted under matrix solid-phase dispersion (MSPD) conditions. The potential utility of sampling PM using Empore membranes followed by dynamic subcritical water extraction (DSWE) for fast, efficient, class-selective extraction of polycyclic aromatic hydrocarbons (PAHs) associated with the particles, prior to changing the solvent and analysis by GC/MS, was then explored. The performance of the method was tested using National Institute of Standards and Technology (NIST)-certified "urban dust" reference material (SRM 1649a) and real samples collected at a site in central Rome with heavy road traffic. The method appears to provide comparable extraction efficiency to that of conventional techniques and with using GC/MS, detection limits ranged in the few picograms per cubic meter level. Sampling PM by Empore membranes may reduce the risks of losses of semivolatile compounds, while allowing relatively high sampling flow rates and safe sample storage. Moreover, the combination of MSPD with DSWE permits specific fractions of the PM components to be eluted, thereby generating clean extracts and reducing both analysis time and sample manipulation. PMID:18393539

  8. Sampling and preparation of air pollutants at the Coal Paiton Power Plant area Probolinggo

    International Nuclear Information System (INIS)

    Sampling has been conducted on April 8 th to 18 th, 2012 at the plant area of Paiton Coal Power Plant using e-sampler for particulated matter PM-2,5 and PM-10, high volume air sampler for total suspended particulate (TSP) at the three sampling locations as the representative pollution. Filter before and after sampling was weighed and extremely guarded contamination. Air filters stored in desiccator filter for 24 hours. Determination of concentration of ambient air pollutants conducted by gravimetric method derived from a reduction in weight the samples on the filter PM-2,5; PM-10 and TSP to the weight of the empty filter. (author)

  9. Simultaneous extraction and clean-up of polychlorinated biphenyls and their metabolites from small tissue samples using pressurized liquid extraction

    OpenAIRE

    Kania-Korwel, Izabela; Zhao, Hongxia; Norstrom, Karin; Li, Xueshu; HORNBUCKLE, KERI C.; Lehmler, Hans-Joachim

    2008-01-01

    A pressurized liquid extraction-based method for the simultaneous extraction and in situ clean-up of polychlorinated biphenyls (PCBs), hydroxylated (OH)-PCBs and methylsulfonyl (MeSO2)-PCBs from small (< 0.5 gram) tissue samples was developed and validated. Extraction of a laboratory reference material with hexane:dichloromethane:methanol (48:43:9, v/v) and Florisil as fat retainer allowed an efficient recovery of PCBs (78–112%; RSD: 13–37%), OH-PCBs (46±2%; RSD: 4%) and MeSO2-PCBs (89±21%; R...

  10. Comparison of stationary and personal air sampling with an air dispersion model for children's ambient exposure to manganese.

    Science.gov (United States)

    Fulk, Florence; Haynes, Erin N; Hilbert, Timothy J; Brown, David; Petersen, Dan; Reponen, Tiina

    2016-09-01

    Manganese (Mn) is ubiquitous in the environment and essential for normal growth and development, yet excessive exposure can lead to impairments in neurological function. This study modeled ambient Mn concentrations as an alternative to stationary and personal air sampling to assess exposure for children enrolled in the Communities Actively Researching Exposure Study in Marietta, OH. Ambient air Mn concentration values were modeled using US Environmental Protection Agency's Air Dispersion Model AERMOD based on emissions from the ferromanganese refinery located in Marietta. Modeled Mn concentrations were compared with Mn concentrations from a nearby stationary air monitor. The Index of Agreement for modeled versus monitored data was 0.34 (48 h levels) and 0.79 (monthly levels). Fractional bias was 0.026 for 48 h levels and -0.019 for monthly levels. The ratio of modeled ambient air Mn to measured ambient air Mn at the annual time scale was 0.94. Modeled values were also time matched to personal air samples for 19 children. The modeled values explained a greater degree of variability in personal exposures compared with time-weighted distance from the emission source. Based on these results modeled Mn concentrations provided a suitable approach for assessing airborne Mn exposure in this cohort. PMID:27168393

  11. Day and night variation in chemical composition and toxicological responses of size segregated urban air PM samples in a high air pollution situation

    Science.gov (United States)

    Jalava, P. I.; Wang, Q.; Kuuspalo, K.; Ruusunen, J.; Hao, L.; Fang, D.; Väisänen, O.; Ruuskanen, A.; Sippula, O.; Happo, M. S.; Uski, O.; Kasurinen, S.; Torvela, T.; Koponen, H.; Lehtinen, K. E. J.; Komppula, M.; Gu, C.; Jokiniemi, J.; Hirvonen, M.-R.

    2015-11-01

    Urban air particulate pollution is a known cause for adverse human health effects worldwide. China has encountered air quality problems in recent years due to rapid industrialization. Toxicological effects induced by particulate air pollution vary with particle sizes and season. However, it is not known how distinctively different photochemical activity and different emission sources during the day and the night affect the chemical composition of the PM size ranges and subsequently how it is reflected to the toxicological properties of the PM exposures. The particulate matter (PM) samples were collected in four different size ranges (PM10-2.5; PM2.5-1; PM1-0.2 and PM0.2) with a high volume cascade impactor. The PM samples were extracted with methanol, dried and thereafter used in the chemical and toxicological analyses. RAW264.7 macrophages were exposed to the particulate samples in four different doses for 24 h. Cytotoxicity, inflammatory parameters, cell cycle and genotoxicity were measured after exposure of the cells to particulate samples. Particles were characterized for their chemical composition, including ions, element and PAH compounds, and transmission electron microscopy (TEM) was used to take images of the PM samples. Chemical composition and the induced toxicological responses of the size segregated PM samples showed considerable size dependent differences as well as day to night variation. The PM10-2.5 and the PM0.2 samples had the highest inflammatory potency among the size ranges. Instead, almost all the PM samples were equally cytotoxic and only minor differences were seen in genotoxicity and cell cycle effects. Overall, the PM0.2 samples had the highest toxic potential among the different size ranges in many parameters. PAH compounds in the samples and were generally more abundant during the night than the day, indicating possible photo-oxidation of the PAH compounds due to solar radiation. This was reflected to different toxicity in the PM

  12. Optimising Bacterial DNA Extraction from Faecal Samples: Comparison of Three Methods

    OpenAIRE

    Smith, Birgitte; Li, Nan; Andersen, Anders Schou; Slotved, Hans Christian; Krogfelt, Karen Angeliki

    2011-01-01

    Culture independent methods are used widely in diagnostic laboratories for infectious disease Isolation of genomic DNA from clinical samples is the first and important step in the procedure. Several procedures for extracting DNA from faecal samples have been described, including different mechanical cell disruptors. To our knowledge, the use of TissueLyser as a mechanical disruptor on faecal samples before DNA extraction has not been previously described. The purpose of the study was to imple...

  13. Development of Radiochemical Analysis of Uranium Isotopes in Soil Samples with Extraction Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Myung Ho; Choi, Guk Sik; Cho, Young Hyun; Lee, Chang Woo [KAERI, Daejeon (Korea, Republic of); Lee, Soo Yong [Hanyang Univ., Seoul (Korea, Republic of)

    2001-03-15

    An accurate and rapid analytical technique of uranium isotopes in highly contaminated soil samples was developed and validated by application to the IAEA-Reference samples. For overcoming the demerits of the TBP extraction method, sample materials were decomposited with HNO{sub 3} and HF, and uranium isotopes were purified by an anion exchange resin and a TRU Spec resin. With the extraction chromatography method, the hindrance elements were completely removed from the uranium fraction. The chemical yields with the extraction chromatography method were more 10% higher than those with the TBP extraction method. The concentrations of uranium isotopes in soil samples using the extraction chromatography method were consistent with the reference values reported by the IAEA.

  14. Dynamic Ultrasound-Assisted Extraction of Catechins and Caffeine in Some Tea Samples

    International Nuclear Information System (INIS)

    A novel dynamic ultrasound-assisted extraction (DUAE) device has been constructed for extraction of five catechins and caffeine in solid sample. The accurate, simple, reproducible and sensitive method for the determination of five catechins and caffeine has been developed and validated. A comparison has been made of the efficiencies by employing DUAE and conventionally static ultrasound-assisted extraction (UAE). The proposed method can not only improve extraction efficiency but also decrease time and solvent consumption. The commercial Chinese tea samples, involving green and black teas, are rapidly analyzed by the proposed DUAE method. The linearity, range, selectivity, precision, accuracy, and robustness also showed acceptable values

  15. Cast Stone Oxidation Front Evaluation: Preliminary Results For Samples Exposed To Moist Air

    Energy Technology Data Exchange (ETDEWEB)

    Langton, C. A.; Almond, P. M.

    2013-11-26

    Cr oxidation front (depth to which soluble Cr was detected) for the Cast Stone sample exposed for 68 days to ambient outdoor temperatures and humid air (total age of sample was 131 days) was determined to be about 35 mm below the top sample surface exposed. The Tc oxidation front, depth at which Tc was insoluble, was not determined. Interpretation of the results indicates that the oxidation front is at least 38 mm below the exposed surface. The sample used for this measurement was exposed to ambient laboratory conditions and humid air for 50 days. The total age of the sample was 98 days. Technetium appears to be more easily oxidized than Cr in the Cast Stone matrix. The oxidized forms of Tc and Cr are soluble and therefore leachable. Longer exposure times are required for both the Cr and Tc spiked samples to better interpret the rate of oxidation. Tc spiked subsamples need to be taken further from the exposed surface to better define and interpret the leachable Tc profile. Finally Tc(VII) reduction to Tc(IV) appears to occur relatively fast. Results demonstrated that about 95 percent of the Tc(VII) was reduced to Tc(IV) during the setting and very early stage setting for a Cast Stone sample cured 10 days. Additional testing at longer curing times is required to determine whether additional time is required to reduce 100 % of the Tc(VII) in Cast Stone or whether the Tc loading exceeded the ability of the waste form to reduce 100 % of the Tc(VII). Additional testing is required for samples cured for longer times. Depth discrete subsampling in a nitrogen glove box is also required to determine whether the 5 percent Tc extracted from the subsamples was the result of the sampling process which took place in air. Reduction capacity measurements (per the Angus-Glasser method) performed on depth discrete samples could not be correlated with the amount of chromium or technetium leached from the depth discrete subsamples or with the oxidation front inferred from soluble

  16. Sample and injection manifolds used to in-place test of nuclear air-cleaning system

    International Nuclear Information System (INIS)

    Objective: According to the regulations of nuclear safety rules and related standards, in-place test of the nuclear air-cleaning systems should be carried out before and during operation of the nuclear facilities, which ensure them to be in good condition. In some special conditions, the use of sample and injection manifolds is required to make the test tracer and ventilating duct air fully mixed, so as to get the on-spot typical sample. Methods: This paper introduces the technology and application of the sample and injection manifolds in nuclear air-cleaning system. Results: Multi point injection and multi point sampling technology as an effective experimental method, has been used in a of domestic and international nuclear facilities. Conclusion: The technology solved the problem of uniformly of on-spot injection and sampling,which plays an important role in objectively evaluating the function of nuclear air-cleaning system. (authors)

  17. Effect of onion extract on corneal haze suppression after air assisted lamellar keratectomy

    OpenAIRE

    Kim, Soohyun; Park, Young Woo; LEE, Euiri; PARK, Sang Wan; Park, Sungwon; Noh, Hyunwoo; Kim, Jong Whi; Seong, Je Kyung; SEO, Kangmoon

    2015-01-01

    This study evaluated the effect of onion extract on corneal haze suppression after applying the air assisted lamellar keratectomy. The air assisted lamellar keratectomy was performed on 24 canine eyes. They were treated with an artificial tear (group C), prednisolone acetate (group P), onion extract (group O) and TGF-β1 (group T) three times per day from 7 to 28 days after the surgery. Corneal haze occurred on the all eyes and was observed beginning 7 days after the surgery. The haze was sign...

  18. method development for extraction, cleaning -up and separation of organic pollutant in extract of contaminated environmental sample

    International Nuclear Information System (INIS)

    separation and determination of organic contaminants in waste is of great importance, where, it is very harmful for the radioactive wastes treatment plant. therefore, direct, versatile and efficient simulation of an analytical method was developed and established for extraction , cleaning-up and separation of some organic pollutants such as; poly chlorinated biphenyls (PCBs) and hexachlorohexane (HCH) either from each other and/or from environmental sample, sediment and/or liquid . the method combines extraction and separation processes of the organic compound from the matrix media using partition chromatography through alumina and silica columns. the used extraction chromatographic system is consisted of 12.5% deactivated alumina column serially connected with 2% deactivated silica bed column. the extraction method was applied for analysis of mixed standard of PCB and HCH in different types of simulated contaminated sample, fortified seas sand samples and deutated soil samples. this method allows the measurements of these contaminants in sediments at trace levels as low as 1.0 μg/g for PCB and HCH with a percent recovery rang 99% ±1.0. HCHs was fully isolated from the PCBs using different eluent . for gas chromatography attached with electron capture detector, determination of PCB and HCH in environmental samples, pre-treatment steps are strongly recommended before measurements

  19. A Procedure for the supercritical fluid extraction of coal samples, with subsequent analysis of extracted hydrocarbons

    Science.gov (United States)

    Kolak, Jonathan J.

    2006-01-01

    Introduction: This report provides a detailed, step-by-step procedure for conducting extractions with supercritical carbon dioxide (CO2) using the ISCO SFX220 supercritical fluid extraction system. Protocols for the subsequent separation and analysis of extracted hydrocarbons are also included in this report. These procedures were developed under the auspices of the project 'Assessment of Geologic Reservoirs for Carbon Dioxide Sequestration' (see http://pubs.usgs.gov/fs/fs026-03/fs026-03.pdf) to investigate possible environmental ramifications associated with CO2 storage (sequestration) in geologic reservoirs, such as deep (~1 km below land surface) coal beds. Supercritical CO2 has been used previously to extract contaminants from geologic matrices. Pressure-temperature conditions within deep coal beds may render CO2 supercritical. In this context, the ability of supercritical CO2 to extract contaminants from geologic materials may serve to mobilize noxious compounds from coal, possibly complicating storage efforts. There currently exists little information on the physicochemical interactions between supercritical CO2 and coal in this setting. The procedures described herein were developed to improve the understanding of these interactions and provide insight into the fate of CO2 and contaminants during simulated CO2 injections.

  20. PRODUCTION OF ACTIVATED CHARCOAL SAMPLER TUBES FOR SAMPLING AIR CONTAMINANTS

    OpenAIRE

    P Nassiri; F Golbabaie; S. Nasseri; M. Mahmoodi; K. Mehrain

    1988-01-01

    The importance of the use of activated charcoal tubes for sampling gases and vapors is very well-known. For producing these tubes in the country, their production started in the laboratory of the department of occupation al health using activated charcoal, polyurethane foam and glass wool and consequently two types of foamed and foamless tubes were produced. To investigate the quality of the raw materials used, 186 tubes were exposed to various proportions of solutions of different volumes of...

  1. PRODUCTION OF ACTIVATED CHARCOAL SAMPLER TUBES FOR SAMPLING AIR CONTAMINANTS

    Directory of Open Access Journals (Sweden)

    P.Nassiri

    1988-08-01

    Full Text Available The importance of the use of activated charcoal tubes for sampling gases and vapors is very well-known. For producing these tubes in the country, their production started in the laboratory of the department of occupation al health using activated charcoal, polyurethane foam and glass wool and consequently two types of foamed and foamless tubes were produced. To investigate the quality of the raw materials used, 186 tubes were exposed to various proportions of solutions of different volumes of known percentages of four compounds of benzene, toluene, O-xylene and P-xlene. The adsorption of various parts of sampler tubes was done by a chemical method using CS2 and the final analysis was done by gas chromatography. The results obtained show that the amount of the above named compounds adsorbed by glass wool and foam in comparison to the activated charcoal isn’t significant (respectively P<0.001 & P,0.05. Also the experiments don’s show any significant differences between the total amount of adsorbed chemicals by charcoal in the back-up layer and the sample layer of the foamed tube and the amount adsorbed in the foamless tube, when treated with various compounds (P,0.001. Considering the equal adsorption of both types of tubes and the advantage of foamed tubes in controlling the time duration and the flow rate of sampling, the foamed type was recommended for production and use.

  2. Efficient Sample Preparation from Complex Biological Samples Using a Sliding Lid for Immobilized Droplet Extractions

    OpenAIRE

    Casavant, Benjamin P.; Guckenberger, David J.; Beebe, David J.; Berry, Scott M

    2014-01-01

    Sample preparation is a major bottleneck in many biological processes. Paramagnetic particles (PMPs) are a ubiquitous method for isolating analytes of interest from biological samples and are used for their ability to thoroughly sample a solution and be easily collected with a magnet. There are three main methods by which PMPs are used for sample preparation: (1) removal of fluid from the analyte-bound PMPs, (2) removal of analyte-bound PMPs from the solution, and (3) removal of the substrate...

  3. Sampling strategies for the analysis of reactive low-molecular weight compounds in air

    NARCIS (Netherlands)

    Henneken, Hartmut

    2006-01-01

    Within this thesis, new sampling and analysis strategies for the determination of airborne workplace contaminants have been developed. Special focus has been directed towards the development of air sampling methods that involve diffusive sampling. In an introductory overview, the current state-of-th

  4. Highly Effective DNA Extraction Method from Fresh, Frozen, Dried and Clotted Blood Samples

    OpenAIRE

    Jaleh Barar; Sina Atashpaz; Abolfazl Barzegari; Vala Kafil; Sepideh Zununi Vahed; Farzaneh Soltanzad; Sara Samadi Shams

    2011-01-01

    Introduction: Today, with the tremendous potential of genomics and other recent advances in science, the role of science to improve reliable DNA extraction methods is more relevant than ever before. The ideal process for genomic DNA extraction demands high quantities of pure, integral and intact genomic DNA (gDNA) from the sample with minimal co-extraction of inhibitors of downstream processes. Here, we report the development of a very rapid, less-hazardous, and high throughput protocol for e...

  5. Saffron Samples of Different Origin: An NMR Study of Microwave-Assisted Extracts

    OpenAIRE

    Sobolev, Anatoly P.; Simone Carradori; Donatella Capitani; Silvia Vista; Agata Trella; Federico Marini; Luisa Mannina

    2014-01-01

    An NMR analytical protocol is proposed to characterize saffron samples of different geographical origin (Greece, Spain, Hungary, Turkey and Italy). A microwave-assisted extraction procedure was developed to obtain a comparable recovery of metabolites with respect to the ISO specifications, reducing the solvent volume and the extraction time needed. Metabolite profiles of geographically different saffron extracts were compared showing significant differences in the content of some metabolites.

  6. Development of Air Sampling Technology by the Atomic Energy Research Establishment, Harwell

    International Nuclear Information System (INIS)

    For many years the Health Physics and Medical Division of the Atomic Energy Research Establishment, Harwell, has pursued a vigorous programme of investigation and development in the field of air-sampling technology. The programme has made important contributions to the development of sampling media, the design of sampling equipment, the characterization of environmental airborne contamination and the interpretation of air-sampling data in terms of personal exposure. These developments form the basis for the present operational and research programmes in this field in the United Kingdom Atomic Energy Authority (U.K.A.E.A). . This paper, which summarizes the advances made in the Harwell laboratories in the above fields, is divided into three sections: 1. Sampling techniques. The development and characterization of glass-fibre filter papers (Stevens and Hounam) with improved surface collection properties has simplified counting procedures and has made ' possible detailed autoradiographic examination of the dust collected. The problem of energy degradation of alpha radiation by absorption in particles and paper has been studied (Stevens and Toureau). Development of charcoal-impregnated papers (Stevens and Hounam) has facilitated the detection and measurement of airborne contamination by iodine vapour. The combination of these papers with granular characoal in the May Pack (May) has given a sampling device which is now in common use for the determination and characterization of atmospheric iodine contamination. The concept and development of the personal air sampler (Sherwood and Greenhalgh) led to a better appreciation of the uncertainties of conventional air sampling and to the first quantitative demonstration of the problems of interpreting air samples in terms of personal inhalation exposure. Work on the design of a size selective head for the personal air sampler has not yet resolved the difficulties. The drawbacks of the cascade impactor as a continuous size

  7. Highly Effective DNA Extraction Method from Fresh, Frozen, Dried and Clotted Blood Samples

    Directory of Open Access Journals (Sweden)

    Jaleh Barar

    2011-09-01

    Full Text Available Introduction: Today, with the tremendous potential of genomics and other recent advances in science, the role of science to improve reliable DNA extraction methods is more relevant than ever before. The ideal process for genomic DNA extraction demands high quantities of pure, integral and intact genomic DNA (gDNA from the sample with minimal co-extraction of inhibitors of downstream processes. Here, we report the development of a very rapid, less-hazardous, and high throughput protocol for extracting of high quality DNA from blood samples. Methods: Dried, clotted and ethylene diamine tetra-acetic acid (EDTA treated fresh and frozen blood samples were extracted using this method in which the quality and integrity of the extracted DNA were corroborated by agarose gel electrophoresis, PCR reaction and DNA digestion using restricted enzyme. The UV spectrophotometric and gel electrophoresis analysis resulted in high A260/A280 ratio (>1.8 with high intactness of DNA. Results: PCR and DNA digestion experiments indicated that the final solutions of extracted DNA contained no inhibitory substances, which confirms that the isolated DNA is of good quality. Conclusion: The high quality and quantity of current method, no enzymatic processing and accordingly its low cost, make it appropriate for DNA extraction not only from human but also from animal blood samples in any molecular biology labs.

  8. A two-step supercritical fluid extraction of polycyclic aromatic hydrocarbons from roadside soil samples.

    Science.gov (United States)

    Lojková, Lea; Sedláková, Jitka; Kubán, Vlastimil

    2005-11-01

    A two-step procedure for the supercritical fluid extraction (SFE) of polycyclic aromatic hydrocarbons from soil samples was developed. The procedure consists of a static supercritical fluid treatment in a closed extraction cell at a high temperature (T=250 or 340degreesC for 20 min) and an SFE with a solvent trapping. During the static phase, the sample is exposed to a supercritical organic solvent (methanol, toluene, dichloromethane, ACN, acetone, and hexane). The solvent penetrates particles of the matrix to substitute strongly bonded molecules and dissolves the analytes in the supercritical phase. At ambient temperature, supercritical fluids became liquid and lost their solvation abilities. Most of the analytes condense on the surface of the particles or on the extraction cell walls without forming strong bonds or penetrating deep into the matrix. Thus, the pretreatment liberates the analytes and they behave similar to those in freshly spiked samples. The common SFE with toluene-modified CO2 as an extraction fluid follows the static phase. With the use of the most suitable extraction phases (toluene, ACN), the extraction efficiency of the combined procedure is much higher (approximately100%). The results of the combined procedure are compared to the SFE procedure of the same untreated sample (difference less than 5%) and to the Soxhlet extraction. The extracts were analyzed using a GC with the flame ionization detection. PMID:16318201

  9. In vitro genotoxicity of PAH mixtures and organic extract from urban air particles

    International Nuclear Information System (INIS)

    , the highest DNA adduct levels were induced by EOM collected in Prague in the winter period, followed by Sofia and Kosice. However, in the summer sampling period, the order was quite opposite: Kosice > Sofia > Prague. When the EOM content per m3 of air was taken into consideration in order to compare real exposures of humans to genotoxic compounds in all three localities, extracts from respirable dust particles collected in Sofia exhibited the highest genotoxicity regardless of the sampling period. The results indicate that most of DNA adducts detected in cells incubated with EOMs have their origin in low concentrations of c-PAHs representing 0.03-0.17% of EOM total mass. Finally, our results suggest that HepG2 cells have a metabolic capacity for PAHs similar to human hepatocytes and represent therefore the best in vitro model for investigating the genotoxic potential of complex mixtures containing PAHs among the three cell lines tested in this study

  10. Determination of chlorophenols in environmental samples using electromembrane extraction and capillary electrophoresis

    OpenAIRE

    Šlampová, Andrea

    2013-01-01

    Combination of electromembrane extraction (EME) with capillary electrophoresis (CE) was used for determination of trace level chlorophenols (CPs) in environmental water samples. The analytes were transported across supported liquid membrane (SLM), composed of 1-ethyl-2-nitrobenzene (ENB), by the application of electrical field. A driving force of 150 V was applied to extract the analytes from neutral sample (donor solution) into strongly alkaline acceptor solutions. The acceptor soluti...

  11. Molecularly Imprinted Solid-Phase Extraction and Liquid Chromatography for Biological Samples

    OpenAIRE

    Möller, Kristina

    2006-01-01

    This thesis focuses on the use of molecularly imprinted polymers as selective sorbents for solid-phase extraction (MISPE). The MISPE methods developed were mainly intended for use with biological samples, such as human urine and blood plasma. These body fluids are complex samples, which often need an effective clean-up step before analysis to reduce the levels of possible interfering substances from the matrix, especially if the analytes are present in trace amounts. Solid-phase extraction (S...

  12. Comparison of Different Extraction Approaches for Heavy Metal Partitioning in Sediment Samples

    Institute of Scientific and Technical Information of China (English)

    M.B.ARAIN1,; T.G.KAZI; M.K.JAMALI; J.A.BAIG; H.I.AFRIDI; N.JALBANI; R.A.SARFRAZ

    2009-01-01

    Three extraction methods,ultrasonic assisted extraction (USE),microwave assisted extraction (MSE),and conven tional single extraction (CSE),in conjunction with the modified three-stage BCR sequential extraction procedure (SEP)were applied to examine the contents of Cd,Cu,Cr,Ni,Pb and Zn from lake sediment samples,to know whether these techniques can reduce extraction time and improve reproducibility.The SEP and developed alternative single extraction methods were validated by the analysis of certified reference material BCR 601.By the use of optimized sonication and microwave conditions,steps 1,2 and 3 of the BCR sequential extraction methods (excluding the hydrogen peroxide digestion in step 3,which was not performed with sonication and microwave) could be completed in 15-30 min and 60150 s,respectively.The recoveries of total extractable metal contents in BCR 601,obtained by three single extractions ranged from 93.3%-102%,88.9%-104% and 81.2%-96.2% for CSE,USE and MSE,respectively.The precision of the single extraction methods was found in the range of 3.7%-9.4% for all metals (n=6).

  13. Microbial diversity in fecal samples depends on DNA extraction method: easyMag DNA extraction compared to QIAamp DNA stool mini kit extraction

    OpenAIRE

    Mirsepasi, Hengameh; Persson, Søren; Struve, Carsten; Andersen, Lee O B; Petersen, Andreas M.; Krogfelt, Karen A.

    2014-01-01

    Background There are challenges, when extracting bacterial DNA from specimens for molecular diagnostics, since fecal samples also contain DNA from human cells and many different substances derived from food, cell residues and medication that can inhibit downstream PCR. The purpose of the study was to evaluate two different DNA extraction methods in order to choose the most efficient method for studying intestinal bacterial diversity using Denaturing Gradient Gel Electrophoresis (DGGE). Findin...

  14. Ice nucleation active particles in continental air samples over Mainz, Germany

    Science.gov (United States)

    Pummer, Bernhard G.; Pöschl, Ulrich; Fröhlich-Nowoisky, Janine

    2016-04-01

    Aerosol particles are of central importance for atmospheric chemistry and physics, climate and public health. Some of these particles possess ice nucleation activity (INA), which is highly relevant for cloud formation and precipitation. In 2010, air filter samples were collected with a high-volume filter sampler separating fine and coarse particles (aerodynamic cut-off diameter 3 μm) in Mainz, Germany. In this study, the INA of the atmospheric particles deposited on these filters was determined. Therefore,they were extracted with ultrapure water, which was then measured in a droplet freezing assay, as described in Fröhlich-Nowoisky et al. (2015). The determined concentration of ice nucleators (INs) was between 0.3 and 2per m³ at 266 K, and between5 and 75 per m³ at 260 K. The INs were further characterized by different treatments, like heating (308 K, 371 K), filtration (0.1 μm, 300 kDa), and digestion with papain (10 mg/ml). We further investigated, which atmospheric conditions (e.g. weather) and distinguished events (e.g. dust storms, volcanic eruptions, and pollen peaks) influenced the number and nature of these INs. Fröhlich-Nowoisky, J., Hill, T. C. J., Pummer, B. G., Yordanova, P., Franc, G. D., and Pöschl, U.: Ice nucleation activity in the widespread soil fungus Mortierella alpina, Biogeosci., 12, 1057-1071, doi:10.5194/bg-12-1057-2015, 2015.

  15. Magnetic hydrophilic-lipophilic balance sorbent for efficient extraction of chemical warfare agents from water samples.

    Science.gov (United States)

    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. PMID:26814366

  16. Influence of various dust sampling and extraction methods on the measurement of airborne endotoxin.

    OpenAIRE

    Douwes, J; Versloot, P.; Hollander, A; Heederik, D; Doekes, G.

    1995-01-01

    The influence of various filter types and extraction conditions on the quantitation of airborne endotoxin with the Limulus amebocyte lysate test was studied by using airborne dusts sampled in a potato processing plant. Samples were collected with an apparatus designed to provide parallel samples. Data from the parallel-sampling experiment were statistically evaluated by using analysis of variance. In addition, the influence of storage conditions on the detectable endotoxin concentration was i...

  17. Extraction and Determination of thorium and its application on Geologic Samples using Trioctyl phos

    International Nuclear Information System (INIS)

    The extraction of thorium from aqueous solution was studied using the organic extractant trioctyl phosphine oxide (TOPO) dissolved in cyclohexane. The parameters affecting the extraction, determination and stripping of Th (IV) included type of extractant, shaking time, extractant concentration, ph, aqueous to organic phase ratio (A/O), temperature, certain interfering ions and stripping agents. Best results were at 0.08 M TOPO, ph 1, 2:1 A/O, shaking time 4 min. at 22±1 degree C. The best factors for stripping process were 2 M H2SO4, 4:1 A/O, shaking time 4 min. at 22±1 degree C. The factors studied were followed by application of the extraction system to extract and determine thorium content from certified reference samples and geologic samples collected from South Eastern Desert, Egypt. Also thorium was separated in a laboratory scale from a representative sample of the geologic comprised six samples in a pure state as thorium oxide. Statistics were performed to evaluate the importance of the data collected and therefore set limitations on each step of the analysis. The final results indicate that the method has high precision and accuracy in addition to be fast and of selective manner

  18. Application of Solid Phase Microextraction followed by Chromatograph-Flame Ionization Detector for Sampling and Analysis of Acetonitrile in Air

    Directory of Open Access Journals (Sweden)

    NEMATULLAH KURD

    2015-10-01

    Full Text Available Acetonitrile used as a solvent in manufactures and affects to central nervous system from inhalation exposure. The aim of this study was to develop a micro-solid phase extraction method for the determination of acetonitrile in the air matrix. The sampling was performed with a small diameter fused silica fiber coated with a thin film of stationary phase and was subsequently desorbed and analyzed by gas chromatograph equipped with a flame ionization detector (GC/FID. The effects of laboratory and sampling parameters were investigated and applied to the determination of acetonitrile in air matrix. The Carboxen/PDMS as thecoating fiber showed better analytical performances compared to the PDMS fiber. Analysis of the data by ANOVA test at a 0.05 level of accuracy showed that the peak area of the sampler was significantly affected by temperature and humidity so that the optimum temperature was 20°C and the optimum humidity was 35%. Besides, the limit of detection (LOD and limit of quantification (LOQ for acetonitrile in the GC system were 0.05 and 0.15 μg/ml, respectively. The solid phase microextraction (SPME has been shown a suitable technique for sampling and analysis of acetonitrile in air. There was a good correlation between the SPME and national institute occupational safety and health (NIOSH 1010 method under the optimum conditions. 

  19. Pre-concentration of uranium from water samples by dispersive liquid-liquid micro-extraction

    International Nuclear Information System (INIS)

    In this study, a simple and rapid dispersive liquid-liquid microextraction (DLLME) was developed for the determination of uranium in water samples prior to high performance liquid chromatography with diode array detection. 1-(2-pyridylazo)-2-naphthol (PAN) was used as complexing agent. The effect of various parameters on the extraction step including type and volume of extraction and dispersive solvents, pH of solution, concentration of PAN, extraction time, sample volume and ionic strength were studied and optimized. Under the optimum conditions, the limit of detection (LOD) and preconcentration factor were 0.3 μg L-1 and 194, respectively. Furthermore, the relative standard deviation of the ten replicate was <2.6%. The developed procedure was then applied to the extraction and determination of uranium in the water samples.

  20. A salting out and resin procedure for extracting Schistosoma mansoni DNA from human urine samples

    Directory of Open Access Journals (Sweden)

    Rodrigues Nilton B

    2010-04-01

    Full Text Available Abstract Background In this paper a simple and cheap salting out and resin (InstaGene matrix® resin - BioRad DNA extraction method from urine for PCR assays is introduced. The DNA of the fluke Schistosoma mansoni was chosen as the target since schistosomiasis lacks a suitable diagnostic tool which is sensitive enough to detect low worm burden. It is well known that the PCR technique provides high sensitivity and specificity in detecting parasite DNA. Therefore it is of paramount importance to take advantage of its excellent performance by providing a simple to handle and reliable DNA extraction procedure, which permits the diagnosis of the disease in easily obtainable urine samples. Findings The description of the extraction procedure is given. This extraction procedure was tested for reproducibility and efficiency in artificially contaminated human urine samples. The reproducibility reached 100%, showing positive results in 5 assay repetitions of 5 tested samples each containing 20 ng DNA/5 ml. The efficiency of the extraction procedure was also evaluated in a serial dilution of the original 20 ng DNA/5 ml sample. Detectable DNA was extracted when it was at a concentration of 1.28 pg DNA/mL, revealing the high efficiency of this procedure. Conclusions This methodology represents a promising tool for schistosomiasis diagnosis utilizing a bio-molecular technique in urine samples which is now ready to be tested under field conditions and may be applicable to the diagnosis of other parasitic diseases.

  1. Assessment of estrogenic activity in PM₁₀ air samples with the ERE-CALUX bioassay: Method optimization and implementation at an urban location in Flanders (Belgium).

    Science.gov (United States)

    Croes, Kim; Debaillie, Pieterjan; Van den Bril, Bo; Staelens, Jeroen; Vandermarken, Tara; Van Langenhove, Kersten; Denison, Michael S; Leermakers, Martine; Elskens, Marc

    2016-02-01

    Endocrine disrupting chemicals represent a broad class of compounds, are widespread in the environment and can pose severe health effects. The objective of this study was to investigate the overall estrogen activating potential of PM10 air samples at an urban location with high traffic incidence in Flanders, using a human in vitro cell bioassay. PM10 samples (n = 36) were collected on glass fiber filters every six days between April 2013 and January 2014 using a high-volume sampler. Extraction was executed with a hexane/acetone mixture before analysis using a recombinant estrogen-responsive human ovarian carcinoma (BG1Luc4E2) cell line. In addition, several samples and procedural blanks were extracted with ultra-pure ethanol or acetonitrile to compare extraction efficiencies. Results were expressed as bioanalytical equivalents (BEQs) in femtogram 17β-estradiol equivalent (fg E2-Eq) per cubic meter of air. High fluctuations in estrogenic activity were observed during the entire sampling period, with mean and median BEQs of 50.7 and 35.9 fg E2-Eq m(-)(3), respectively. Estrogenic activity was measured in more than 70% of the samples and several sample extracts showed both high BEQs and high cytotoxicity, which could not be related to black carbon, PM10 or heavy metal concentrations. At this moment, it remains unclear which substances cause this toxicity, but comparison of results obtained with different extraction solvents indicated that acetone/hexane extracts contained more compounds that were cytotoxic and suppressive of responses than those extracted using ultra-pure ethanol. Although more research is needed, the use of a more polar extraction solvent seems to be advisable. PMID:26383266

  2. Extraction and spectrophotometric determination of uranium in indigenous samples of Bangladesh

    International Nuclear Information System (INIS)

    Uranium has been determined in a number of indigenous geological samples supplied by Nuclear Mineral Division of Institute of Nuclear Science and Technology (INST), Atomic Energy Research Establishment, Savar, Dhaka. Selective extraction followed by spectrophotometric determination has been used for assessment of uranium in the sample matrix. Among the samples so far studied, only the Fultali sample from Sylhet showed substantial uranium content of 1036 ± 26 ppm. The leachability of some prospective samples by dilute sulfuric acid has also been studied. The results showed that uranium in the Fultali sample could be leached almost quantitatively by dilute sulfuric acid, whereas only one fifth of uranium is leachable from low content uranium samples. The analytical parameters involved in the present method of extraction and determination of uranium have been evaluated. (author). 16 refs., 3 tabs., 2 figs

  3. Influence of various dust sampling and extraction methods on the measurement of airborne endotoxin.

    Science.gov (United States)

    Douwes, J; Versloot, P; Hollander, A; Heederik, D; Doekes, G

    1995-05-01

    The influence of various filter types and extraction conditions on the quantitation of airborne endotoxin with the Limulus amebocyte lysate test was studied by using airborne dusts sampled in a potato processing plant. Samples were collected with an apparatus designed to provide parallel samples. Data from the parallel-sampling experiment were statistically evaluated by using analysis of variance. In addition, the influence of storage conditions on the detectable endotoxin concentration was investigated by using commercially available lipopolysaccharides (LPS) and endotoxin-containing house dust extracts. The endotoxin extraction efficiency of 0.05% Tween 20 in pyrogen-free water was seven times higher than that of pyrogen-free water only. Two-times-greater amounts of endotoxin were extracted from glass fiber, Teflon, and polycarbonate filters than from cellulose ester filters. The temperature and shaking intensity during extraction were not related to the extraction efficiency. Repeated freeze (-20 degrees C)-and-thaw cycles with commercial LPS reconstituted in pyrogen-free water had a dramatic effect on the detectable endotoxin level. A 25% loss in endotoxin activity per freeze-thaw cycle was observed. Storage of LPS samples for a period of 1 year at 7 degrees C had no effect on the endotoxin level. House dust extracts showed a decrease of about 20% in the endotoxin level after they had been frozen and thawed for a second time. The use of different container materials (borosilicate glass, "soft" glass, and polypropylene) did not result in different endotoxin levels. This study indicates that the assessment of endotoxin exposure may differ considerably between groups when different sampling, extraction, and storage procedures are employed. PMID:7646014

  4. AN EVALUATION OF SAMPLE DISPERSION MEDIAS USED WITH ACCELERATED SOLVENT EXTRACTION FOR THE EXTRACTION AND RECOVERY OF ARSENICALS FROM LFB AND DORM-2

    Science.gov (United States)

    An accelerated solvent extraction (ASE) device was evaluated as a semi-automated means for extracting arsenicals from quality control (QC) samples and DORM-2 [standard reference material (SRM)]. Unlike conventional extraction procedures, the ASE requires that the sample be dispe...

  5. Determination of persistent organic pollutants in solid environmental samples using accelerated solvent extraction and supercritical fluid extraction. Exhaustive extraction and sorption/desorption studies of PCBs

    Energy Technology Data Exchange (ETDEWEB)

    Bjoerklund, E.

    1998-10-01

    Human activity is constantly causing environmental problems due to production and release of numerous chemicals. A group of compounds of special concern is persistent organic pollutants (POP). These toxic, lipophilic chemicals have a high chemical and biological stability, and tend to accumulate in the lipid phase of living organisms. A major sink for POPs are sediments, and consequently these are important for the distribution of POPs in the aquatic environment. Traditionally, determination of POPs relay on exhaustive extraction using liquid extraction techniques (e.g. Soxhlet extraction developed in the late 19th century) followed by gas chromatographic analysis. Since liquid-solid extraction normally requires large volumes of organic solvents in combination with long extraction times and extract clean-up, there has been an increasing demand for improved technology. This should result in reduced organic solvent consumption and sample preparation time, at the same time improving the environment and cutting costs for POP monitoring. In this thesis two modern techniques with capability of fulfilling at least one of these goals have been investigated: (1) Supercritical Fluid Extraction (SFE), and (2) Accelerated Solvent Extraction (ASE). Polychlorinated biphenyls (PCBs) were chosen as model compounds in all experiments performed on environmental matrices, since they cover a relatively large range of physiochemical parameters. Important parameters influencing the overall extraction efficiency in ASE and SFE, are discussed and illustrated for a large number of sediments. It was demonstrated that, by careful consideration of the experimental parameters, both techniques are capable of replacing old methods such as Soxhlet extraction. ASE is somewhat faster than SFE, but the extracts generated in SFE are much cleaner and can be analyzed without sample clean-up. Consequently the overall sample preparation time may be substantially lower using SFE. However, ASE is important

  6. A modular method for the extraction of DNA and RNA, and the separation of DNA pools from diverse environmental sample types

    Directory of Open Access Journals (Sweden)

    Mark Alexander Lever

    2015-05-01

    Full Text Available A method for the extraction of nucleic acids from a wide range of environmental samples was developed. This method consists of several modules, which can be individually modified to maximize yields in extractions of DNA and RNA or separations of DNA pools. Modules were designed based on elaborate tests, in which permutations of all nucleic acid extraction steps were compared. The final modular protocol is suitable for extractions from igneous rock, air, water, and sediments. Sediments range from high-biomass, organic rich coastal samples to samples from the most oligotrophic region of the world’s oceans and the deepest borehole ever studied by scientific ocean drilling. Extraction yields of DNA and RNA are higher than with widely used commercial kits, indicating an advantage to optimizing extraction procedures to match specific sample characteristics. The ability to separate soluble extracellular DNA pools without cell lysis from intracellular and particle-complexed DNA pools may enable new insights into the cycling and preservation of DNA in environmental samples in the future. A general protocol is outlined, along with recommendations for optimizing this general protocol for specific sample types and research goals.

  7. Development of a multicopter-carried whole air sampling apparatus and its applications in environmental studies.

    Science.gov (United States)

    Chang, Chih-Chung; Wang, Jia-Lin; Chang, Chih-Yuan; Liang, Mao-Chang; Lin, Ming-Ren

    2016-02-01

    To advance the capabilities of probing chemical composition aloft, we designed a lightweight remote-controlled whole air sampling component (WASC) and integrated it into a multicopter drone with agile maneuverability to perform aerial whole air sampling. A field mission hovering over an exhaust shaft of a roadway tunnel to collect air samples was performed to demonstrate the applicability of the multicopter-carried WASC apparatus. Ten aerial air samples surrounding the shaft vent were collected by the multicopter-carried WASC. Additional five samples were collected manually inside the shaft for comparison. These samples were then analyzed in the laboratory for the chemical composition of 109 volatile organic compounds (VOCs), CH4, CO, CO2, or CO2 isotopologues. Most of the VOCs in the upwind samples (the least affected by shaft exhaust) were low in concentrations (5.9 ppbv for total 109 VOCs), posting a strong contrast to those in the shaft exhaust (235.8 ppbv for total 109 VOCs). By comparing the aerial samples with the in-shaft samples for chemical compositions, the influence of the shaft exhaust on the surrounding natural air was estimated. Through the aerial measurements, three major advantages of the multicopter-carried WASC were demonstrated: 1. The highly maneuverable multicopter-carried WASC can be readily deployed for three-dimensional environmental studies at a local scale (0-1.5 km); 2. Aerial sampling with superior sample integrity and preservation conditions can now be performed with ease; and 3. Data with spatial resolution for a large array of gaseous species with high precision can be easily obtained. PMID:26386435

  8. Comparison of Soxhlet and Shake Extraction of Polycyclic Aromatic Hydrocarbons from Coal Tar Polluted Soils Sampled in the Field

    DEFF Research Database (Denmark)

    Lindhardt, Bo; Holst, Helle; Christensen, Thomas Højlund

    1994-01-01

    This study compares three extraction methods for PAHs in coal tar polluted soil: 3-times repeated shaking of the soil with dichloromethane-methanol (1:1), Soxhlet extraction with dichloromethane, and Soxhlet extraction with dichloromethane followed by Soxhlet extraction with methanol. The...... extraction efficiencies were determined for ten selected PAHs in triplicate samples of six soils sampled at former gasworks sites. The samples covered a wide range of PAH concentrations, from 0.6 to 397 mg/kg soil. Soxhlet extraction with dichloromethane followed by Soxhlet extraction with methanol, in...

  9. Impacted canine extraction by ridge expansion using air scaler surgical instruments: a case report.

    Science.gov (United States)

    Agabiti, Ivo; Bernardello, Fabio; Nevins, Myron; Wang, Hom-Lay

    2014-01-01

    The presence of an impacted tooth interferes with ideal implant placement. In such cases, atraumatic extraction is recommended in order to avoid difficult and complex bone regeneration procedures. In the present case report, a novel surgical approach to extract a horizontally impacted canine using an edentulous ridge expansion (ERE) technique and air scaler surgical devices is described. A 74-year-old female patient had a maxillary left horizontally impacted canine. The tooth was extracted after elevating a partial-thickness flap and performing an ERE technique using air scaler surgical instruments. The impacted tooth was fragmented through the breach created in the expanded ridge, and the fragments were carefully removed. A suitably sized implant was placed at the time of surgery. The treated site healed without complication. The implant was integrated, successfully restored, and stable after a 3-year follow-up period. This case report demonstrates a novel surgical approach to extract an impacted canine through ridge expansion, using air scaler surgical devices that allow implant placement in an ideal position. PMID:25171039

  10. Accelerated solvent extraction (ASE) - a fast and automated technique with low solvent consumption for the extraction of solid samples (T12)

    International Nuclear Information System (INIS)

    Full text: Accelerated solvent extraction (ASE) is a modern extraction technique that significantly streamlines sample preparation. A common organic solvent as well as water is used as extraction solvent at elevated temperature and pressure to increase extraction speed and efficiency. The entire extraction process is fully automated and performed within 15 minutes with a solvent consumption of 18 ml for a 10 g sample. For many matrices and for a variety of solutes, ASE has proven to be equivalent or superior to sonication, Soxhlet, and reflux extraction techniques while requiring less time, solvent and labor. First ASE has been applied for the extraction of environmental hazards from solid matrices. Within a very short time ASE was approved by the U.S. EPA for the extraction of BNAs, PAHs, PCBs, pesticides, herbicides, TPH, and dioxins from solid samples in method 3545. Especially for the extraction of dioxins the extraction time with ASE is reduced to 20 minutes in comparison to 18 h using Soxhlet. In food analysis ASE is used for the extraction of pesticide and mycotoxin residues from fruits and vegetables, the fat determination and extraction of vitamins. Time consuming and solvent intensive methods for the extraction of additives from polymers as well as for the extraction of marker compounds from herbal supplements can be performed with higher efficiencies using ASE. For the analysis of chemical weapons the extraction process and sample clean-up including derivatization can be automated and combined with GC-MS using an online ASE-APEC-GC system. (author)

  11. Characterization of citrus pectin samples extracted under different conditions: influence of acid type and pH of extraction

    DEFF Research Database (Denmark)

    Kaya, Merve; Sousa, Antonio G.; Crepeau, Marie-Jeanne;

    2014-01-01

    on fruit peel, a waste product from the juicing industry, in which thousands of tons of citrus are processed worldwide every year. This study examines how pectin components vary in relation to the plant source (orange, lemon, lime, grapefruit) and considers the influence of extraction conditions on......Background and Aims Pectin is a complex macromolecule, the fine structure of which is influenced by many factors. It is used as a gelling, thickening and emulsifying agent in a wide range of applications, from food to pharmaceutical products. Current industrial pectin extraction processes are based...... the chemical and macromolecular characteristics of pectin samples. Methods Citrus peel (orange, lemon, lime and grapefruit) from a commercial supplier was used as raw material. Pectin samples were obtained on a bulk plant scale (kilograms; harsh nitric acid, mild nitric acid and harsh oxalic acid...

  12. Determination of sequential extracted uranium speciation in geological samples with HR-ICP-MS method

    International Nuclear Information System (INIS)

    This paper presents a method of determing uranium speciation in geological samples by means of sequential extraction procedure with HR-ICP-MS and its application to sandstone uranium exploration. The extraction chemical procedure is modified from Tessier, uranium in sample is classified into five speclarion: exchangeable, bound to carbonates, bound to Fe-Mn oxides, bound to sulfide-organic matter, and residual. The uranium is extracted respectively and the extractants are measured by the high-resolution inductively coupled mass spectrometry (HR-ICP-MS) with high sensitivity and low background. The extraction procedure has been proved to be satisfactory by means of national reference standard materials, international reference standard materials, and artificial uranium mine sample. Experiment results obtained on replicate samples demonstrate that the relative standard deviation (RSD) of the sequential extraction procedure followed by HR-ICP-MS is 2.6 % for bound to carbonates, 4.0% for bound to sulfide -organic matter, 6.0% for residual, 6.1% bound to Fe-Mn oxides, and 26% for exchangeable fraction. The ratio of uranium in bound to uranium carbonates in residual can be used to indicated the probability of buried uranium deposit. (authors)

  13. Evaluating leaf litter beetle data sampled by Winkler extraction from Atlantic forest sites in southern Brazil

    Directory of Open Access Journals (Sweden)

    Philipp Werner Hopp

    2011-06-01

    Full Text Available Evaluating leaf litter beetle data sampled by Winkler extraction from Atlantic forest sites in southern Brazil. To evaluate the reliability of data obtained by Winkler extraction in Atlantic forest sites in southern Brazil, we studied litter beetle assemblages in secondary forests (5 to 55 years after abandonment and old-growth forests at two seasonally different points in time. For all regeneration stages, species density and abundance were lower in April compared to August; but, assemblage composition of the corresponding forest stages was similar in both months. We suggest that sampling of small litter inhabiting beetles at different points in time using the Winkler technique reveals identical ecological patterns, which are more likely to be influenced by sample incompleteness than by differences in their assemblage composition. A strong relationship between litter quantity and beetle occurrences indicates the importance of this variable for the temporal species density pattern. Additionally, the sampled beetle material was compared with beetle data obtained with pitfall traps in one old-growth forest. Over 60% of the focal species captured with pitfall traps were also sampled by Winkler extraction in different forest stages. Few beetles with a body size too large to be sampled by Winkler extraction were only sampled with pitfall traps. This indicates that the local litter beetle fauna is dominated by small species. Hence, being aware of the exclusion of large beetles and beetle species occurring during the wet season, the Winkler method reveals a reliable picture of the local leaf litter beetle community.

  14. Pesticide detection in air samples from contrasted houses and in their inhabitants' hair.

    Science.gov (United States)

    Raeppel, Caroline; Salquèbre, Guillaume; Millet, Maurice; Appenzeller, Brice M R

    2016-02-15

    In order to identify associations between indoor air contamination and human exposure to pesticides, hair samples from 14 persons (9 adults and 5 children below 12 years) were collected simultaneously with the air of their 5 contrasted houses. Three houses were situated in Alsace (France), one in Lorraine (France) and one in Luxembourg (Luxembourg). Houses were located in urban (n=3), semi-urban (n=1) and rural areas (n=1). Twenty five (25) pesticides were detected at least once in indoor air samples and 20 pesticides were detected at least once in hair samples. The comparison between hair and air samples for the same sampling periods shows that pesticides detected in the two matrices were not necessarily associated. Exposure profiles varied from one home to another but also between inhabitants of the same home, suggesting that exposure can be different between inhabitants of the same home. This study demonstrated the usefulness and the complementarity of hair analysis, for the personalized biomonitoring of people exposure to pesticides, and air analysis, for the identification of airborne exposure and house contamination. PMID:26706757

  15. COMPARISONS OF SOXHLET EXTRACTION, PRESSURIZED LIQUID EXTRACTION, SUPERCRITICAL FLUID EXTRACTION, AND SUBCRITICAL WATER EXTRACTION FOR ENVIRONMENTAL SOLIDS: RECOVERY, SELECTIVITY, AND EFFECTS ON SAMPLE MATRIX. (R825394)

    Science.gov (United States)

    Extractions of a polycyclic aromatic hydrocarbon (PAH)-contaminated soil from a former manufactured gas plant site were performed with a Soxhlet apparatus (18 h), by pressurized liquid extraction (PLE) (50 min at 100°C), supercritical fluid extraction (SFE) (1 h at 150°...

  16. Comparison of sampling methods for radiocarbon dating of carbonyls in air samples via accelerator mass spectrometry

    Science.gov (United States)

    Schindler, Matthias; Kretschmer, Wolfgang; Scharf, Andreas; Tschekalinskij, Alexander

    2016-05-01

    Three new methods to sample and prepare various carbonyl compounds for radiocarbon measurements were developed and tested. Two of these procedures utilized the Strecker synthetic method to form amino acids from carbonyl compounds with either sodium cyanide or trimethylsilyl cyanide. The third procedure used semicarbazide to form crystalline carbazones with the carbonyl compounds. The resulting amino acids and semicarbazones were then separated and purified using thin layer chromatography. The separated compounds were then combusted to CO2 and reduced to graphite to determine 14C content by accelerator mass spectrometry (AMS). All of these methods were also compared with the standard carbonyl compound sampling method wherein a compound is derivatized with 2,4-dinitrophenylhydrazine and then separated by high-performance liquid chromatography (HPLC).

  17. Measurements of an ion beam diameter extracted into air through a large-bore metal capillary

    Energy Technology Data Exchange (ETDEWEB)

    Hirano, Y.; Umigishi, M. [Graduate School of Humanities and Sciences, Nara Women’s University, Nara 630-8506 (Japan); Ishii, K.; Ogawa, H. [Department of Physics, Nara Women’s University, Nara 630-8506 (Japan)

    2015-07-01

    To extract an ion beam into air, the technique using a single macro-capillary has been paid attention. We have expanded the bore of the metal capillary up to 500 μm∅ inlet diameter to increase the beam intensity and have measured the intensity distributions of the extracted 3 MeV proton beam. Furthermore, we have tilted the capillary angle and measured the intensity distributions of the ion beam. In this article, we will present the experimental results together with the simulation which takes the tilt angles of the capillary into account.

  18. Measurements of an ion beam diameter extracted into air through a large-bore metal capillary

    International Nuclear Information System (INIS)

    To extract an ion beam into air, the technique using a single macro-capillary has been paid attention. We have expanded the bore of the metal capillary up to 500 μm∅ inlet diameter to increase the beam intensity and have measured the intensity distributions of the extracted 3 MeV proton beam. Furthermore, we have tilted the capillary angle and measured the intensity distributions of the ion beam. In this article, we will present the experimental results together with the simulation which takes the tilt angles of the capillary into account

  19. Fabric phase sorptive extraction: Two practical sample pretreatment techniques for brominated flame retardants in water.

    Science.gov (United States)

    Huang, Guiqi; Dong, Sheying; Zhang, Mengfei; Zhang, Haihan; Huang, Tinglin

    2016-09-15

    Sample pretreatment is the critical section for residue monitoring of hazardous pollutants. In this paper, using the cellulose fabric as host matrix, three extraction sorbents such as poly (tetrahydrofuran) (PTHF), poly (ethylene glycol) (PEG) and poly (dimethyldiphenylsiloxane) (PDMDPS), were prepared on the surface of the cellulose fabric. Two practical extraction techniques including stir bar fabric phase sorptive extraction (stir bar-FPSE) and magnetic stir fabric phase sorptive extraction (magnetic stir-FPSE) have been designed, which allow stirring of fabric phase sorbent during the whole extraction process. In the meantime, three brominated flame retardants (BFRs) [tetrabromobisphenol A (TBBPA), tetrabromobisphenol A bisallylether (TBBPA-BAE), tetrabromobisphenol A bis(2,3-dibromopropyl)ether (TBBPA-BDBPE)] in the water sample were selected as model analytes for the practical evaluation of the proposed two techniques using high-performance liquid chromatography (HPLC). Moreover, various experimental conditions affecting extraction process such as the type of fabric phase, extraction time, the amount of salt and elution conditions were also investigated. Due to the large sorbent loading capacity and unique stirring performance, both techniques possessed high extraction capability and fast extraction equilibrium. Under the optimized conditions, high recoveries (90-99%) and low limits of detection (LODs) (0.01-0.05 μg L(-1)) were achieved. In addition, the reproducibility was obtained by evaluating the intraday and interday precisions with relative standard deviations (RSDs) less than 5.1% and 6.8%, respectively. The results indicated that two pretreatment techniques were promising and practical for monitoring of hazardous pollutants in the water sample. Due to low solvent consumption and high repeated use performance, proposed techniques also could meet green analytical criteria. PMID:27300591

  20. Methodologies for the Extraction of Phenolic Compounds from Environmental Samples: New Approaches

    Directory of Open Access Journals (Sweden)

    Cristina Mahugo Santana

    2009-01-01

    Full Text Available Phenolic derivatives are among the most important contaminants present in the environment. These compounds are used in several industrial processes to manufacture chemicals such as pesticides, explosives, drugs and dyes. They also are used in the bleaching process of paper manufacturing. Apart from these sources, phenolic compounds have substantial applications in agriculture as herbicides, insecticides and fungicides. However, phenolic compounds are not only generated by human activity, but they are also formed naturally, e.g., during the decomposition of leaves or wood. As a result of these applications, they are found in soils and sediments and this often leads to wastewater and ground water contamination. Owing to their high toxicity and persistence in the environment, both, the US Environmental Protection Agency (EPA and the European Union have included some of them in their lists of priority pollutants. Current standard methods of phenolic compounds analysis in water samples are based on liquid–liquid extraction (LLE while Soxhlet extraction is the most used technique for isolating phenols from solid matrices. However, these techniques require extensive cleanup procedures that are time-intensive and involve expensive and hazardous organic solvents, which are undesirable for health and disposal reasons. In the last years, the use of news methodologies such as solid-phase extraction (SPE and solid-phase microextraction (SPME have increased for the extraction of phenolic compounds from liquid samples. In the case of solid samples, microwave assisted extraction (MAE is demonstrated to be an efficient technique for the extraction of these compounds. In this work we review the developed methods in the extraction and determination of phenolic derivatives in different types of environmental matrices such as water, sediments and soils. Moreover, we present the new approach in the use of micellar media coupled with SPME process for the

  1. Methods for Integrated Air Sampling and DNA Analysis for Detection of Airborne Fungal Spores

    OpenAIRE

    Williams, Roger H.; Ward, Elaine; McCartney, H. Alastair

    2001-01-01

    Integrated air sampling and PCR-based methods for detecting airborne fungal spores, using Penicillium roqueforti as a model fungus, are described. P. roqueforti spores were collected directly into Eppendorf tubes using a miniature cyclone-type air sampler. They were then suspended in 0.1% Nonidet P-40, and counted using microscopy. Serial dilutions of the spores were made. Three methods were used to produce DNA for PCR tests: adding untreated spores to PCRs, disrupting spores (fracturing of s...

  2. Lyophyllization improves the extraction of PCR-quality community DNA from pig faecal samples

    OpenAIRE

    Ruiz, Raquel; Luis A. Rubio

    2012-01-01

    BACKGROUND. Faeces are increasingly used as sources of DNA for genetic and ecological studies. Although multiple methods to preserve faecal samples prior to DNA extraction have been used (e.g. 70 % or absolute ethanol, freezing at -20ºC or in liquid nitrogen) no information is at present available in the literature on the use of lyophilized faeces. Accordingly, the yield and quality of the community DNA obtained by using four different commercial DNA extraction kits (QIAamp DNA Stool Mini Kit...

  3. Reliability of non-invasive tissue sampling methods for DNA extraction in rabbits (Oryctolagus Cuniculus)

    OpenAIRE

    Manel Ben Larbi; Tircazes, A.; K. Feve; TUDELA, F.; Bolet, G

    2012-01-01

    Deoxyribonucleic acid (DNA) can be extracted from different tissue sources. The most common is blood, but in some situations it can be easier to take a biopsy. In some cases when it is difficult to capture animals, especially in wild populations, faeces and hairs can be considered as a source of DNA. This paper presents a pilot study conducted to compare the applicability of invasive and non-invasive sampling methods for extracting DNA for use in genetic studies of rabbits (Oryctolagus cunicu...

  4. Evaluating leaf litter beetle data sampled by Winkler extraction from Atlantic forest sites in southern Brazil

    OpenAIRE

    Philipp Werner Hopp; Edilson Caron; Richard Ottermanns; Martina Roß-Nickoll

    2011-01-01

    Evaluating leaf litter beetle data sampled by Winkler extraction from Atlantic forest sites in southern Brazil. To evaluate the reliability of data obtained by Winkler extraction in Atlantic forest sites in southern Brazil, we studied litter beetle assemblages in secondary forests (5 to 55 years after abandonment) and old-growth forests at two seasonally different points in time. For all regeneration stages, species density and abundance were lower in April compared to August; but, assemblage...

  5. Antioxidant activity of portuguese honey samples: different contribution of the entire honey and phenolic extract

    OpenAIRE

    Ferreira, Isabel C. F. R.; Aires, Edmur; Barreira, João C. M.; Estevinho, Leticia M.

    2009-01-01

    The antioxidant activity of Portuguese honeys was evaluated considering the different contribution of entire samples and phenolic extracts. Several chemical and biochemical assays were used to screen the antioxidant properties of entire honeys with different colour intensity and phenolic extracts: reducing power, 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical-scavenging capacity, and inhibition of lipid peroxidation using the b-carotene linoleate model system and the thiobarbituric ...

  6. On the Methodology of Nematode Extraction from Field Samples: Density Flotation Techniques

    OpenAIRE

    Viglierchio, David R.; Yamashita, Tom T.

    1983-01-01

    Density flotation has been frequently used for the extraction of nematodes from field samples. Density flotation curves for four nematode species and five solutes have been prepared. The curves confirm that flotation was governed by several factors: solute density, solute osmotic activity, and physiological properties of the nematode species. Nematode viability and function can be adversely affected by improper selection of solute for density extraction of nematodes; nevertheless, some nemato...

  7. Single column sequential extraction of Ra, Nd, Th, Pa and U from a natural sample

    OpenAIRE

    Jeandel, C.; Venchiarutti, C.; Bourquin, M.; Pradoux, C; Lacan, F.; P. van Beek; Riotte, Jean

    2011-01-01

    A new procedure allowing the sequential extraction of Ra, Nd, Th, Pa and U from the same initial natural sample (sea or river waters, particles, sediments, rocks) is proposed. Extraction recoveries were better than 90%. Procedural blanks ranged from 80 pg (for Nd) to below 1 fg, the detection limit of the MC-ICP-MS used (for Pa); all were negligible compared with the amounts of elements currently determined. Based on classical anionic resins attached to a peristaltic pump allowing precise flo...

  8. Double use of focused microwave irradiation for accelerated matrix hydrolysis and lipid extraction in milk samples

    International Nuclear Information System (INIS)

    Irradiation with microwave energy has allowed to carry out the extraction of lipids from milk samples (namely, cow, goat and sheep) with quantitative results similar to the Weibull–Berntrop extraction procedure but milk fat obtained by microwave assisted extraction undergoes lesser chemical transformation of triglycerides during the whole process. A considerable reduction of the procedure time (50 min versus 10 h) is achieved with similar reproducibility to that provided by the conventional method. An in situ’ solvent recycling step makes the method environmentally clean

  9. Fractionation of plutonium in environmental and bio-shielding concrete samples using dynamic sequential extraction

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin

    2010-01-01

    Fractionation of plutonium isotopes (238Pu, 239,240Pu) in environmental samples (i.e. soil and sediment) and bio-shielding concrete from decommissioning of nuclear reactor were carried out by dynamic sequential extraction using an on-line sequential injection (SI) system combined with a specially...... designed extraction column. Plutonium in the fractions from the sequential extraction was separated by ion exchange chromatography and measured using alpha spectrometry. The analytical results show a higher mobility of plutonium in bio-shielding concrete, which means attention should be paid...

  10. Determination of metals in air samples using X-Ray fluorescence associated the APDC preconcentration technique

    International Nuclear Information System (INIS)

    Air pollution has become one of the leading quality degradation factors of life for people in large urban centers. Studies indicate that the suspended particulate matter in the atmosphere is directly associated with risks to public health, in addition, it can cause damage to fauna, flora and public / cultural patrimonies. The inhalable particulate materials can cause the emergence and / or worsening of chronic diseases related to respiratory system and other diseases, such as reduced physical strength. In this study, we propose a new method to measure the concentration of total suspended particulate matter (TSP) in the air using an impinger as an air cleaning apparatus, preconcentration with APDC and Total Reflection X-ray Fluorescence technique (TXRF) to analyze the heavy metals present in the air. The samples were collected from five random points in the city of Rio de Janeiro/Brazil. Analyses of TXRF were performed at the Brazilian Synchrotron Light Laboratory (LNLS). The technique proved viable because it was able to detect five important metallic elements to environmental studies: Cr, Fe, Ni, Cu and Zn. This technique presented substantial efficiency in determining the elementary concentration of air pollutants, in addition to low cost. It can be concluded that the metals analysis technique in air samples using an impinger as sample collection instrument associated with a complexing agent (APDC) was viable because it is a low-cost technique, moreover, it was possible the detection of five important metal elements in environmental studies associated with industrial emissions and urban traffic. (author)

  11. Determination of metals in air samples using X-Ray fluorescence associated the APDC preconcentration technique

    Energy Technology Data Exchange (ETDEWEB)

    Nardes, Raysa C.; Santos, Ramon S.; Sanches, Francis A.C.R.A.; Gama Filho, Hamilton S.; Oliveira, Davi F.; Anjos, Marcelino J., E-mail: rc.nardes@gmail.com, E-mail: ramonziosp@yahoo.com.br, E-mail: francissanches@gmail.com, E-mail: hamiltongamafilho@hotmail.com, E-mail: davi.oliveira@uerj.br, E-mail: marcelin@uerj.br [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil). Instituto de Fisica. Departamento de Fisica Aplicada e Termodinamica

    2015-07-01

    Air pollution has become one of the leading quality degradation factors of life for people in large urban centers. Studies indicate that the suspended particulate matter in the atmosphere is directly associated with risks to public health, in addition, it can cause damage to fauna, flora and public / cultural patrimonies. The inhalable particulate materials can cause the emergence and / or worsening of chronic diseases related to respiratory system and other diseases, such as reduced physical strength. In this study, we propose a new method to measure the concentration of total suspended particulate matter (TSP) in the air using an impinger as an air cleaning apparatus, preconcentration with APDC and Total Reflection X-ray Fluorescence technique (TXRF) to analyze the heavy metals present in the air. The samples were collected from five random points in the city of Rio de Janeiro/Brazil. Analyses of TXRF were performed at the Brazilian Synchrotron Light Laboratory (LNLS). The technique proved viable because it was able to detect five important metallic elements to environmental studies: Cr, Fe, Ni, Cu and Zn. This technique presented substantial efficiency in determining the elementary concentration of air pollutants, in addition to low cost. It can be concluded that the metals analysis technique in air samples using an impinger as sample collection instrument associated with a complexing agent (APDC) was viable because it is a low-cost technique, moreover, it was possible the detection of five important metal elements in environmental studies associated with industrial emissions and urban traffic. (author)

  12. An automatic device for sample insertion and extraction to/from reactor irradiation facilities

    International Nuclear Information System (INIS)

    At the previous European Triga Users Conference in Vienna,a paper was given describing a new handling tool for irradiated samples at the L.E.N.A plant. This tool was the first part of an automatic device for the management of samples to be irradiated in the TRIGA MARK ii reactor and successively extracted and stored. So far sample insertion and extraction to/from irradiation facilities available on reactor top (central thimble,rotatory specimen rack and channel f),has been carried out manually by reactor and health-physics operators using the ''traditional'' fishing pole provided by General Atomic, thus exposing reactor personnel to ''unjustified'' radiation doses. The present paper describes the design and the operation of a new device, a ''robot''type machine,which, remotely operated, takes care of sample insertion into the different irradiation facilities,sample extraction after irradiation and connection to the storage pits already described. The extraction of irradiated sample does not require the presence of reactor personnel on the reactor top and,therefore,radiation doses are strongly reduced. All work from design to construction has been carried out by the personnel of the electronic group of the L.E.N.A plant. (orig.)

  13. Technical basis and evaluation criteria for an air sampling/monitoring program

    International Nuclear Information System (INIS)

    Air sampling and monitoring programs at DOE facilities need to be reviewed in light of revised requirements and guidance found in, for example, DOE Order 5480.6 (RadCon Manual). Accordingly, the Oak Ridge National Laboratory (ORNL) air monitoring program is being revised and placed on a sound technical basis. A draft technical basis document has been written to establish placement criteria for instruments and to guide the ''retrospective sampling or real-time monitoring'' decision. Facility evaluations are being used to document air sampling/monitoring needs, and instruments are being evaluated in light of these needs. The steps used to develop this program and the technical basis for instrument placement are described

  14. Ultimate detectability of volatile organic compounds: how much further can we reduce their ambient air sample volumes for analysis?

    Science.gov (United States)

    Kim, Yong-Hyun; Kim, Ki-Hyun

    2012-10-01

    To understand the ultimately lowest detection range of volatile organic compounds (VOCs) in air, application of a high sensitivity analytical system was investigated by coupling thermal desorption (TD) technique with gas chromatography (GC) and time-of-flight (TOF) mass spectrometry (MS). The performance of the TD-GC/TOF MS system was evaluated using liquid standards of 19 target VOCs prepared in the range of 35 pg to 2.79 ng per μL. Studies were carried out using both total ion chromatogram (TIC) and extracted ion chromatogram (EIC) mode. EIC mode was used for calibration to reduce background and to improve signal-to-noise. The detectability of 19 target VOCs, if assessed in terms of method detection limit (MDL, per US EPA definition) and limit of detection (LOD), averaged 5.90 pg and 0.122 pg, respectively, with the mean coefficient of correlation (R(2)) of 0.9975. The minimum quantifiable mass of target analytes, when determined using real air samples by the TD-GC/TOF MS, is highly comparable to the detection limits determined experimentally by standard. In fact, volumes for the actual detection of the major aromatic VOCs like benzene, toluene, and xylene (BTX) in ambient air samples were as low as 1.0 mL in the 0.11-2.25 ppb range. It was thus possible to demonstrate that most target compounds including those in low abundance could be reliably quantified at concentrations down to 0.1 ppb at sample volumes of less than 10 mL. The unique sensitivity of this advanced analytical system can ultimately lead to a shift in field sampling strategy with smaller air sample volumes facilitating faster, simpler air sampling (e.g., use of gas syringes rather than the relative complexity of pumps or bags/canisters), with greatly reduced risk of analyte breakthrough and minimal interference, e.g., from atmospheric humidity. The improved detection limits offered by this system can also enhance accuracy and measurement precision. PMID:22934885

  15. A sample holder for measuring the magnetic properties of air-sensitive compounds

    Science.gov (United States)

    Berlie, Adam; Terry, Ian; Szablewski, Marek

    2011-01-01

    A sample holder is reported which has allowed the magnetic characterization of air-sensitive compounds to be made in a Quantum Design Magnetic Properties Measurement System as a function of the applied field (0-5 T), and at temperatures ranging from 2 to 290 K. The sample holder is in the form of a specially designed tube, which is made from high purity quartz, utilizes PTFE (polytetrafluoroethylene) plugs and is reusable. This construction also offers the benefit that no heat treatment of the holder is required during sample loading, making the sample holder suitable for thermally sensitive compounds. The application of this sample holder is demonstrated for the case of Ni(cod)2 (cod = 1,5-cyclooctadiene), a compound that decomposes when exposed to air and/or heat. This material's instability has, so far, prevented the magnetic characterization of the compound, with nickel nanoparticles, a product of the decomposition, usually being measured instead.

  16. Simultaneous separation of ergot alkaloids by capillary electrophoresis after cloud point extraction from cereal samples.

    Science.gov (United States)

    Felici, Emiliano; Wang, Chien C; Fernández, Liliana P; Gomez, María R

    2015-01-01

    A new and sensitive analytical methodology for ergot alkaloids (EA) determination from cereal samples based on cloud point extraction (CPE) prior to CE-UV absorbance was developed. The methodology involves extraction under acid conditions and subsequent preconcentration by applying a simple, rapid and environmentally friendly low volume surfactant extraction procedure. After extraction, CE analysis was carried out by performing dilutions on preconcentrated surfactant rich phase, achieving a single peak or simultaneous alkaloids determination. A real preconcentration factor of 22 of total EA was obtained, demonstrating the efficiency of this methodology. The limits of detection were 2.6 and 2.2 μg/kg for ergotamine and ergonovine, respectively. Validation procedure revealed suitable linearity, accuracy and precision. The average extraction and clean-up recoveries were compared with the theoretical values and were better than 92%. This method was successfully applied to the determination of EA in different varieties of commercial flour samples, two grain samples and one of the leading brands cereal-based product for infant feeding. The high sensitivity achieved for EA determinations in real samples suggests CPE procedure as an interesting approach to improve CE-UV visible detection limits. Moreover, the whole process could be considered as a contribution to green chemistry because nonorganic solvents were involved, demonstrating its great potential over conventional techniques. PMID:25257749

  17. Analysis of tree bark samples for air pollution biomonitoring of an urban area

    Energy Technology Data Exchange (ETDEWEB)

    Martins, Ana Paula G.; Negri, Elnara M.; Saldiva, Paulo H.N., E-mail: paulista@usp.b [Universidade de Sao Paulo (USP), SP (Brazil). Faculdade de Medicina. Dept. de Patologia; Saiki, Mitiko; Scapin, Marcos A.; Ribeiro, Andreza P.; Salvador, Vera L., E-mail: mitiko@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2009-07-01

    Air pollution is receiving much attention as a public health problem around the world due to its adverse health effects from exposures by urban populations. Within this context, the use of vegetal biomonitoring to evaluate air quality has been investigated throughout the world. Air pollutant levels are high in the city of Sao Paulo, SP, Brazil and being the vehicle emissions its main source. The aim of this study was to evaluate concentrations of As, Ba, Br, Ca, Co, Cr, Cu, Fe, Mn, Pb, S, Sb and Zn in tree bark samples used as biomonitor of urban air pollution. Concentrations of these elements were determined in barks collected in trees of the Ibirapuera Park, one of the biggest and most visited parks of the city of Sao Paulo city. Samples of tree barks were also collected in a site outside the city of Sao Paulo, in a rural area of Embu-Guacu, considered as a control site. The element concentrations were determined by the methods of Instrumental Neutron Activation Analysis (INAA) and of Energy Dispersive X-ray Fluorescence Spectrometry (EDXRF). The findings of this study showed that tree bark samples may be used as biomonitors of urban air pollution in a micro scale, and both techniques, INAA and EDXRF, can be used to evaluate element concentrations in tree bark samples. (author)

  18. Analysis of tree bark samples for air pollution biomonitoring of an urban area

    International Nuclear Information System (INIS)

    Air pollution is receiving much attention as a public health problem around the world due to its adverse health effects from exposures by urban populations. Within this context, the use of vegetal biomonitoring to evaluate air quality has been investigated throughout the world. Air pollutant levels are high in the city of Sao Paulo, SP, Brazil and being the vehicle emissions its main source. The aim of this study was to evaluate concentrations of As, Ba, Br, Ca, Co, Cr, Cu, Fe, Mn, Pb, S, Sb and Zn in tree bark samples used as biomonitor of urban air pollution. Concentrations of these elements were determined in barks collected in trees of the Ibirapuera Park, one of the biggest and most visited parks of the city of Sao Paulo city. Samples of tree barks were also collected in a site outside the city of Sao Paulo, in a rural area of Embu-Guacu, considered as a control site. The element concentrations were determined by the methods of Instrumental Neutron Activation Analysis (INAA) and of Energy Dispersive X-ray Fluorescence Spectrometry (EDXRF). The findings of this study showed that tree bark samples may be used as biomonitors of urban air pollution in a micro scale, and both techniques, INAA and EDXRF, can be used to evaluate element concentrations in tree bark samples. (author)

  19. Blue Chitin columns for the extraction of heterocyclic amines from urine samples

    DEFF Research Database (Denmark)

    Bang, J.; Frandsen, Henrik Lauritz; Skog, K.

    During normal cooking of meat, a class of mutagenic/carcinogenic compounds called heterocyclic amines is formed. Heterocyclic amines are rapidly absorbed and metabolised in the human body, and for estimation of the intake of heterocyclic amines, it is useful to determinate their levels in the urine....... Blue Chitin columns were used for the extraction and purification of heterocyclic amines from urine samples spiked with 14 different heterocyclic amines. The samples were analysed using LC-MS. The results show that Blue Chitin columns provide a straightforward and rapid means of extracting heterocyclic...

  20. Extraction X-ray fluorescence determination of gold in natural samples

    International Nuclear Information System (INIS)

    The behaviour of gold and other elements impeding its X-ray fluorescence (XRF) determination, namely, of zinc, lead, and arsenic, has been studied during their extraction by TBP from hydrochloric, nitric, and aqua regia solutions using solid extractant (SE(TBP)). Gold extraction from pulps after aqua regia leaching, with the gold distribution coefficient (D) being equal to about 104, was observed as the most favourable one for the quantitative and selective recovery of gold. For extraction from hydrochloric solutions the DAu value does not depend on the gold content of initial solutions (10-8 - 10-4 M), but it decreases substantially with increasing extraction temperature (from 5x105 at 20 deg C to 9x103 at 70 deg C). An anomalously high distribution coefficient of lead (DPb=103) was observed during extraction from hydrochloric solutions in the presence of chlorine. This fact could be explained by the formation of the chlorocomplexes of lead (IV). The XRF method of gold determination in natural samples has been developed, which includes the aqua regia decomposition of the samples, recovery of gold from the pulp after its leaching by SE(TBP) and back - extraction using a 0.025 M hot thiourea solution providing a thin sample film for secondary XRF spectrometry. For 25 g of the sample material the limit of determination is set at 0.01 g per ton (10-6%). The accuracy of the technique has been checked on different reference materials. The results agree within 10%. 16 refs.; 5 figs.; 1 tab

  1. Reliability of non-invasive tissue sampling methods for DNA extraction in rabbits (Oryctolagus cuniculus

    Directory of Open Access Journals (Sweden)

    Manel Ben Larbi

    2012-05-01

    Full Text Available Deoxyribonucleic acid (DNA can be extracted from different tissue sources. The most common is blood, but in some situations it can be easier to take a biopsy. In some cases when it is difficult to capture animals, especially in wild populations, faeces and hairs can be considered as a source of DNA. This paper presents a pilot study conducted to compare the applicability of invasive and non-invasive sampling methods for extracting DNA for use in genetic studies of rabbits (Oryctolagus cuniculus. The study included 24 rabbits from the INRA 1001 strain.  Blood, hair, ear biopsies and faeces were collected and used as DNA sources. Our aim was to verify the quantity of DNA obtained from different tissues using two or three types of extraction. DNA was obtained for all tissue types and all extraction methods. DNA extraction was shown to be optimal with the LGC (Laboratory of Cellular Genetics blood extraction method. With regard to non-invasive methods, DNA extraction for hair using the LGC protocol and QIAamp® DNA mini kit gave very low quantities of DNA that could not be used for PCR reactions. The Chelex extraction protocol gave good results for PCR but could not be quantified. DNA extracted from faeces is a viable source of DNA for determining individual genotypes. The use of such non-invasive samples as a source of genetic material is a recent and very promising technique, especially for the study of endangered species, but these techniques are still too unreliable and costly to altogether replace invasive techniques when the latter are possible.

  2. Liquid Phase Micro-Extraction of Linear Alkylbenzene Sulfonate Anionic Surfactants in Aqueous Samples

    Directory of Open Access Journals (Sweden)

    Jan Åke Jönsson

    2011-10-01

    Full Text Available Hollow fiber liquid phase micro-extraction (LPME of linear alkylbenzene sulfonates (LAS from aqueous samples was studied. Ion pair extraction of C10, C11, C12 and C13 homologues was facilitated with trihexylamine as ion-pairing agent, using di-n-hexylether as solvent for the supported liquid membrane (SLM. Effects of extraction time, acceptor buffer concentration, stirring speed, sample volume, NaCl and humic acids were studied. At 10–50 µg L−1 linear R2-coefficients were 0.99 for C10 and C11 and 0.96 for C12. RSD was typically ~15%. Three observations were especially made. Firstly, LPME for these analytes was unusually slow with maximum enrichment observed after 15–24 h (depending on sample volume. Secondly, the enrichment depended on LAS sample concentration with 35–150 times enrichment below ~150 µg L−1 and 1850–4400 times enrichment at 1 mg L−1. Thirdly, lower homologues were enriched more than higher homologues at low sample concentrations, with reversed conditions at higher concentrations. These observations may be due to the fact that LAS and the amine counter ion themselves influence the mass transfer at the water-SLM interface. The observations on LPME of LAS may aid in LPME application to other compounds with surfactant properties or in surfactant enhanced membrane extraction of other compounds.

  3. Data Quality Objectives for Regulatory Requirements for Hazardous and Radioactive Air Emissions Sampling and Analysis

    International Nuclear Information System (INIS)

    This document describes the results of the data quality objective (DQO) process undertaken to define data needs for state and federal requirements associated with toxic, hazardous, and/or radiological air emissions under the jurisdiction of the River Protection Project (RPP). Hereafter, this document is referred to as the Air DQO. The primary drivers for characterization under this DQO are the regulatory requirements pursuant to Washington State regulations, that may require sampling and analysis. The federal regulations concerning air emissions are incorporated into the Washington State regulations. Data needs exist for nonradioactive and radioactive waste constituents and characteristics as identified through the DQO process described in this document. The purpose is to identify current data needs for complying with regulatory drivers for the measurement of air emissions from RPP facilities in support of air permitting. These drivers include best management practices; similar analyses may have more than one regulatory driver. This document should not be used for determining overall compliance with regulations because the regulations are in constant change, and this document may not reflect the latest regulatory requirements. Regulatory requirements are also expected to change as various permits are issued. Data needs require samples for both radionuclides and nonradionuclide analytes of air emissions from tanks and stored waste containers. The collection of data is to support environmental permitting and compliance, not for health and safety issues

  4. Nonparametric feature extraction for classification of hyperspectral images with limited training samples

    Science.gov (United States)

    Kianisarkaleh, Azadeh; Ghassemian, Hassan

    2016-09-01

    Feature extraction plays a crucial role in improvement of hyperspectral images classification. Nonparametric feature extraction methods show better performance compared to parametric ones when distribution of classes is non normal-like. Moreover, they can extract more features than parametric methods do. In this paper, a new nonparametric linear feature extraction method is introduced for classification of hyperspectral images. The proposed method has no free parameter and its novelty can be discussed in two parts. First, neighbor samples are specified by using Parzen window idea for determining local mean. Second, two new weighting functions are used. Samples close to class boundaries will have more weight in the between-class scatter matrix formation and samples close to class mean will have more weight in the within-class scatter matrix formation. The experimental results on three real hyperspectral data sets, Indian Pines, Salinas and Pavia University, demonstrate that the proposed method has better performance in comparison with some other nonparametric and parametric feature extraction methods.

  5. Passive air sampling of PCBs, PBDEs, and organochlorine pesticides across Europe.

    Science.gov (United States)

    Jaward, Foday M; Farrar, Nick J; Harner, Tom; Sweetman, Andrew J; Jones, Kevin C

    2004-01-01

    This study presents concurrently sampled ambient air data for a range of persistent organic pollutants at the continental scale. This was achieved using a passive air sampling system, deploying polyurethane foam disks, which was prepared in one laboratory, sealed to prevent contamination, sent out by courier to volunteers participating in different countries, exposed for 6 weeks, collected, resealed, and returned to the laboratory for analysis. Europe was the study area--a region with a history of extensive POPs usage and emission and with marked national differences in population density, the degree of urbanization and industrial/agricultural development. Samplers were deployed at remote/rural/urban locations in 22 countries and analyzed for PCBs, a range of organochlorine pesticides (HCB, alpha-HCH, gamma-HCH, ppDDT, ppDDE), and PBDEs. Calculated air concentrations were in line with those obtained by conventional active air sampling techniques. The geographical pattern of all compounds reflected suspected regional emission patterns and highlighted localized hotspots. PCB and PBDE levels varied by over 2 orders of magnitude; the highest values were detected in areas of high usage and were linked to urbanized areas. HCB was relatively uniformly distributed, reflecting its persistence and high degree of mixing in air. Higher gamma-HCH, ppDDT, and ppDDE levels generally occurred in South and East Europe. PMID:14740714

  6. Comparison of air samples, nasal swabs, ear-skin swabs and environmental dust samples for detection of Methicillin Resistant Staphylococcus aureus (MRSA) in pig herds

    DEFF Research Database (Denmark)

    Agersø, Yvonne; Vigre, Håkan; Cavaco, Lina;

    2014-01-01

    To identify a cost-effective and practical method for detection of methicillin-resistant Staphylococcus aureus (MRSA) in pig herds, the relative sensitivity of four sample types: nasal swabs, ear-skin (skin behind the ears) swabs, environmental dust swabs and air was compared. Moreover, dependency...... conclusion, MRSA detection by air sampling is easy to perform, reduces costs and analytical time compared to existing methods, and is recommended for initial testing of herds. Ear-skin swab sampling may be more sensitive for MRSA detection than air sampling or nasal swab sampling....

  7. Pressure drop measurement of column weight in disc and doughnut pulsed extraction column by external air purge method

    International Nuclear Information System (INIS)

    The pressure drop of column weight was measured in a disc and doughnut pulsed extraction column with the inertial diameter of 0.3 m and height of 5.6 m by internal and external air purge methods, respectively. The experimental results show that the pressure drops of column weight measured by external air purge method are in good agreement with those by internal air purge method, therefore, the external air purge method is recommended to measure the pressure drop of column weight in the pulsed extraction column in plutonium purification cycle. (authors)

  8. Development of Air Sampling and Analytical Methods for Acetoin, Diacetyl, and 2,3-Pentanedione

    OpenAIRE

    Takaku-Pugh, Sayaka

    2012-01-01

    Acetoin, diacetyl, and 2,3-pentanedione are artificial butter flavoring ingredients. Occupational exposures to diacetyl are associated with severe respiratory disease including bronchiolitis obliterans. Dynamic and passive air sampling and analytical methods were developed for simultaneous sampling of these ketones using 10 % (w/w) O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) on Tenax TA (80/100 mesh). PFBHA O-oximes of the ketones were synthesized with above 95 % pur...

  9. Air sampling in the workplace to meet the new part 20 requirements

    International Nuclear Information System (INIS)

    The US Nuclear Regulatory Commission is developing a Regulatory Guide on air sampling in the workplace to meet the requirements of the revised Part 20. The guide will be accompanied by a technical manual describing and giving examples of how to meet the recommendations in the guide. Draft versions of the guide and manual are scheduled to be published for public comment this year. A final guide and manual, revised to consider the public comments, are scheduled to be published in 1992. This talk will summarize some of the more important features of the guide and manual. In particular, the talk will discuss how to demonstrate that samples taken to estimate worker intakes are representative of the air inhaled by workers and what measurements are necessary if a licensee wants to adjust derived air concentrations to account for particle size

  10. Supercritical-fluid extraction of soil samples and determination of polycyclic aromatic hydrocarbons (PAHs) by HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Wenclawiak, B.; Rathmann, C.; Teuber, A. (Siegen Univ. (Gesamthochschule) (Germany). Analytische Chemie 1)

    1992-12-01

    Soil samples were dried and extracted with supercritical CO[sub 2]. A clean-up procedure was necessary before the PAH's were determinated by HPLC. Losses of PAHs during clean-up were studied with the internal standard 2,2'-binaphthyl. (orig.).

  11. Technical assessment of compliance with workplace air sampling requirements in the 300 Area

    International Nuclear Information System (INIS)

    The purpose of this Technical Work Document is to satisfy HSRCM-1, the ''Hanford Site Radiological Control Manual.'' Article 551.4 of that manual states a requirement for a documented study of facility workplace air sampling programs (WPAS). This first revision of the original Supporting Document covers the period from January 1, 1995 to December 31, 1995. HSRCM-1 is the primary guidance for radiological control at Westinghouse Hanford Company (WHC). It was written to implement DOE/EH-0256T ''US Department of Energy Radiological Control Manual'' as it applies to programs at Hanford. As such, it complies with Title 10, Part 835 of the Code of Federal Regulations. There are also several Department of Energy (DOE) Orders, national consensus standards, and reports that provide criteria, standards, and requirements for workplace air sampling programs. This document provides a summary of these, as they apply to WHC facility workplace air sampling programs. This document also provides an evaluation of the compliance of 300 Areas' workplace air sampling program to the criteria, standards, and requirements and documents compliance with the requirements where appropriate. Where necessary, it also indicates changes needed to bring specific locations into compliance. The areas evaluated were the 340 Facility, the Advanced Reactor Operations Division Facilities, the N Reactor Fuels Supply Facility, and The Geotechnical Engineering Laboratory

  12. Air and smear sample calculational tool for Fluor Hanford Radiological control

    International Nuclear Information System (INIS)

    A spreadsheet calculation tool was developed to automate the calculations performed for determining the concentration of airborne radioactivity and smear counting as outlined in HNF--13536, Section 5.2.7, ''Analyzing Air and Smear Samples''. This document reports on the design and testing of the calculation tool. Radiological Control Technicians (RCTs) will save time and reduce hand written and calculation errors by using an electronic form for documenting and calculating work place air samples. Current expectations are RCTs will perform an air sample and collect the filter or perform a smear for surface contamination. RCTs will then survey the filter for gross alpha and beta/gamma radioactivity and with the gross counts utilize either hand calculation method or a calculator to determine activity on the filter. The electronic form will allow the RCT with a few key strokes to document the individual's name, payroll, gross counts, instrument identifiers; produce an error free record. This productivity gain is realized by the enhanced ability to perform mathematical calculations electronically (reducing errors) and at the same time, documenting the air sample

  13. Technical assessment of workplace air sampling requirements at tank farm facilities. Revision 2

    International Nuclear Information System (INIS)

    Tank Farm facilities compliance with the workplace air sampling (WPAS) program has been assessed. Requirements bases for determining compliance and recommendations are included. In the current condition all buildings are in compliance with the WPAS program. This document also supersedes WHC-SD-SQA-TA-20012, revision 0

  14. the nature of air flow near the inlets of blunt dust sampling probes

    Science.gov (United States)

    Vincent, J. H.; Hutson, D.; Mark, D.

    This paper sets out to describe the nature of air flow near blunt dust samplers in a way which allows a relatively simple assessment of their performances for collecting dust particles. Of particular importance is the shape of the limiting stream surface which divides the sampled air from that which passes outside the sampler, and how this is affected by the free-stream air velocity, the sampling flow rate, and the shape of the sampler body. This was investigated for two-dimensional and axially-symmetric sampler systems by means of complementary experiments using electrolytic tank potential flow analogues and a wind tunnel respectively. For extreme conditions the flow of air entering the sampling orifice may be wholly divergent or wholly convergent. For a wide range of intermediate conditions, however, the flow first diverges then converges, exhibiting a so-called "spring onion effect". Whichever of these applies for a particular situation, the flow may be considered to consist of two parts, the outer one dominated by the flow about the sampler body and the inner one dominated by the flow into the sampling orifice. Particle transport in this two-part flow may be assessed using ideas borrowed from thin-walled probe theory.

  15. Measurement of the carbon 14 activity at natural level in air samples

    International Nuclear Information System (INIS)

    The aim of the study was to measure the carbon 14 activity at natural level in air samples using classical methods of radiochemistry and beta counting. Three different methods have been tested in order to minimise the detection limit. In the three methods, the first step consists in trapping the atmospheric carbon 14 into NaOH (1N) using a bubbling chamber. The atmospheric carbon dioxide reacts with NaOH to form Na2CO3. In the first method the Na2CO3 solution is mixed with a liquid scintillate and is directly analysed by liquid scintillation counting (LSC). The detection limit is approximately 1 Bq/m3 of air samples. The second method consists in evaporating the carbonate solution and then counting the solid residue with a proportional gas circulation counter. The detection limit obtained is lower than the first method (0.4 Bq/m3 of air samples). In the third method, Na2CO3 is precipitated into CaCO3 in presence of CaCl2. CaCO3 is then analysed by LSC. This method appear to be the most appropriate, the detection limit is 0.05 Bq/m3 of air samples. (author)

  16. EXTRACT

    DEFF Research Database (Denmark)

    Pafilis, Evangelos; Buttigieg, Pier Luigi; Ferrell, Barbra;

    2016-01-01

    The microbial and molecular ecology research communities have made substantial progress on developing standards for annotating samples with environment metadata. However, sample manual annotation is a highly labor intensive process and requires familiarity with the terminologies used. We have the...... and text-mining-assisted curation revealed that EXTRACT speeds up annotation by 15-25% and helps curators to detect terms that would otherwise have been missed.Database URL: https://extract.hcmr.gr/......., organism, tissue and disease terms. The evaluators in the BioCreative V Interactive Annotation Task found the system to be intuitive, useful, well documented and sufficiently accurate to be helpful in spotting relevant text passages and extracting organism and environment terms. Comparison of fully manual...

  17. The use of a solvent extraction technique for the analysis of trace metal pollutants in estuarine water samples

    International Nuclear Information System (INIS)

    A solvent extraction technique, based on metal carbamate complex formation is investigated for its usefulness in the analysis of estuarine water samples. Preliminary results indicate an extraction efficiency over 90% and a good precision. (author)

  18. A study on the separation and extraction of polycyclic aromatic hydrocarbons in water sample by gas chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    The separation and sample extraction methods of 19 polycyclic aromatic hydrocarbons (PAHS) in water samples were investigated by gas chromatography/mass spectrometry (GC/MS) and some ex-traction methods involved liquid-liquid extraction, disk extraction and solid-phase extraction methods. The separation of 19 PAHs was possible by partial variation of oven temperature of GC/MS in temperature range 80∼310.deg.C. Extraction procedures of PAHs in water samples were somewhat modified and com-pared as extraction recoveries and the simplicity of methods. Extraction recoveries of PAHs were 71.3∼109.5% by liquid-liquid extraction method. By using disk extraction, good extraction recoveries (80.7∼94.9%) were obtained in case of C18 disk extraction method by filtration. And extraction recoveries of PAHs by C18 solid-phase were in the range of 51.8∼77.9%. Method detection limits (S/N=5) of 19 PAHs were in the range of 0.25∼6.25 ppb by liquid-liquid extraction and solid-phase extraction and 0.05∼1.25 ppb by disk extraction methods

  19. Assessing genetic polymorphisms using DNA extracted from cells present in saliva samples

    Directory of Open Access Journals (Sweden)

    Nemoda Zsofia

    2011-12-01

    Full Text Available Abstract Background Technical advances following the Human Genome Project revealed that high-quality and -quantity DNA may be obtained from whole saliva samples. However, usability of previously collected samples and the effects of environmental conditions on the samples during collection have not been assessed in detail. In five studies we document the effects of sample volume, handling and storage conditions, type of collection device, and oral sampling location, on quantity, quality, and genetic assessment of DNA extracted from cells present in saliva. Methods Saliva samples were collected from ten adults in each study. Saliva volumes from .10-1.0 ml, different saliva collection devices, sampling locations in the mouth, room temperature storage, and multiple freeze-thaw cycles were tested. One representative single nucleotide polymorphism (SNP in the catechol-0-methyltransferase gene (COMT rs4680 and one representative variable number of tandem repeats (VNTR in the serotonin transporter gene (5-HTTLPR: serotonin transporter linked polymorphic region were selected for genetic analyses. Results The smallest tested whole saliva volume of .10 ml yielded, on average, 1.43 ± .77 μg DNA and gave accurate genotype calls in both genetic analyses. The usage of collection devices reduced the amount of DNA extracted from the saliva filtrates compared to the whole saliva sample, as 54-92% of the DNA was retained on the device. An "adhered cell" extraction enabled recovery of this DNA and provided good quality and quantity DNA. The DNA from both the saliva filtrates and the adhered cell recovery provided accurate genotype calls. The effects of storage at room temperature (up to 5 days, repeated freeze-thaw cycles (up to 6 cycles, and oral sampling location on DNA extraction and on genetic analysis from saliva were negligible. Conclusions Whole saliva samples with volumes of at least .10 ml were sufficient to extract good quality and quantity DNA. Using

  20. Measurement of overall uptake coefficients for HO2 radicals by aerosol particles sampled from ambient air at Mts. Tai and Mang (China)

    OpenAIRE

    Taketani, F.; Y. Kanaya; P. Pochanart; Liu, Y; Li, J.; K. Okuzawa; K. Kawamura; Z. Wang; H. Akimoto

    2012-01-01

    HO2 uptake coefficients for ambient aerosol particles, collected on quartz fiber filter using a high-volume air sampler in China, were measured using an aerosol flow tube coupled with a chemical conversion/laser-induced fluorescence technique at 760 Torr and 298 K, with a relative humidity of 75%. Aerosol particles were regenerated with an atomizer using the water extracts from the aerosol particles. Over 10 samples, the measured HO2 uptake coefficients for the aerosol parti...

  1. Measurement of overall uptake coefficients for HO2 radicals by aerosol particles sampled from ambient air at Mts. Tai and Mang, China

    OpenAIRE

    H. Akimoto; Z. Wang; K. Okuzawa; K. Kawamura; Li, J.; Liu, Y; P. Pochanart; Taketani, F.; Y. Kanaya

    2012-01-01

    HO2 uptake coefficients for ambient aerosol particles, collected on quartz filter using a high-volume air sampler in China, were measured using an aerosol flow tube coupled with a chemical conversion/laser-induced fluorescence technique at 760 Torr and 298 K, with a relative humidity of 75%. Aerosol particles were regenerated with an atomizer using the water extracts from the aerosol particles. Over 10 samples, the measured HO2 uptake coefficients for the aerosol particles at the Mt. ...

  2. Determination of 15 isomers of chlorobenzoic acid in soil samples using accelerated sample extraction followed by liquid chromatography.

    Science.gov (United States)

    Křesinová, Zdena; Muzikář, Milan; Olšovská, Jana; Cajthaml, Tomáš

    2011-05-30

    A study was conducted to elaborate a fast, simple and efficient method for determination of 15 isomers chlorobenzoic acids (CBAs) in soil using HPLC-UV. Artificially contaminated soil samples were extracted using accelerated solvent extraction (ASE) with 1% acetic acid in a mixture of hexane and acetone (1:1, V/V) under a pressure of 10.34 MPa and temperature of 150°C. The recovery of the ASE method was above 82%. The extracts were concentrated; dimethyl sulfoxide was used to prevent CBA volatilization and the final analysis was performed with a C18 XBridge HPLC column employing a mobile phase consisting of acetonitrile and 0.1% trifluoracetic acid in water. A HPLC procedure with gradient elution and UV detection was developed and validated. The method exhibited a linear range for 2-CBA; 2,6-CBA; 3-CBA; 4-CBA; 2,3-CBA; 2,3,6-CBA; 2,5-CBA; and 2,4-CBA from 5 to 120 μg/mL with a limit of quantification (LOQ) of 5 μg/mL, RSD from 2.42 to 9.42% and accuracy from 82 ± 2 to 103 ± 3%. The linear range of determination of 2,4,6-CBA, 3,4-CBA, 2,3,5,6-CBA, 3,5-CBA, 2,3,5-CBA, 2,3,4,5,6-CBA and 2,3,4,5-CBA was 10-120 μg/mL with LOQ 10 μg/mL, RSD from 0.74 to 5.84% and accuracy from 94 ± 1 to 114 ± 1%. The optimized analytical procedure was finally applied on two historically PCB contaminated soils and 9 CBAs were quantified in the samples. PMID:21530790

  3. Optimization of arsenic extraction in rice samples by Plackett-Burman design and response surface methodology.

    Science.gov (United States)

    Ma, Li; Wang, Lin; Tang, Jie; Yang, Zhaoguang

    2016-08-01

    Statistical experimental designs were employed to optimize the extraction condition of arsenic species (As(III), As(V), monomethylarsonic acid (MMA) and dimethylarsonic acid (DMA)) in paddy rice by a simple solvent extraction using water as an extraction reagent. The effect of variables were estimated by a two-level Plackett-Burman factorial design. A five-level central composite design was subsequently employed to optimize the significant factors. The desirability parameters of the significant factors were confirmed to 60min of shaking time and 85°C of extraction temperature by compromising the experimental period and extraction efficiency. The analytical performances, such as linearity, method detection limits, relative standard deviation and recovery were examined, and these data exhibited broad linear range, high sensitivity and good precision. The proposed method was applied for real rice samples. The species of As(III), As(V) and DMA were detected in all the rice samples mostly in the order As(III)>As(V)>DMA. PMID:26988503

  4. A comparative evaluation of four DNA extraction protocols from whole blood sample.

    Science.gov (United States)

    Ghaheri, M; Kahrizi, D; Yari, K; Babaie, A; Suthar, R S; Kazemi, E

    2016-01-01

    All organisms have Deoxyribonucleic acid (DNA) within their cells. DNA is a complex molecule that contains all of the information necessary to build and maintain an organism. DNA extraction is one of the most basic and essential techniques in the study of DNA that allow huge advances in molecular biology, biotechnology and bioinformatics laboratories. Whole blood samples are one of the main sources used to obtain DNA and there are many different protocols available in this issue. In current research, compared four DNA extraction protocols from blood samples; include modified phenol-chloroform protocol, two salting-out and enzyme free method and from commercial kit. The extracted DNAs by these protocols were analyzed according to their time demands, quality and quantity, toxicity and functionality in PCR method. Also the quality and quantity of the extracted DNA were surveyed by gel electrophoresis and Nanodrop spectrophotometry methods. It was observed that there are not significantly differences between these methods about DNA Purity (A260/A280), but the DNA yield (ng DNA/μl) of phenol/chloroform method was higher than other methods. In addition, phenol/chloroform was the most toxic method and it takes more time than other methods. Roche diagnostics GmbH kit was the most expensive among the four methods but the least extraction time was required and it was the safest method. PMID:27064884

  5. Results of Self-Absorption Study on the Versapor 3000 Filters for Radioactive Particulate Air Sampling

    International Nuclear Information System (INIS)

    Since the mid-1980s the Pacific Northwest National Laboratory (PNNL) has used a value of 0.85 as a correction factor for the self absorption of activity of particulate radioactive air samples. More recently, an effort was made to evaluate the current particulate radioactive air sample filters (Versapor(regsign) 3000) used at PNNL for self absorption effects. There were two methods used in the study, (1) to compare the radioactivity concentration by direct gas-flow proportional counting of the filter to the results obtained after acid digestion of the filter and counting again by gas-flow proportional detection and (2) to evaluate sample filters by high resolution visual/infrared microscopy to determine the depth of material loading on or in the filter fiber material. Sixty samples were selected from the archive for acid digestion in the first method and about 30 samples were selected for high resolution visual/infrared microscopy. Mass loading effects were also considered. From the sample filter analysis, large error is associated with the average self absorption factor, however, when the data is compared directly one-to-one, statistically, there appears to be good correlation between the two analytical methods. The mass loading of filters evaluated was <0.2 mg cm-2 and was also compared against other published results. The microscopy analysis shows the sample material remains on the top of the filter paper and does not imbed into the filter media. Results of the microscopy evaluation lead to the conclusion that there is not a mechanism for significant self absorption. The overall conclusion is that self-absorption is not a significant factor in the analysis of filters used at PNNL for radioactive air stack sampling of radionuclide particulates and that an applied correction factor is conservative in determining overall sample activity. A new self absorption factor of 1.0 is recommended

  6. Evaluation of metal ions in rice samples: extraction and direct determination by ICP OES

    International Nuclear Information System (INIS)

    A method for extraction of metal ions present in rice samples using ammoniacal EDTA solution, pH = 10, as extractor agent is proposed under the following optimized conditions: 0.20 g of rice sample and 5.00 mL of ammoniacal EDTA (ethylenediaminetetraacetic acid) solution, with 5 min of ultrasound exposure time. Using robust ICP OES (inductively coupled plasma atomic emission spectrometry) conditions, direct analysis of the extraction solution was allowed, and the recovery values obtained were above 90% for most of the studied elements (P, K, Mg, Ca, Zn, Mn, Cu and Mo) with RSD -1 (Mn) - 48.68 mg kg-1 (K), showing adequate detectability for the determination of the analytes. The analysis of different samples indicated that Brazilian 'integral' rice contains higher contents of the constituents studied, followed by 'parboiled' rice, and the 'agulhinha' rice a long and thin grain type. (author)

  7. Online recovery of radiocesium from soil, tissue paper and plant samples by supercritical fluid extraction

    International Nuclear Information System (INIS)

    The feasibility of recovery of radio-cesium from soil, tissue papers, and plant samples has been evaluated by supercritical fluid extraction (SFE) route employing calix(4)arene-mono(crown-6) (CC) dissolved in acetonitrile. These studies showed that quantitative recovery of 137Cs from soil samples was difficult under the conditions of these studies. However, experiments performed on tissue papers (cellulose matrix) showed quantitative recovery of 137Cs. On the other hand, 137Cs recovery from plant samples varied between ∼50 % (for stems) and ∼67.2 % (for leaves) employing 1x10-3 M CC + 4 M HNO3 dissolved in acetonitrile. (author)

  8. Effect of onion extract on corneal haze suppression after air assisted lamellar keratectomy.

    Science.gov (United States)

    Kim, Soohyun; Park, Young Woo; Lee, Euiri; Park, Sang Wan; Park, Sungwon; Noh, Hyunwoo; Kim, Jong Whi; Seong, Je Kyung; Seo, Kangmoon

    2016-04-01

    This study evaluated the effect of onion extract on corneal haze suppression after applying the air assisted lamellar keratectomy. The air assisted lamellar keratectomy was performed on 24 canine eyes. They were treated with an artificial tear (group C), prednisolone acetate (group P), onion extract (group O) and TGF-β1 (group T) three times per day from 7 to 28 days after the surgery. Corneal haze occurred on the all eyes and was observed beginning 7 days after the surgery. The haze was significantly decreased in groups P and O from day 14 compared with the group C using the clinical (group P; P=0.021, group O; P=0.037) and objective evaluation method (group P; P=0.021, group O; P=0.039). In contrast, it was significantly increased in group T from day 14 compared with group C based on the clinical (P=0.002) and objective evaluation method (Peuthanasia, and immunohistochemistry with α-SMA antibodies was done. The total green intensity for α-SMA was significantly more expressed in group T and significantly less expressed in groups P and O than in group C. Onion extract could have potential as a therapeutic in preventing corneal haze development by suppressing the differentiation of fibroblasts into myofibroblasts. PMID:26607134

  9. Determination of selected heavy metals in air samples from the northern part of Jordan.

    Science.gov (United States)

    Gharaibeh, Ahmad A; El-Rjoob, Abdul-Wahab O; Harb, Mohammed K

    2010-01-01

    In this work, the atmospheric concentrations of selected heavy metals including lead (Pb), iron (Fe), cadmium (Cd), copper (Cu), nickel (Ni), manganese (Mn), and zinc (Zn) were measured for two different sampling sites (urban and rural) in the northern part of Jordan (Irbid city). Samples were collected according to a certain schedule for 1 year. High volume air samplers and glass fiber filters were used to collect the samples. Collected samples were digested using a mixture of analytical grade nitric acid and analytical grade hydrochloric acid, and analyzed to evaluate the levels of heavy metals by atomic absorption spectrophotometry. Six heavy metals (Pb, Fe, Cu, Ni, Mn, and Zn) were measured in all samples; the concentrations of Cd and Co were not detected in Irbid atmosphere by atomic absorption spectroscopy. The results were used to determine the levels of heavy metal pollutants in air, possible sources, and to compare the levels of selected heavy metals in the two studied sites. Aerosols from the rural site have lower concentrations for all the metals compared to those from the urban site. The daily and monthly variations of the elements were investigated. All heavy metals in urban and rural sites reached maximum concentrations in June, July, and August. This is consistent with the increased activities leading to particulate matter emission during the summer period. The enrichment factors with respect to earth crust and correlation coefficients of heavy metals were investigated to predict the possible sources of heavy metals in air. PMID:19083108

  10. Data Quality Objectives for Regulatory Requirements for Hazardous and Radioactive Air Emissions Sampling and Analysis

    Energy Technology Data Exchange (ETDEWEB)

    MULKEY, C.H.

    1999-07-06

    This document describes the results of the data quality objective (DQO) process undertaken to define data needs for state and federal requirements associated with toxic, hazardous, and/or radiological air emissions under the jurisdiction of the River Protection Project (RPP). Hereafter, this document is referred to as the Air DQO. The primary drivers for characterization under this DQO are the regulatory requirements pursuant to Washington State regulations, that may require sampling and analysis. The federal regulations concerning air emissions are incorporated into the Washington State regulations. Data needs exist for nonradioactive and radioactive waste constituents and characteristics as identified through the DQO process described in this document. The purpose is to identify current data needs for complying with regulatory drivers for the measurement of air emissions from RPP facilities in support of air permitting. These drivers include best management practices; similar analyses may have more than one regulatory driver. This document should not be used for determining overall compliance with regulations because the regulations are in constant change, and this document may not reflect the latest regulatory requirements. Regulatory requirements are also expected to change as various permits are issued. Data needs require samples for both radionuclides and nonradionuclide analytes of air emissions from tanks and stored waste containers. The collection of data is to support environmental permitting and compliance, not for health and safety issues. This document does not address health or safety regulations or requirements (those of the Occupational Safety and Health Administration or the National Institute of Occupational Safety and Health) or continuous emission monitoring systems. This DQO is applicable to all equipment, facilities, and operations under the jurisdiction of RPP that emit or have the potential to emit regulated air pollutants.

  11. Data Quality Objectives for Regulatory Requirements for Hazardous and Radioactive Air Emissions Sampling and Analysis

    International Nuclear Information System (INIS)

    This document describes the results of the data quality objective (DQO) process undertaken to define data needs for state and federal requirements associated with toxic, hazardous, and/or radiological air emissions under the jurisdiction of the River Protection Project (RPP). Hereafter, this document is referred to as the Air DQO. The primary drivers for characterization under this DQO are the regulatory requirements pursuant to Washington State regulations, that may require sampling and analysis. The federal regulations concerning air emissions are incorporated into the Washington State regulations. Data needs exist for nonradioactive and radioactive waste constituents and characteristics as identified through the DQO process described in this document. The purpose is to identify current data needs for complying with regulatory drivers for the measurement of air emissions from RPP facilities in support of air permitting. These drivers include best management practices; similar analyses may have more than one regulatory driver. This document should not be used for determining overall compliance with regulations because the regulations are in constant change, and this document may not reflect the latest regulatory requirements. Regulatory requirements are also expected to change as various permits are issued. Data needs require samples for both radionuclides and nonradionuclide analytes of air emissions from tanks and stored waste containers. The collection of data is to support environmental permitting and compliance, not for health and safety issues. This document does not address health or safety regulations or requirements (those of the Occupational Safety and Health Administration or the National Institute of Occupational Safety and Health) or continuous emission monitoring systems. This DQO is applicable to all equipment, facilities, and operations under the jurisdiction of RPP that emit or have the potential to emit regulated air pollutants

  12. Report on sampling and analysis of exhaust air at the 221-T and 2706-T buildings

    Energy Technology Data Exchange (ETDEWEB)

    Stauffer, M.

    1997-09-22

    This report presents analytical results from exhaust air samples collected at stacks 221-T and 2706-T of the T-Plant. The samples were collected with SUMMA canisters over a 24 hour interval and were analyzed by gas chromatography-mass spectrometry using a modified EPA TO-14 procedure. The data suggest that the buildings had generally low concentrations of volatile organic compounds (< 40 ppbv). However, samples from building 2706-T did have significant amounts of non-target higher-boiling hydrocarbons, probably from a petroleum destination fraction.

  13. Determination of plutonium americium and curium in soil samples by solvent extraction with trioctylphosphine oxide

    International Nuclear Information System (INIS)

    A method of Pu, Am and Cm determination in soil samples, which was developed for analyzing samples from territories subjected to radioactive contamination as a result of the Chernobyl accident is described. After preliminary treatment the samples were leached by solution of 7 mol/l HNO23+0.3 mol/l KBrO3 during heating. Pu was isolated by extraction with 0.05 mol TOPO from 7 mol/l HNO3. 144Ce and partially remaining in water phase isotopes of Zr, U and Th were isolated in an extraction-chromatographic column with TOPO and PbO2. Then Am and Cm were extracted by 0.2 mol/l TOPO from solution 1 mol/l HLact+0.07 mol/l DTPA+1 mol/l Al(NO3)3. Alpha-activity of both extracted products was determined in liquid scintillation counter. Chemical yield of plutonium counted to 85±10%, that of americium and curium -75±10%. 17 refs

  14. A new CF-IRMS system for the quantification of the stable isotopes of carbon monoxide from ice cores and small air samples

    Directory of Open Access Journals (Sweden)

    Z. Wang

    2009-10-01

    Full Text Available A new simultaneous analysis technique for stable isotope ratios (δ13C and δ18O of atmospheric carbon monoxide (CO from ice core samples and small air samples is presented, based on an on-line cryogenic vacuum extraction followed by continuous-flow isotope ratio mass spectrometry (CF-IRMS. The CO extraction system includes two multi-loop cryogenic cleanup traps, a chemical oxidant for oxidation to CO2, a cryogenic collection trap, a cryofocusing unit, purification by gas chromatography, and subsequent injection into a Finnigan Delta Plus IRMS. Analytical precision of 0.2‰(±1σ for δ13C and 0.6‰(±1σ for δ18O can be obtained for 100 mL (STP air sample with CO mixing ratio ranging from 60 to 140 ppbv (~268–625 pmol CO. Six South Pole ice core samples with depth ranging from 133 to 177 m are also processed for CO isotope analysis based on a wet extraction line attached to the above cryogenic vacuum system. This is the first report on measuring isotope ratios of CO in ice core samples.

  15. Sampling technologies and air pollution control devices for gaseous and particulate arsenic: a review

    International Nuclear Information System (INIS)

    Direct measurement of arsenic release requires a good sampling and analysis procedure in order to capture and detect the total amount of metals emitted. The literature is extensively reviewed in order to evaluate the efficiency of full field-scale and laboratory scale techniques for capturing particulate and gaseous emissions of arsenic from the thermo-chemical treatment of different sources of arsenic. Furthermore, trace arsenic concentrations in ambient air, national standard sampling methods and arsenic analysis methods are considered. Besides sampling techniques, the use of sorbents is also reviewed with respect to both approaches (1) to prevent the metals from exiting with the flue gas and (2) to react or combine with the metals in order to be collected in air pollution control systems. The most important conclusion is that submicron arsenic fumes are difficult to control in conventional air pollution control devices. Complete capture of the arsenic species requires a combination of particle control and vapour control devices. - Submicron arsenic fumes are difficult to control in conventional air pollution control devices

  16. Water and entrapped air redistribution in heterogeneous sand sample: Quantitative neutron imaging of the process

    Science.gov (United States)

    Snehota, Michal; Jelinkova, Vladimira; Sobotkova, Martina; Sacha, Jan; Vontobel, Peter; Hovind, Jan

    2015-02-01

    Saturated flow in soil with the occurrence of preferential flow often exhibits temporal changes of saturated hydraulic conductivity even during the time scale of a single infiltration event. These effects, observed in a number of experiments done mainly on heterogeneous soils, are often attributed to the changing distribution of water and air in the sample. We have measured the variation of the flow rates during the steady state stage of the constant head ponded infiltration experiment conducted on a packed sample composed of three different grades of sand. The experiment was monitored by quantitative neutron imaging, which provided information about the spatial distribution of water in the sample. Measurements were taken during (i) the initial stages of infiltration by neutron radiography and (ii) during the steady state flow by neutron tomography. A gradual decrease of the hydraulic conductivity has been observed during the first 4 h of the infiltration event. A series of neutron tomography images taken during the quasi-steady state stage showed the trapping of air bubbles in coarser sand. Furthermore, the water content in the coarse sand decreased even more while the water content in the embedded fine sand blocks gradually increased. The experimental results support the hypothesis that the effect of the gradual hydraulic conductivity decrease is caused by entrapped air redistribution and the build up of bubbles in preferential pathways. The trapped air thus restricts the preferential flow pathways and causes lower hydraulic conductivity.

  17. Sequential extraction for radionuclide fractionation in soil samples: a comparative study

    International Nuclear Information System (INIS)

    Two sequential extraction procedures, Tessier's method (Anal. Chem. 51(7) (1979) 844), and a current version known as Schultz's method (J. Environ. Radioact. 40(2) (1998) 155), were compared. The two procedures were applied to a natural soil sample that presents high activity concentrations in natural radionuclides of the 238U series. Reproducibility studies of each method and a comparison between the two sets of results were performed for uranium, thorium, and radium. The results were different for each radionuclide. Analysis of the extracted fractions was carried out by alpha spectrometry

  18. Study of microtip-based extraction and purification of DNA from human samples for portable devices

    Science.gov (United States)

    Fotouhi, Gareth

    DNA sample preparation is essential for genetic analysis. However, rapid and easy-to-use methods are a major challenge to obtaining genetic information. Furthermore, DNA sample preparation technology must follow the growing need for point-of-care (POC) diagnostics. The current use of centrifuges, large robots, and laboratory-intensive protocols has to be minimized to meet the global challenge of limited access healthcare by bringing the lab to patients through POC devices. To address these challenges, a novel extraction method of genomic DNA from human samples is presented by using heat-cured polyethyleneimine-coated microtips generating a high electric field. The microtip extraction method is based on recent work using an electric field and capillary action integrated into an automated device. The main challenges to the method are: (1) to obtain a stable microtip surface for the controlled capture and release of DNA and (2) to improve the recovery of DNA from samples with a high concentration of inhibitors, such as human samples. The present study addresses these challenges by investigating the heat curing of polyethyleneimine (PEI) coated on the surface of the microtip. Heat-cured PEI-coated microtips are shown to control the capture and release of DNA. Protocols are developed for the extraction and purification of DNA from human samples. Heat-cured PEI-coated microtip methods of DNA sample preparation are used to extract genomic DNA from human samples. It is discovered through experiment that heat curing of a PEI layer on a gold-coated surface below 150°C could inhibit the signal of polymerase chain reaction (PCR). Below 150°C, the PEI layer is not completely cured and dissolved off the gold-coated surface. Dissolved PEI binds with DNA to inhibit PCR. Heat curing of a PEI layer above 150°C on a gold-coated surface prevents inhibition to PCR and gel electrophoresis. In comparison to gold-coated microtips, the 225°C-cured PEI-coated microtips improve the

  19. Comparison of RNA extraction methods from biofilm samples of Staphylococcus epidermidis

    Directory of Open Access Journals (Sweden)

    França Angela

    2011-12-01

    Full Text Available Abstract Background Microbial biofilms are communities of bacteria adhered to a surface and surrounded by an extracellular polymeric matrix. Biofilms have been associated with increased antibiotic resistance and tolerance to the immune system. Staphylococcus epidermidis is the major bacterial species found in biofilm-related infections on indwelling medical devices. Obtaining high quality mRNA from biofilms is crucial to validate the transcriptional measurements associated with the switching to the biofilm mode of growth. Therefore, we selected three commercially available RNA extraction kits with distinct characteristics, including those using silica membrane or organic extraction methods, and enzymatic or mechanical cell lysis, and evaluated the RNA quality obtained from two distinct S. epidermidis bacterial biofilms. Results RNA extracted using the different kits was evaluated for quantity, purity, integrity, and functionally. All kits were able to extract intact and functional total RNA from the biofilms generated from each S. epidermidis strain. The results demonstrated that the kit based on mechanical lysis and organic extraction (FastRNA® Pro Blue was the only one that was able to isolate pure and large quantities of RNA. Normalized expression of the icaA virulence gene showed that RNA extracted with PureLink™ had a significant lower concentration of icaA mRNA transcripts than the other kits tested. Conclusions When working with complex samples, such as biofilms, that contain a high content extracellular polysaccharide and proteins, special care should be taken when selecting the appropriate RNA extraction system, in order to obtain accurate, reproducible, and biologically significant results. Among the RNA extraction kits tested, FastRNA® Pro Blue was the best option for both S. epidermidis biofilms used.

  20. Development of blood extraction system designed by female mosquito's blood sampling mechanism for bio-MEMS

    Science.gov (United States)

    Tsuchiya, Kazuyoshi; Nakanishi, Naoyuki; Nakamachi, Eiji

    2005-02-01

    A compact and wearable wristwatch type Bio-MEMS such as a health monitoring system (HMS) to detect blood sugar level for diabetic patient, was newly developed. The HMS consists of (1) a indentation unit with a microneedle to generate the skin penetration force using a shape memory alloy(SMA) actuator, (2) a pumping unit using a bimorph PZT piezoelectric actuator to extract the blood and (3) a gold (Au) electrode as a biosensor immobilized GOx and attached to the gate electrode of MOSFET to detect the amount of Glucose in extracted blood. GOx was immobilized on a self assembled spacer combined with an Au electrode by the cross-link method using BSA as an additional bonding material. The device can extract blood in a few microliter through a painless microneedle with the negative pressure by deflection of the bimorph PZT piezoelectric actuator produced in the blood chamber, by the similar way the female mosquito extracts human blood with muscle motion to flex or relax. The performances of the liquid sampling ability of the pumping unit through a microneedle (3.8mm length, 100μm internal diameter) using the bimorph PZT piezoelectric microactuator were measured. The blood extraction micro device could extract human blood at the speed of 2μl/min, and it is enough volume to measure a glucose level, compared to the amount of commercial based glucose level monitor. The electrode embedded in the blood extraction device chamber could detect electrons generated by the hydrolysis of hydrogen peroxide produced by the reaction between GOx and glucose in a few microliter extracted blood, using the constant electric current measurement system of the MOSFET type hybrid biosensor. The output voltage for the glucose diluted in the chamber was increased lineally with increase of the glucose concentration.

  1. Electronic Nose and Use of Bags to Collect Odorous Air Samples in Meat Quality Analysis

    Science.gov (United States)

    Sala, G.; Masoero, G.; Battaglini, L. M.; Cornale, P.; Barbera, S.

    2009-05-01

    To test EN reliability and use of bags on meat, 17 bulls (one group of 9 and one of 8) fed similarly, except for a supplementary feedingstuff, were used. Samples were prepared according to the MCS protocol and repeated three times on different days for a total of 51 samples. Bags were used to collect raw and cooked meat air samples, and to test odour changes among samples analysed at different times. The first time analysis was performed immediately after collection then was repeated, 1 hour, 1 day and 1 week later. The Electronic Nose is very discriminant and clear differences were evident among raw, cooked and bags odorous profiles. The highest values were found in cooked samples and the broad range class (W5S) was the most representative. The EN also recognized the two tested feed treatments. In the cooked samples, all sensor responses decrease while time enhances, indicating a progressive chemical variation of the air composition in the bag, with a less correlation shown in the raw samples. When using bags, to avoid bias, is important to fix analysis in order to obtain useful results.

  2. Diffusive sampling and measurement of microbial volatile organic compounds in indoor air.

    Science.gov (United States)

    Araki, A; Eitaki, Y; Kawai, T; Kanazawa, A; Takeda, M; Kishi, R

    2009-10-01

    Microbial volatile organic compounds (MVOC), chemicals emitted from various microorganisms, in indoor air have been of concern in recent years. For large field studies, diffusive samplers are widely used to measure indoor environments. Since the sampling rate of a sampler is a fundamental parameter to calculate concentration, the sampling rates of eight MVOC with diffusive samplers were determined experimentally using a newly developed water-bubbling method: air was supplied to the MVOC-solutions and the vapor collected in an exposure bag, where diffusive and active samplers were placed in parallel for comparison. Correlations between the diffusive and active samplings gave good linear regressions. The sampling rates were 30-35 ml/min and the detection limits were 0.044-0.178 microg/m(3), as determined by GC/MS analysis. Application of the sampling rates in indoor air was validated by parallel sampling of the diffusive and active sampling method. 5% Propan-2-ol/CS(2) was the best solvent to desorb the compounds from absorbents. The procedure was applied to a field study in 41 dwellings. The most frequently detected compounds were hexan-2-one and heptan-2-one, with 97.5% detection rates and geometric mean values of 0.470 and 0.302 microg/m(3), respectively. This study shows that diffusive samplers are applicable to measure indoor MVOC levels. Practical Implications At present, there are still limited reports on indoor Microbial Volatile Organic Compounds (MVOC) levels in general dwellings and occupants' health. Compared with active sampling methods, air sampling using a diffusive sampler is particularly advantageous for use in large field studies due to its smallness, light-size, easy-handling, and cost-effectiveness. In this study, sampling rates of selected MVOC of the diffusive sampler were determined using the water-bubbling method: generating gases by water-bubbling and exposing the diffusive and active samplers at the same time. The obtained sampling rates

  3. Monitoring Airborne Fungal Spores in an Experimental Indoor Environment To Evaluate Sampling Methods and the Effects of Human Activity on Air Sampling

    OpenAIRE

    Buttner, M P; Stetzenbach, L D

    1993-01-01

    Aerobiological monitoring was conducted in an experimental room to aid in the development of standardized sampling protocols for airborne microorganisms in the indoor environment. The objectives of this research were to evaluate the relative efficiencies of selected sampling methods for the retrieval of airborne fungal spores and to determine the effect of human activity on air sampling. Dry aerosols containing known concentrations of Penicillium chrysogenum spores were generated, and air sam...

  4. Polyurethane foam (PUF) disks passive air samplers: Wind effect on sampling rates

    Energy Technology Data Exchange (ETDEWEB)

    Tuduri, Ludovic [Equipe Perigourdine de Chimie Appliquee, Laboratoire de Physico-toxicochimie des systemes naturels, Universite Bordeaux I, Site universitaire, 24019 Perigueux cedex (France)]. E-mail: l.tuduri@epca.u-bordeaux1.fr; Harner, Tom [Science and Technology Branch, Environment Canada, 4905 Dufferin Street, Toronto, Ontario M3H 5T4 (Canada); Hung, Hayley [Science and Technology Branch, Environment Canada, 4905 Dufferin Street, Toronto, Ontario M3H 5T4 (Canada)

    2006-11-15

    Different passive sampler housings were evaluated for their wind dampening ability and how this might translate to variability in sampler uptake rates. Polyurethane foam (PUF) disk samplers were used as the sampling medium and were exposed to a PCB-contaminated atmosphere in a wind tunnel. The effect of outside wind speed on PUF disk sampling rates was evaluated by exposing polyurethane foam (PUF) disks to a PCB-contaminated air stream in a wind tunnel over air velocities in the range 0 to 1.75 m s{sup -1}. PUF disk sampling rates increased gradually over the range 0-0.9 m s{sup -1} at {approx}4.5-14.6 m{sup 3} d{sup -1} and then increased sharply to {approx}42 m{sup 3} d{sup -1} at {approx}1.75 m s{sup -1} (sum of PCBs). The results indicate that for most field deployments the conventional 'flying saucer' housing adequately dampens the wind effect and will yield approximately time-weighted air concentrations. - Passive sampler housings dampen wind speed and reduce the variability in sampling rates.

  5. Greenhouse gas analysis of air samples collected onboard the CARIBIC passenger aircraft

    Science.gov (United States)

    Schuck, T. J.; Brenninkmeijer, C. A. M.; Slemr, F.; Xueref-Remy, I.; Zahn, A.

    2009-08-01

    CARIBIC (Civil Aircraft for the Regular Investigation of the atmosphere Based on an Instrument Container) is a long-term atmospheric measurement program based on the use of a comprehensive scientific instrument package aboard a commercial passenger aircraft. In addition to real-time measurements, whole air sampling is performed regularly at cruising altitudes in the tropical middle troposphere and the extra-tropical UT/LS region. Air samples are analyzed for greenhouse gases, NMHCs, halocarbons, and trace gas isotopic composition. The routinely performed greenhouse gas analysis comprises gas chromatography measurements of CO2, CH4, N2O and SF6. The air sampling procedure, the GC system and its performance are described. Comparisons with similar systems employed in other laboratories and a comparison with results from a CO2 in-situ analyzer that is also part of the CARIBIC instrumentation are shown. In addition, the time series of CO2, obtained from the collection of 684 samples at latitudes between 30° N and 56° N on 21 round trips out of Germany to different destinations in Asia between November 2005 and October 2008, is presented. A time shift in the seasonal cycle of about one month was observed between the upper troposphere and the tropopause region. For two sets of return flights from Germany to the Philippines the relationship between the four greenhouse gases is briefly discussed.

  6. Polyurethane foam (PUF) disks passive air samplers: Wind effect on sampling rates

    International Nuclear Information System (INIS)

    Different passive sampler housings were evaluated for their wind dampening ability and how this might translate to variability in sampler uptake rates. Polyurethane foam (PUF) disk samplers were used as the sampling medium and were exposed to a PCB-contaminated atmosphere in a wind tunnel. The effect of outside wind speed on PUF disk sampling rates was evaluated by exposing polyurethane foam (PUF) disks to a PCB-contaminated air stream in a wind tunnel over air velocities in the range 0 to 1.75 m s-1. PUF disk sampling rates increased gradually over the range 0-0.9 m s-1 at ∼4.5-14.6 m3 d-1 and then increased sharply to ∼42 m3 d-1 at ∼1.75 m s-1 (sum of PCBs). The results indicate that for most field deployments the conventional 'flying saucer' housing adequately dampens the wind effect and will yield approximately time-weighted air concentrations. - Passive sampler housings dampen wind speed and reduce the variability in sampling rates

  7. Usefulness of FTA® cards as a Pneumocystis-DNA extraction method in bronchoalveolar lavage samples.

    Science.gov (United States)

    Rodiño, Jenniffer M; Aguilar, Yudy A; Rueda, Zulma Vanessa; Vélez, Lázaro A

    2016-05-01

    Background FTA® cards (Fast Technology for Analysis of Nucleic Acids) are an alternative DNA extraction method in bronchoalveolar lavage (BAL) samples for Pneumocystis jirovecii molecular analyses. The goal was to evaluate the usefulness of FTA® cards to detect P. jirovecii-DNA by PCR in BAL samples compared to silica adsorption chromatography (SAC). Methods This study used 134 BAL samples from immunocompromised patients previously studied to establish microbiological aetiology of pneumonia, among them 15 cases of Pneumocystis pneumonia (PCP) documented by staining and 119 with other alternative diagnoses. The FTA® system and SAC were used for DNA extraction and then amplified by nested PCR to detect P. jirovecii. Performance and concordance of the two DNA extraction methods compared to P. jirovecii microscopy were calculated. The influence of the macroscopic characteristics, transportation of samples and the duration of the FTA® card storage (1, 7, 10 or 12 months) were also evaluated. Results Among 134 BAL samples, 56% were positive for P. jirovecii-DNA by SAC and 27% by FTA®. All 15 diagnosed by microscopy were detected by FTA® and SAC. Specificity of the FTA® system and SAC were 82.4% and 49.6%, respectively. Compared to SAC, positivity by FTA® decreased with the presence of blood in BAL (62% vs 13.5%). The agreement between samples at 7, 10 and 12 months was 92.5% for FTA®. Positive cases by FTA® remained the same after shipment by mail. Conclusions Results suggest that FTA® is a practical, safe and economical method to preserve P. jirovecii-DNA in BAL samples for molecular studies. PMID:26950684

  8. PLS regression using real sample calibration for aluminum and iron determination in plant extracts.

    Science.gov (United States)

    Coscione, Aline Renée; de, AndradeJoãoCarlos; Poppi, Ronei J

    2002-01-01

    Real samples were used for PLS model calibration and validation steps, showing that this approach can be of value in preventing deviations in the results caused by the matrix effects for the simultaneous spectrophotometric determination of aluminum and iron in plant extracts. One hundred UV-vis spectra, obtained from samples of the 1997 to 2000 International Plant-Analytical Exchange (IPE) program (The Netherlands), were used for model development, with ICP-AES aluminum and iron determinations as reference values for model calculation. The plant extracts were analyzed both by ICP-AES and by the PLS models developed in this work, using calibrations with both aqueous standard solutions and with real sample extracts. In addition, since the use of smaller calibration sets could be of value in reducing both the cost and the time of analysis, sets with fewer calibration samples were also investigated, with the help of the Kennard and Stone algorithm for sample selection. Comparison of the predictability of the best model obtained with each calibration set was made using the ratio of their relative root mean square error (%RMSEV) for samples in the validation set, for aluminum or iron determinations, and were compared against F-test tabulated values. For all the models developed with real samples, the differences in the %RMSEV values for the aluminum or iron determinations were found not to be statistically significant, at a confidence level of 95%. Although it was observed that the aluminum, but not the iron, determinations with the PLS 2 model prepared with aqueous standards tend to be slightly lower than the ICP-AES determinations, this model has a good global prediction ability, as observed through the correlation curves presented, and can be used for screening determinations or for other agricultural purposes. PMID:11827380

  9. Studies on radioactivities of dust samples in the air at high-altitudes

    International Nuclear Information System (INIS)

    The radioactivity concentrations of airborne dust samples were studied. The samples had been collected at high altitude by the Japan Air Self-Defense Force in June 2011 and from September 2011 to March 2012. The obtained data were gross beta radioactivity analysis and gamma nuclide analysis. It is shown that cesium 137 and cesium 134 were detected at the 10 km and 3 km altitude of central area of Japan in almost all the samples. Also, those nuclides were detected around north and west areas of Japan in some samples. Radioactive gases (gaseous radioiodine and radioactive xenon gas) are not detected in all the samples. Refer the report already submitted with regard to the results on radionuclide measurements of Technical Research and Development Institute executed for examining 'the nuclear emergency situation at Fukushima Daiichi and Daini nuclear power plants' after 'Tohoku Region Pacific Ocean Earthquake' on March 11, 2011. (author)

  10. Portable monitors for measuring radon and its progenies air by intergrated sampling method

    International Nuclear Information System (INIS)

    Two kinds of portable monitors have been developed, which can be used to measure the concentration of radon or potential energy concentration of radon or potential energy concentration of radon progenies in air. The thermoluminescent material CaSO4(Tm) is used as a detecting element for both of them. The lowest detectable limit of the passive radon monitor is about 1.5 Bq/m3 for radon in air, as the exposure time being one week. Its main advantages are high reliability and convenient manipulation. The working level monitor for radon progenies in air consists of a mini membrane pump and an integrating probe. The lowest detectable limit is about 6.2 x 10-9 J/m3, as the sampling time being 6 hours. It weights only about 0.35 kg

  11. Desorption atmospheric pressure photoionization with polydimethylsiloxane as extraction phase and sample plate material

    Energy Technology Data Exchange (ETDEWEB)

    Vaikkinen, A. [Division of Pharmaceutical Chemistry, Faculty of Pharmacy, P.O. Box 56, FIN-00014 University of Helsinki (Finland); Kotiaho, T. [Division of Pharmaceutical Chemistry, Faculty of Pharmacy, P.O. Box 56, FIN-00014 University of Helsinki (Finland); Laboratory of Analytical Chemistry, Department of Chemistry, P.O. Box 55, FIN-00014 University of Helsinki (Finland); Kostiainen, R. [Division of Pharmaceutical Chemistry, Faculty of Pharmacy, P.O. Box 56, FIN-00014 University of Helsinki (Finland); Kauppila, T.J., E-mail: tiina.kauppila@helsinki.fi [Division of Pharmaceutical Chemistry, Faculty of Pharmacy, P.O. Box 56, FIN-00014 University of Helsinki (Finland)

    2010-12-03

    Desorption atmospheric pressure photoionization (DAPPI) is an ambient ionization technique for mass spectrometry (MS) that can be used to ionize polar as well as neutral and completely non-polar analytes. In this study polydimethylsiloxane (PDMS) was used as a solid phase extraction sorbent for DAPPI-MS analysis. Pieces of PDMS polymer were soaked in an aqueous sample, where the analytes were sorbed from the sample solution to PDMS. After this, the extracted analytes were desorbed directly from the polymer by the hot DAPPI spray solvent plume, without an elution step. Swelling and extracting the PDMS with a cleaning solvent prior to extraction diminished the high background in the DAPPI mass spectrum caused by PDMS oligomers. Acetone, hexane, pentane, toluene, diisopropylamine and triethylamine were tested for this purpose. The amines were most efficient in reducing the PDMS background, but they also suppressed the signals of low proton affinity analytes. Toluene was chosen as the optimum cleaning solvent, since it reduced the PDMS background efficiently and gave intensive signals of most of the studied analytes. The effects of DAPPI spray solvents toluene, acetone and anisole on the PDMS background and the ionization of analytes were also compared and extraction conditions were optimized. Anisole gave a low background for native PDMS, but toluene ionized the widest range of analytes. Analysis of verapamil, testosterone and anthracene from purified, spiked wastewater was performed to demonstrate that the method is suited for in-situ analysis of water streams. In addition, urine spiked with several analytes was analyzed by the PDMS method and compared to the conventional DAPPI procedure, where sample droplets are applied on PMMA surface. With the PDMS method the background ion signals caused by the urine matrix were lower, the S/N ratios of analytes were 2-10 times higher, and testosterone, anthracene and benzo[a]pyrene that were not detected from PMMA in urine

  12. Radium 226 and lead 210 water extraction from mill tailings samples

    International Nuclear Information System (INIS)

    Depositories for waste from the processing of uranium ore may release seepage waters into the environment through their impoundments. Seepage waters, when percolating through the wastes, extract radium 226. In the design or rehabilitation stage of such depositories, the exposure of critical groups of the population to radium 226 from the ground water pathway must be assessed. The same applies to lead 210. The first step is to assess the possibility of extracting the radium 226 and the lead 210 from samples of solid wastes and sludges in laboratory tests using water from the site. Extensive tests of this type were carried out in our laboratories between 1982 and 1991 on samples of mill tailings which had been collected in six installations of COGEMA and its subsidiaries. The main results are presented and analyzed. Physical, chemical and mineralogical factors influencing the leaching rates and the total quantity of water-extractable radium 226 are identified. In the case of a wet storage option, a tentative modelling of the water extraction phenomenon is proposed for the prediction of the source term both in the short term, and in the long term when all more or less soluble salts have been eliminated from the solid wastes

  13. Ion-exchange molecularly imprinted polymer for the extraction of negatively charged acesulfame from wastewater samples.

    Science.gov (United States)

    Zarejousheghani, Mashaalah; Schrader, Steffi; Möder, Monika; Lorenz, Pierre; Borsdorf, Helko

    2015-09-11

    Acesulfame is a known indicator that is used to identify the introduction of domestic wastewater into water systems. It is negatively charged and highly water-soluble at environmental pH values. In this study, a molecularly imprinted polymer (MIP) was synthesized for negatively charged acesulfame and successfully applied for the selective solid phase extraction (SPE) of acesulfame from influent and effluent wastewater samples. (Vinylbenzyl)trimethylammonium chloride (VBTA) was used as a novel phase transfer reagent, which enhanced the solubility of negatively charged acesulfame in the organic solvent (porogen) and served as a functional monomer in MIP synthesis. Different molecularly imprinted polymers were synthesized to optimize the extraction capability of acesulfame. The different materials were evaluated using equilibrium rebinding experiments, selectivity experiments and scanning electron microscopy (SEM). The most efficient MIP was used in a molecularly imprinted-solid phase extraction (MISPE) protocol to extract acesulfame from wastewater samples. Using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) analysis, detection and quantification limits were achieved at 0.12μgL(-1) and 0.35μgL(-1), respectively. Certain cross selectivity for the chemical compounds containing negatively charged sulfonamide functional group was observed during selectivity experiments. PMID:26256920

  14. Results Of Analytical Sample Crosschecks For Next Generation Solvent Extraction Samples Isopar L Concentration And pH

    International Nuclear Information System (INIS)

    As part of the implementation process for the Next Generation Cesium Extraction Solvent (NGCS), SRNL and F/H Lab performed a series of analytical cross-checks to ensure that the components in the NGCS solvent system do not constitute an undue analytical challenge. For measurement of entrained Isopar(regsign) L in aqueous solutions, both labs performed similarly with results more reliable at higher concentrations (near 50 mg/L). Low bias occurred in both labs, as seen previously for comparable blind studies for the baseline solvent system. SRNL recommends consideration to use of Teflon(trademark) caps on all sample containers used for this purpose. For pH measurements, the labs showed reasonable agreement but considerable positive bias for dilute boric acid solutions. SRNL recommends consideration of using an alternate analytical method for qualification of boric acid concentrations.

  15. 14C AMS measurements of tree leaf samples to monitor air pollution induced by city traffic

    International Nuclear Information System (INIS)

    In the past, many radiocarbon measurement have been made for environmental studies such as source apportionment of air-borne particulates, and studies of the anthropogenic effects of nuclear power plants. In this presentation we report our accelerator mass spectrometry (AMS) measurements of radiocarbon on tree leaf samples to investigate the impact of city traffic on our living-environment. The fossil-burning vehicles emit carbon dioxide (CO2) free of 14C content and, when mixed with the clean air CO2, lower 14C ratio compared to the normal reservoir value. This so-called Suess effect can be incorporated to monitor air quality in our living environments, since metabolic processes maintain the 14C content of living organism in equilibrium with atmospheric 14C. In other words, dead CO2 is admixed to the normal atmospheric CO2 and then photo-synthetically assimilated by the plants. Two kinds of tree leaf samples; pine tree needles and Ginkgo tree leaves were collected during a one-week period in the summer 1996 at five different locations with various traffic conditions in the region, within a 10-km diameter circle, south of the River Han, Seoul. The AMS targets were made by a simple sample-making procedure. The leaves have been pretreated by a standard acid-alkali treatment and then charred in a vacuum evaporator by applying ca. 800 deg C heat. The charred samples were mixed with Ag powder and pressed into the Al target holder for the AMS measurement.The AMS measurements were made using the accelerator mass spectrometry facilities of the Leibniz-Labor at the Christian-Albrecht University, Kiel,Germany. The observed Δ14C values, which ranged from 60TM to 158TM, have a good correlation with the traffic conditions in the places where the sampling took place and show a remarkable capability of 14C AMS measurements to monitor our fossil burning environment. The volume ratios of clean air to air from fossil-burn origin in the environmental CO2 reached to a level of 8

  16. Sample pretreatment microfluidic chip for DNA extraction from rat peripheral blood

    Institute of Scientific and Technical Information of China (English)

    CHEN Xing; CUI Dafu; LIU Changchun; LI Hui; ZHAO Weixing

    2007-01-01

    A sample pretreatment microfluidic chip was described based on the principle of solid phase extraction and micro electro mechanical system technology.Oxidized porous silicon with the large surface area as the solid phase matrix for absorption of DNA from a biological sample can greatly improve the DNA yield.The factors that could affect the DNA yield were analyzed and the preparation technology and the experiment procedure were improved.The DNA purification process from the rat peripheral blood can be achieved and the DNA yield is 24 ng/(μL whole blood),which can reach the level of the commercial DNA purification kits.Furthermore,the DNA extracted from the whole blood can be amplified by polymerase chain reaction,which can achieve a high efficiency of the amplification.

  17. Optimized methods for extracting circulating small RNAs from long-term stored equine samples.

    Science.gov (United States)

    Unger, Lucia; Fouché, Nathalie; Leeb, Tosso; Gerber, Vincent; Pacholewska, Alicja

    2016-01-01

    Circulating miRNAs in body fluids, particularly serum, are promising candidates for future routine biomarker profiling in various pathologic conditions in human and veterinary medicine. However, reliable standardized methods for miRNA extraction from equine serum and fresh or archived whole blood are sorely lacking. We systematically compared various miRNA extraction methods from serum and whole blood after short and long-term storage without addition of RNA stabilizing additives prior to freezing. Time of storage at room temperature prior to freezing did not affect miRNA quality in serum. Furthermore, we showed that miRNA of NGS-sufficient quality can be recovered from blood samples after >10 years of storage at -80 °C. This allows retrospective analyses of miRNAs from archived samples. PMID:27356979

  18. CAS-H3 type device for sampling tritium from air

    International Nuclear Information System (INIS)

    CAS-H3 type devices is designed for sampling tritiated water vapors and H3 inside nuclear power plants or outside, within a 30 km radius. The devices is supplied by means of two 1.25 Vcc batteries while to ensure an independent long operation it is provided with two photocells for recharge the batteries. The device is conceived to retain integrally both tritiated water vapors and free tritium from the air flow passing through it. The principal components are: - mechanical filter; - oxidizing catalyst; - photocell; - bag; - minipump; - shaking box; - 2.5 V battery; - flowmeter. Technical characteristics are: - air sampling flowrate, 12 l/min; - minipump motor power, 3 W / 3 V; - supply voltage 2.5 Vcc; - size 450 x 350 x 120 mm; - weight 5 kg

  19. Methods for extracting genomic DNA from whole blood samples: current perspectives

    OpenAIRE

    Griffiths, Lyn

    2014-01-01

    Diego Chacon-Cortes, Lyn R Griffiths Genomics Research Centre, Institute of Health and Biomedical Innovation, Queensland University of Technology, Kelvin Grove, QLD, Australia Abstract: Deoxyribonucleic acid (DNA) extraction has considerably evolved since it was initially performed back in 1869. It is the first step required for many of the available downstream applications used in the field of molecular biology. Whole blood samples are one of the main sources used to obtain DNA, and there a...

  20. Detection of Streptococcus mutans Genomic DNA in Human DNA Samples Extracted from Saliva and Blood

    OpenAIRE

    weyant, Robert J.; Richard Crout; McNeil, Daniel W.; Adriana Modesto; Iêda M. Orioli; Figen Seymen; Eduardo E. Castilla; Lopez-Camelo, Jorge S.; Steven Wendell; Renato Menezes; Ariadne Letra; Mereb, Juan C.; Mine Yildirim; Poletta, Fernando A.; Christopher Rozhon

    2011-01-01

    Caries is a multifactorial disease, and studies aiming to unravel the factors modulating its etiology must consider all known predisposing factors. One major factor is bacterial colonization, and Streptococcus mutans is the main microorganism associated with the initiation of the disease. In our studies, we have access to DNA samples extracted from human saliva and blood. In this report, we tested a real-time PCR assay developed to detect copies of genomic DNA from Streptococcus mutans in 1,4...

  1. Release of Free DNA by Membrane-Impaired Bacterial Aerosols Due to Aerosolization and Air Sampling

    OpenAIRE

    Zhen, Huajun; Han, Taewon; Fennell, Donna E.; Mainelis, Gediminas

    2013-01-01

    We report here that stress experienced by bacteria due to aerosolization and air sampling can result in severe membrane impairment, leading to the release of DNA as free molecules. Escherichia coli and Bacillus atrophaeus bacteria were aerosolized and then either collected directly into liquid or collected using other collection media and then transferred into liquid. The amount of DNA released was quantified as the cell membrane damage index (ID), i.e., the number of 16S rRNA gene copies in ...

  2. A fast responding continuous tritium-in-air monitor with multi stream sampling for area monitoring

    International Nuclear Information System (INIS)

    A fast responding Tritium-in-Air monitor with multi stream sampling up to a maximum of 8 lines has been developed and field tested for continuous area monitoring in Pressurised Heavy Water Reactors (PHWR) and other tritium handling facilities. The instrument has built in electronic compensation for external gamma and gaseous radionuclide 133Xe (FPNG). The monitor is based on plastic scintillator detector prepared from 5μm thick scintillator film of surface area (each side) of about 250 cm2. Four such films of each weighing 150 mg are packed in a flow cell of 6.3 cm3 volume, made of stainless steel body and Teflon window. The flow cell is coupled face to face to a matched pair of photomultipliers. Measurement is made in coincidence mode of counting. The complete monitor consists of electronic counting system, the detector probe assembly, a diaphragm type of air sampling pump, a particulate filter trap and a rotometer for controlling the air flow rate. For multi stream sampling an external solenoid driver cum isolation unit has been integrated with the system. The efficiency for Tritium vapour for direct passage of sample air through the detector is ∼22%. The instrument records 0.2 cps under normal gamma background of 0.1 - 0.2 μSv/hr, without shielding. With the detector fully shielded (∼ 10 cm thick lead), the instrument does not register significant increase in the background counts with 200 μSv/hr ambient gamma field. Under conditions of gaseous radionuclide interference such as 133Xe (26 MBq/m3 concentrations) the MDA rises to ∼1 DAC for a counting time of 300 s. The MDA under ideal conditions is found to be 0.2 DAC for Tritium vapour. The sensitivity of the system is 0.4 CPS per DAC. The instrument response time is 10 minutes. (author)

  3. Microporous Carbon Spheres Solid Phase Membrane Tip Extraction for the Analysis of Nitrosamines in Water Samples

    International Nuclear Information System (INIS)

    A simple solid phase membrane tip extraction (SPMTE) utilizing microporous carbon spheres (MCS) was developed for the analysis of nitrosamines in aqueous samples. The method termed MCS-SPMTE was optimized for various important extraction parameters namely conditioning organic solvent, extraction time, effects of salt addition and pH change, desorption time, desorption solvent and sample volume. Under the optimized conditions, the method indicated good linearity in the range of 10-100 μg/ L with coefficients of determination, r2≥0.9984. The method also demonstrated good reproducibility with % RSDs values ranging from 2.2 - 8.9 (n = 3). Limit of detection (LOD) and limit of quantification (LOQ) for the method ranged from 3.2 - 4.8 μg/ L and 10.9 - 15.9 μg/L respectively. Recoveries for both tap-water and lake water samples spiked at 10 μg/L were in the range of 83.2 - 107.5 %. (author)

  4. Evaluation of metal ions in rice samples: extraction and direct determination by ICP OES

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Andrea; Cadore, Solange, E-mail: cadore@iqm.unicamp.br [Instituto de Quimica, Universidade Estadual de Campinas, Campinas-SP (Brazil); Baccan, Nivaldo [Faculdade de Paulinia, Paulinia-SP (Brazil)

    2012-05-15

    A method for extraction of metal ions present in rice samples using ammoniacal EDTA solution, pH = 10, as extractor agent is proposed under the following optimized conditions: 0.20 g of rice sample and 5.00 mL of ammoniacal EDTA (ethylenediaminetetraacetic acid) solution, with 5 min of ultrasound exposure time. Using robust ICP OES (inductively coupled plasma atomic emission spectrometry) conditions, direct analysis of the extraction solution was allowed, and the recovery values obtained were above 90% for most of the studied elements (P, K, Mg, Ca, Zn, Mn, Cu and Mo) with RSD < 5%. The results were in good agreement with those obtained by microwave assisted extraction and for the reference material of rice flour (NIST SRM 1568a). The limits of detection of method were in the range of 0.007 mg kg{sup -1} (Mn) - 48.68 mg kg{sup -1} (K), showing adequate detectability for the determination of the analytes. The analysis of different samples indicated that Brazilian 'integral' rice contains higher contents of the constituents studied, followed by 'parboiled' rice, and the 'agulhinha' rice a long and thin grain type. (author)

  5. Electromembrane extraction of gonadotropin-releasing hormone agonists from plasma and wastewater samples.

    Science.gov (United States)

    Nojavan, Saeed; Bidarmanesh, Tina; Mohammadi, Ali; Yaripour, Saeid

    2016-03-01

    In the present study, for the first time electromembrane extraction followed by high performance liquid chromatography coupled with ultraviolet detection was optimized and validated for quantification of four gonadotropin-releasing hormone agonist anticancer peptides (alarelin, leuprolide, buserelin and triptorelin) in biological and aqueous samples. The parameters influencing electromigration were investigated and optimized. The membrane consists 95% of 1-octanol and 5% di-(2-ethylhexyl)-phosphate immobilized in the pores of a hollow fiber. A 20 V electrical field was applied to make the analytes migrate from sample solution with pH 7.0, through the supported liquid membrane into an acidic acceptor solution with pH 1.0 which was located inside the lumen of hollow fiber. Extraction recoveries in the range of 49 and 71% within 15 min extraction time were obtained in different biological matrices which resulted in preconcentration factors in the range of 82-118 and satisfactory repeatability (7.1 < RSD% < 19.8). The method offers good linearity (2.0-1000 ng/mL) with estimation of regression coefficient higher than 0.998. The procedure allows very low detection and quantitation limits of 0.2 and 0.6 ng/mL, respectively. Finally, it was applied to determination and quantification of peptides in human plasma and wastewater samples and satisfactory results were yielded. PMID:26799761

  6. Isotopic air sampling in a tallgrass prairie to partition net ecosystem CO2 exchange

    Science.gov (United States)

    Lai, Chun-Ta; Schauer, Andrew J.; Owensby, Clenton; Ham, Jay M.; Ehleringer, James R.

    2003-09-01

    Stable isotope ratios of various ecosystem components and net ecosystem exchange (NEE) CO2 fluxes were measured in a C3-C4 mixture tallgrass prairie near Manhattan, Kansas. The July 2002 study period was chosen because of contrasting soil moisture contents, which allowed us to address the effects of drought on photosynthetic CO2 uptake and isotopic discrimination. Significantly higher NEE fluxes were observed for both daytime uptake and nighttime respiration during well-watered conditions when compared to a drought period. Given these differences, we investigated two carbon-flux partitioning questions: (1) What proportions of NEE were contributed by C3 versus C4 species? (2) What proportions of NEE fluxes resulted from canopy assimilation versus ecosystem respiration? To evaluate these questions, air samples were collected every 2 hours during daytime for 3 consecutive days at the same height as the eddy covariance system. These air samples were analyzed for both carbon isotope ratios and CO2 concentrations to establish an empirical relationship for isoflux calculations. An automated air sampling system was used to collect nighttime air samples to estimate the carbon isotope ratios of ecosystem respiration (δR) at weekly intervals for the entire growing season. Models of C3 and C4 photosynthesis were employed to estimate bulk canopy intercellular CO2 concentration in order to calculate photosynthetic discrimination against 13C. Our isotope/NEE results showed that for this grassland, C4 vegetation contributed ˜80% of the NEE fluxes during the drought period and later ˜100% of the NEE fluxes in response to an impulse of intense precipitation. For the entire growing season, the C4 contribution ranged from ˜68% early in the spring to nearly 100% in the late summer. Using an isotopic approach, the calculated partitioned respiratory fluxes were slightly greater than chamber-measured estimates during midday under well-watered conditions. In addition, time series

  7. Solvent extraction method for rapid separation of strontium-90 in milk and food samples

    International Nuclear Information System (INIS)

    A solvent extraction method, using tributyl phosphate, for rapid separation of strontium-90 in milk and other food samples has been presented in this report in view of large number of samples recieved after Chernobyl accident for checking radioactive contamination. The earlier nitration method in use for the determination of 90Sr through its daughter 90Y takes over two weeks for analysis of a sample. While by this extraction method it takes only 4 to 5 hours for sample analysis. Complete estimation including initial counting can be done in a single day. The chemical recovery varies between 80-90% compared to nitration method which is 65-80%. The purity of the method has been established by following the decay of yttrium-90 separated. Some of the results obtained by adopting this chemical method for food analysis are included. The method is, thus, found to be rapid and convenient for accurate estimation of strontium-90 in milk and food samples. (author). 2 tabs., 1 fig

  8. Technical assessment of TRUSAF for compliance with work place air sampling. Revision 1

    International Nuclear Information System (INIS)

    The purpose of this Technical Work Document is to satisfy WHC-CM-1-6, the ''WHC Radiological Control Manual.'' This first revision of the original Supporting Document covers the period from January 1, 1994 to December 31, 1994. WHC-CM-1-6 is the primary guidance for radiological control at Westinghouse Hanford Company (WHC). As such, it complies with Title 10, Part 835 of the Code of Federal Regulations. In addition to WHC-CM-1-6, there is HSRCM-1, the ''Hanford Site Radiological Control Manual'' and several Department of Energy (DOE) Orders, national consensus standards, and reports that provide criteria, standards, and requirements for workplace air sampling programs. This document provides a summary of these, as they apply to WHC facility workplace air sampling programs. this document also provides an evaluation of the compliance of the TRUSAF workplace air sampling program to the criteria, standards, and requirements and documents. Where necessary, it also indicates changes needed to bring specific locations into compliance

  9. Technical assessment of workplace air sampling requirements at tank farm facilities. Revision 1

    International Nuclear Information System (INIS)

    WHC-CM-1-6 is the primary guidance for radiological control at Westinghouse Hanford Company (WHC). It was written to implement DOE N 5480.6 ''US Department of Energy Radiological Control Manual'' as it applies to programs at Hanford which are now overseen by WHC. As such, it complies with Title 10, Part 835 of the Code of Federal Regulations. In addition to WHC-CM-1-6, there is HSRCM-1, the ''Hanford Site Radiological Control Manual'' and several Department of Energy (DOE) Orders, national consensus standards, and reports that provide criteria, standards, and requirements for workplace air sampling programs. This document provides a summary of these, as they apply to WHC facility workplace air sampling programs. This document also provides an evaluation of the compliance of Tank Farms' workplace air sampling program to the criteria, standards, and requirements and documents compliance with the requirements where appropriate. Where necessary, it also indicates changes needed to bring specific locations into compliance

  10. Estimation of regional air-quality damages from Marcellus Shale natural gas extraction in Pennsylvania

    International Nuclear Information System (INIS)

    This letter provides a first-order estimate of conventional air pollutant emissions, and the monetary value of the associated environmental and health damages, from the extraction of unconventional shale gas in Pennsylvania. Region-wide estimated damages ranged from $7.2 to $32 million dollars for 2011. The emissions from Pennsylvania shale gas extraction represented only a few per cent of total statewide emissions, and the resulting statewide damages were less than those estimated for each of the state’s largest coal-based power plants. On the other hand, in counties where activities are concentrated, NOx emissions from all shale gas activities were 20–40 times higher than allowable for a single minor source, despite the fact that individual new gas industry facilities generally fall below the major source threshold for NOx. Most emissions are related to ongoing activities, i.e., gas production and compression, which can be expected to persist beyond initial development and which are largely unrelated to the unconventional nature of the resource. Regulatory agencies and the shale gas industry, in developing regulations and best practices, should consider air emissions from these long-term activities, especially if development occurs in more populated areas of the state where per-ton emissions damages are significantly higher. (letter)

  11. Machine learning based sample extraction for automatic speech recognition using dialectal Assamese speech.

    Science.gov (United States)

    Agarwalla, Swapna; Sarma, Kandarpa Kumar

    2016-06-01

    Automatic Speaker Recognition (ASR) and related issues are continuously evolving as inseparable elements of Human Computer Interaction (HCI). With assimilation of emerging concepts like big data and Internet of Things (IoT) as extended elements of HCI, ASR techniques are found to be passing through a paradigm shift. Oflate, learning based techniques have started to receive greater attention from research communities related to ASR owing to the fact that former possess natural ability to mimic biological behavior and that way aids ASR modeling and processing. The current learning based ASR techniques are found to be evolving further with incorporation of big data, IoT like concepts. Here, in this paper, we report certain approaches based on machine learning (ML) used for extraction of relevant samples from big data space and apply them for ASR using certain soft computing techniques for Assamese speech with dialectal variations. A class of ML techniques comprising of the basic Artificial Neural Network (ANN) in feedforward (FF) and Deep Neural Network (DNN) forms using raw speech, extracted features and frequency domain forms are considered. The Multi Layer Perceptron (MLP) is configured with inputs in several forms to learn class information obtained using clustering and manual labeling. DNNs are also used to extract specific sentence types. Initially, from a large storage, relevant samples are selected and assimilated. Next, a few conventional methods are used for feature extraction of a few selected types. The features comprise of both spectral and prosodic types. These are applied to Recurrent Neural Network (RNN) and Fully Focused Time Delay Neural Network (FFTDNN) structures to evaluate their performance in recognizing mood, dialect, speaker and gender variations in dialectal Assamese speech. The system is tested under several background noise conditions by considering the recognition rates (obtained using confusion matrices and manually) and computation time

  12. Measurement of the Tracer Gradient and Sampling System Bias of the Hot Fuel Examination Facility Stack Air Monitoring System

    Energy Technology Data Exchange (ETDEWEB)

    Glissmeyer, John A.; Flaherty, Julia E.

    2011-07-20

    This report describes tracer gas uniformity and bias measurements made in the exhaust air discharge of the Hot Fuel Examination Facility at Idaho National Laboratory. The measurements were a follow-up on earlier measurements which indicated a lack of mixing of the two ventilation streams being discharged via a common stack. The lack of mixing is detrimental to the accuracy of air emission measurements. The lack of mixing was confirmed in these new measurements. The air sampling probe was found to be out of alignment and that was corrected. The suspected sampling bias in the air sample stream was disproved.

  13. High-quality genomic DNA extraction from formalin-fixed and paraffin-embedded samples deparaffinized using mineral oil

    OpenAIRE

    Lin, Jianghai; Kennedy, Stephen H.; Svarovsky, Therese; Rogers, Jeffrey; Kemnitz, Joseph W.; Xu, Anlong; Zondervan, Krina T

    2009-01-01

    Extracting DNA from formalin-fixed and paraffin-embedded (FFPE) tissue remains a challenge, despite numerous attempts to develop a more effective method. Polymerase chain reaction (PCR) success rates with DNA extracted using current methods remain low. We extracted DNA from 140 long-term archived FFPE samples using a simple but effective deparaffinization method, removing the wax with mineral oil, and a commercially available DNA extraction kit. DNA quality was subsequently tested in a genoty...

  14. Passive airborne dust sampling with the electrostatic dustfall collector: optimization of storage and extraction procedures for endotoxin and glucan measurement.

    Science.gov (United States)

    Noss, Ilka; Doekes, Gert; Sander, Ingrid; Heederik, Dick J J; Thorne, Peter S; Wouters, Inge M

    2010-08-01

    We recently introduced a passive dust sampling method for airborne endotoxin and glucan exposure assessment-the electrostatic dustfall collector (EDC). In this study, we assessed the effects of different storage and extraction procedures on measured endotoxin and glucan levels, using 12 parallel EDC samples from 10 low exposed indoor environments. Additionally, we compared 2- and 4-week sampling with the prospect of reaching higher dust yields. Endotoxin concentrations were highest after extraction with pyrogen-free water (pf water) + Tween. Phosphate-buffered saline (PBS)-Tween yielded significantly (44%) lower levels, and practically no endotoxin was detected after extraction in pf water without Tween. Glucan levels were highest after extraction in PBS-Tween at 120 degrees C, whereas extracts made in NaOH at room temperature or 120 degrees C were completely negative. Direct extraction from the EDC cloth or sequential extraction after a preceding endotoxin extraction yielded comparable glucan levels. Sample storage at different temperatures before extraction did not affect endotoxin and glucan concentrations. Doubling the sampling duration yielded similar endotoxin and only 50% higher glucan levels. In conclusion, of the tested variables, the extraction medium was the predominant factor affecting endotoxin and glucan yields. PMID:20354054

  15. Rapid dioxin analysis using accelerated solvent extraction (ASE), multi-column sample cleanup and Rtx-Dioxin2 gas chromatography column

    Energy Technology Data Exchange (ETDEWEB)

    Robinson, C.; Blow, P. [Australian Laboratory Services, Brisbane (Australia); Dorman, F. [Restek Corporation, Bellefonte, PA (United States)

    2004-09-15

    One of the main aims of many dioxin analysis laboratories is to reduce sample turnaround times to the absolute minimum. Often shorter times between sample receipt and reporting of results can attract a premium price for the analysis. It is generally accepted that the GC-MS portion of dioxin/PCB analysis is not the rate determining step in the overall scheme. Therefore, sample extraction and clean up is the obvious step to investigate for time-saving purposes. The use of accelerated solvent extraction (ASE) and multi column cleanup has been investigated for soil, sediment, air sampling media (XAD-2 resin) and fly-ash samples. For water samples the ASE step is replaced with a liquid/liquid separatory funnel extraction. Environmental analyses regularly require the use of two GC-MS runs to produce dioxin results that may be relied upon. The use of the classical 5MS type column coupled with the more polar 2331 type to produce final results is typical. The innovative capillary GC column, Rtx-Dioxin2, has offered the possibility of performing a dioxin analysis in a single GC-MS run. The analysis of the WHO-12 PCB (PCBs 77, 81, 105, 114, 118, 123, 126, 156, 157, 167, 169 and 189) congeners has also been investigated using this column.

  16. Utilizing a sequential injection system furnished with an extraction microcolumn as a novel approach for executing sequential extractions of metal species in solid samples

    DEFF Research Database (Denmark)

    Chomchoei, R.; Hansen, Elo Harald; Shiowatana, J.

    2007-01-01

    This communication presents a novel approach to perform sequential extraction of elements in solid samples by using a sequential injection (SI) system incorporating a specially designed extraction microcolumn. Based on the operation of the syringe pump, different modes of extraction are potentially...... feasible, uni-directional and bi-directional flow schemes being used herein. A three-step sequential extraction scheme, using conventionally adopted extractants, was used to evaluate the system by determining Ca, Fe, Mn, Cu, Zn in a soil certified reference material (NIST, SRM 2710). It is demonstrated...... ranging from 50 to 100 mul sec-1 show any effect on the extractability of the metals studied. With uni-directional and bi-directional flows the extractable amounts of metals are, with the exception of Mn, not different from those obtained in conventional procedures, but the saving in operation time is...

  17. Occupational exposure to complex mixtures of volatile organic compounds in ambient air: desorption from activated charcoal using accelerated solvent extraction can replace carbon disulfide?

    Science.gov (United States)

    Fabrizi, Giovanni; Fioretti, Marzia; Rocca, Lucia Mainero

    2013-01-01

    A desorption study of 57 volatile organic compounds (VOCs) has been conducted by use of accelerated solvent extraction (ASE) and gas chromatography-mass spectrometry. Different solvents were tested to extract activated charcoal tubes with the objective of replacing carbon disulfide, used in official methods, because of its highly toxic health and environmental effects. Extraction conditions, for example temperature and number of cycles, were investigated and optimized. The definitive extraction procedure selected was use of acetone at 150 °C and two consecutive extraction cycles at a pressure of 1,500 psi. Considering a sample volume of 0.005 Nm(3), corresponding to a sampling time of 8 h at a flow rate of 0.01 L min(-1), the method was validated over the concentration range 65-26,300 μg Nm(-3). The lowest limit of quantification was 6 μg Nm(-3), and recovery for the 93 % of analytes ranged from 65 to 102 %. For most of the compounds, relative standard deviations were less than 15 % for inter and intra-day precision. Uncertainty of measurement was also determined: the relative expanded uncertainty was always below 29.6 %, except for dichlorodifluoromethane. This work shows that use of friendlier solvent, for example acetone, coupled with use of ASE, can replace use of CS(2) for chemical removal of VOCs from activated charcoal. ASE has several advantages over traditional solvent-extraction methods, including shorter extraction time, minimum sample manipulation, high reproducibility, and less extraction discrimination. No loss of sensitivity occurs and there is also a salutary effect on bench workers' health and on the smell of laboratory air. PMID:22968683

  18. Estimation of uranium isotope in urine samples using extraction chromatography resin

    International Nuclear Information System (INIS)

    Internal exposure monitoring for alpha emitting radionuclides is carried out by bioassay samples analysis. For occupational radiation workers who handle uranium in reprocessing or fuel fabrication facilities, there exist a possibility of internal exposure and urine assay is the preferred method for monitoring such exposure. Separation of uranium is carried out by extraction chromatography using diamyl amyl phosphonate (U/TEVA) resin. This resin contains diamyl amyl phosphonate extractant supported on inert Amberlite XAD-7 (an acrylic ester) resin. The electrodeposited samples are counted using octet alpha spectrometry. The analysis time involved from sample loading to stripping is 2 h compared with the 3.5 h involved in conventional ion exchange method. The radiochemical yield was found in the range of 69-91%. Minimum detectable activity for uranium estimation for 3,60,000 s counting time at an average percentage recovery of 82 ± 8 works out to 0.21 mBq/d. The technique gives good and consistent radiochemical yield of 82% on repeated use of the chromatographic column when compared with ion exchange technique. Analysis time involved from sample loading to stripping using UTEVA is 2 h compared with the time involved of 3.5 h by the conventional ion exchange method. (author)

  19. Solid phase extraction for determination of 90Sr in water sample

    International Nuclear Information System (INIS)

    We studied the use of an extraction chromatography for determination of 90Sr in samples of contaminated water. The aim of the thesis was to compare selected products from the point of view of the strontium yields and time needed. Three commercial products: 3M Empore Strontium Rad Disk, AnaLig, Sr-Resin and two classical methods: liquid-liquid extraction with tributylphosphate and carbonate co-precipitation (to eliminate interferers) were used for separation of 90Sr. The water sample was used in radiochemical analysis for determination volume activity of 90Sr. A radiochemical strontium yield was traced by using radionuclide 85Sr. Samples were counted over a two week period to monitor the ingrowth of 90Y on TRI CARB LSC counter. Samples were measured using an HPGe detector to find out 85Sr recoveries at 514 keV line and they were counted directly by Cherenkov counting after the growth of 90Y using TriCarb LSC counter after a two- week period (author)

  20. Alternative sorptive extraction method for gas chromatography determination of halogenated anisoles in water and wine samples

    Energy Technology Data Exchange (ETDEWEB)

    Montes, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain); Rodriguez, I. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain)], E-mail: qnisaac@usc.es; Rubi, E.; Bollain, M.H.; Cela, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain)

    2007-09-05

    An alternative sorptive microextraction method for the determination of five halogenated anisoles in water and wine matrices is proposed. Analytes were concentrated in an inexpensive and disposable piece of bulk polydimethylsiloxane (PDMS), desorbed with a small volume of organic solvent, and determined by gas chromatography with electron-capture detection (GC-ECD) or tandem mass spectrometry (GC-MS/MS). The influence of several factors on the efficiency of extraction and desorption steps was investigated in detail and the observed behaviour justified on the basis of thermodynamics and kinetics of the solid-phase microextraction technique. Under optimised conditions, analytes were first extracted in the headspace (HS) mode, at room temperature, for 2.5 h and then desorbed with 1 mL of n-pentane. This extract was further evaporated to 50 {mu}L. The overall extraction yield of the procedure ranged from 40 to 55% and the limits of quantification remained between 0.5 and 20 ng L{sup -1}, depending on the compound considered and the detection technique. Precision and linearity of the method were excellent for all species with both GC-ECD and GC-MS/MS detection. Matrix effects were evaluated with different water and wine samples; moreover, the suitability of the PDMS sorbent for storage of analytes, under different conditions, was demonstrated.

  1. Alternative sorptive extraction method for gas chromatography determination of halogenated anisoles in water and wine samples

    International Nuclear Information System (INIS)

    An alternative sorptive microextraction method for the determination of five halogenated anisoles in water and wine matrices is proposed. Analytes were concentrated in an inexpensive and disposable piece of bulk polydimethylsiloxane (PDMS), desorbed with a small volume of organic solvent, and determined by gas chromatography with electron-capture detection (GC-ECD) or tandem mass spectrometry (GC-MS/MS). The influence of several factors on the efficiency of extraction and desorption steps was investigated in detail and the observed behaviour justified on the basis of thermodynamics and kinetics of the solid-phase microextraction technique. Under optimised conditions, analytes were first extracted in the headspace (HS) mode, at room temperature, for 2.5 h and then desorbed with 1 mL of n-pentane. This extract was further evaporated to 50 μL. The overall extraction yield of the procedure ranged from 40 to 55% and the limits of quantification remained between 0.5 and 20 ng L-1, depending on the compound considered and the detection technique. Precision and linearity of the method were excellent for all species with both GC-ECD and GC-MS/MS detection. Matrix effects were evaluated with different water and wine samples; moreover, the suitability of the PDMS sorbent for storage of analytes, under different conditions, was demonstrated

  2. Accelerating sample preparation through enzyme-assisted microfiltration of Salmonella in chicken extract.

    Science.gov (United States)

    Vibbert, Hunter B; Ku, Seockmo; Li, Xuan; Liu, Xingya; Ximenes, Eduardo; Kreke, Thomas; Ladisch, Michael R; Deering, Amanda J; Gehring, Andrew G

    2015-01-01

    Microfiltration of chicken extracts has the potential to significantly decrease the time required to detect Salmonella, as long as the extract can be efficiently filtered and the pathogenic microorganisms kept in a viable state during this process. We present conditions that enable microfiltration by adding endopeptidase from Bacillus amyloliquefaciens to chicken extracts or chicken rinse, prior to microfiltration with fluid flow on both retentate and permeate sides of 0.2 μm cutoff polysulfone and polyethersulfone hollow fiber membranes. After treatment with this protease, the distribution of micron, submicron, and nanometer particles in chicken extracts changes so that the size of the remaining particles corresponds to 0.4-1 μm. Together with alteration of dissolved proteins, this change helps to explain how membrane fouling might be minimized because the potential foulants are significantly smaller or larger than the membrane pore size. At the same time, we found that the presence of protein protects Salmonella from protease action, thus maintaining cell viability. Concentration and recovery of 1-10 CFU Salmonella/mL from 400 mL chicken rinse is possible in less than 4 h, with the microfiltration step requiring less than 25 min at fluxes of 0.028-0.32 mL/cm(2) min. The entire procedure-from sample processing to detection by polymerase chain reaction-is completed in 8 h. PMID:26400739

  3. Urban air quality assessment using monitoring data of fractionized aerosol samples, chemometrics and meteorological conditions.

    Science.gov (United States)

    Yotova, Galina I; Tsitouridou, Roxani; Tsakovski, Stefan L; Simeonov, Vasil D

    2016-06-01

    The present article deals with assessment of urban air by using monitoring data for 10 different aerosol fractions (0.015-16 μm) collected at a typical urban site in City of Thessaloniki, Greece. The data set was subject to multivariate statistical analysis (cluster analysis and principal components analysis) and, additionally, to HYSPLIT back trajectory modeling in order to assess in a better way the impact of the weather conditions on the pollution sources identified. A specific element of the study is the effort to clarify the role of outliers in the data set. The reason for the appearance of outliers is strongly related to the atmospheric condition on the particular sampling days leading to enhanced concentration of pollutants (secondary emissions, sea sprays, road and soil dust, combustion processes) especially for ultra fine and coarse particles. It is also shown that three major sources affect the urban air quality of the location studied-sea sprays, mineral dust and anthropogenic influences (agricultural activity, combustion processes, and industrial sources). The level of impact is related to certain extent to the aerosol fraction size. The assessment of the meteorological conditions leads to defining of four downwind patterns affecting the air quality (Pelagic, Western and Central Europe, Eastern and Northeastern Europe and Africa and Southern Europe). Thus, the present study offers a complete urban air assessment taking into account the weather conditions, pollution sources and aerosol fractioning. PMID:26942452

  4. Sample Results From The Extraction, Scrub, And Strip Test For The Blended NGS Solvent

    Energy Technology Data Exchange (ETDEWEB)

    Washington, A. L. II; Peters, T. B.

    2014-03-03

    This report summarizes the results of the extraction, scrub, and strip testing for the September 2013 sampling of the Next Generation Solvent (NGS) Blended solvent from the Modular Caustic Side-Solvent Extraction Unit (MCU) Solvent Hold Tank. MCU is in the process of transitioning from the BOBCalixC6 solvent to the NGS Blend solvent. As part of that transition, MCU has intentionally created a blended solvent to be processed using the Salt Batch program. This sample represents the first sample received from that blended solvent. There were two ESS tests performed where NGS blended solvent performance was assessed using either the Tank 21 material utilized in the Salt Batch 7 analyses or a simulant waste material used in the V-5/V-10 contactor testing. This report tabulates the temperature corrected cesium distribution, or DCs values, step recovery percentage, and actual temperatures recorded during the experiment. This report also identifies the sample receipt date, preparation method, and analysis performed in the accumulation of the listed values. The calculated extraction DCs values using the Tank 21H material and simulant are 59.4 and 53.8, respectively. The DCs values for two scrub and three strip processes for the Tank 21 material are 4.58, 2.91, 0.00184, 0.0252, and 0.00575, respectively. The D-values for two scrub and three strip processes for the simulant are 3.47, 2.18, 0.00468, 0.00057, and 0.00572, respectively. These values are similar to previous measurements of Salt Batch 7 feed with lab-prepared blended solvent. These numbers are considered compatible to allow simulant testing to be completed in place of actual waste due to the limited availability of feed material.

  5. Sample Results From The Extraction, Scrub, And Strip Test For The Blended NGS Solvent

    International Nuclear Information System (INIS)

    This report summarizes the results of the extraction, scrub, and strip testing for the September 2013 sampling of the Next Generation Solvent (NGS) Blended solvent from the Modular Caustic Side-Solvent Extraction Unit (MCU) Solvent Hold Tank. MCU is in the process of transitioning from the BOBCalixC6 solvent to the NGS Blend solvent. As part of that transition, MCU has intentionally created a blended solvent to be processed using the Salt Batch program. This sample represents the first sample received from that blended solvent. There were two ESS tests performed where NGS blended solvent performance was assessed using either the Tank 21 material utilized in the Salt Batch 7 analyses or a simulant waste material used in the V-5/V-10 contactor testing. This report tabulates the temperature corrected cesium distribution, or DCs values, step recovery percentage, and actual temperatures recorded during the experiment. This report also identifies the sample receipt date, preparation method, and analysis performed in the accumulation of the listed values. The calculated extraction DCs values using the Tank 21H material and simulant are 59.4 and 53.8, respectively. The DCs values for two scrub and three strip processes for the Tank 21 material are 4.58, 2.91, 0.00184, 0.0252, and 0.00575, respectively. The D-values for two scrub and three strip processes for the simulant are 3.47, 2.18, 0.00468, 0.00057, and 0.00572, respectively. These values are similar to previous measurements of Salt Batch 7 feed with lab-prepared blended solvent. These numbers are considered compatible to allow simulant testing to be completed in place of actual waste due to the limited availability of feed material

  6. The Survey of Microbial Quality of the Dry Sample, Extract and Brewing of some Medicinal Plants

    Directory of Open Access Journals (Sweden)

    Razieh VALIASILL

    2014-12-01

    Full Text Available Medicinal plants may be exposed to a wide range of microbial contamination during pre- and post- harvest stages and they can present high microbial counts. In this study, the microbial quality of 44 samples of dry herbs namely: mint (Menthaspp., lemon balm (Melissa officinalis, summer savory (Satureja hortensis, zataria (Zataria multiflora, Indian valerian (Valeriana wallichii, their brewing and extracts were analyzed. Total count using plate count agar medium (PCA, coliform count by Violet Red Bile Agar (VRBL, Enterobacteriacea by Violet Red Bile Glucose (VRBG were evaluated. Medium Baird-Parker agar (BP medium and Tryptone Bile X-Gluc (TBX medium were used for the isolation and enumeration of Staphylococcus aurous and E. coli spp. respectively. Furthermore, Xylose Lysine Deoxycholate agar medium (XLD and Bismuth Sulfite Agar medium(BSA were used for detection of Salmonella spp. Fungal and mold contamination was assessed using yeast extract glucose chloramphenicol agar. The results showed that the contamination of the samples with total count (100% and Enterobacteriaceae (85%, total coliform (83%, mold and yeast (98% and E. coli ssp. (2.27 were detected, including in the study samples the absence of pathogenic bacteria like Staphylococcus aurous, Salmonella spp. Moreover, the extract had a lower microbial load in comparison to dry herb samples. Also, the lowest and the highest of contamination rates were observed for Indian valerian and zataria, respectively. According to the results, there is a need to control the environmental conditions and improve hygiene in the production process; even more, it is recommended to choose a suitable decontamination method for disinfection during packing medicinal plants and during post-packing manipulation and transport.

  7. Comparison of two sequential extraction protocols for fractionation of natural radionuclides in soil samples

    International Nuclear Information System (INIS)

    Revised BCR (Bureau Communautaire de Reference) and the Schultz modification of Tessier's sequential extraction protocols are compared for fractionation of uranium, thorium and radium in soil samples. Six soil samples were collected near to the uranium mill tailings waste pile and some of them had enhanced levels of natural radionuclides. The samples were processed by both protocols and the radionuclide content assayed by alpha spectrometric determination. The analysis revealed that results obtained by the two protocols are not fully comparable as data are mostly protocol- and element-dependent. Nevertheless, general conclusions about potential source of the particular radionuclide, which could be drawn from the specific study carried out, are mostly similar for both protocols. (orig.)

  8. Extraction, interpretation and validation of information for comparing samples in metabolic LC/MS data sets.

    Science.gov (United States)

    Jonsson, Par; Bruce, Stephen J; Moritz, Thomas; Trygg, Johan; Sjöström, Michael; Plumb, Robert; Granger, Jennifer; Maibaum, Elaine; Nicholson, Jeremy K; Holmes, Elaine; Antti, Henrik

    2005-05-01

    LC/MS is an analytical technique that, due to its high sensitivity, has become increasingly popular for the generation of metabolic signatures in biological samples and for the building of metabolic data bases. However, to be able to create robust and interpretable (transparent) multivariate models for the comparison of many samples, the data must fulfil certain specific criteria: (i) that each sample is characterized by the same number of variables, (ii) that each of these variables is represented across all observations, and (iii) that a variable in one sample has the same biological meaning or represents the same metabolite in all other samples. In addition, the obtained models must have the ability to make predictions of, e.g. related and independent samples characterized accordingly to the model samples. This method involves the construction of a representative data set, including automatic peak detection, alignment, setting of retention time windows, summing in the chromatographic dimension and data compression by means of alternating regression, where the relevant metabolic variation is retained for further modelling using multivariate analysis. This approach has the advantage of allowing the comparison of large numbers of samples based on their LC/MS metabolic profiles, but also of creating a means for the interpretation of the investigated biological system. This includes finding relevant systematic patterns among samples, identifying influential variables, verifying the findings in the raw data, and finally using the models for predictions. The presented strategy was here applied to a population study using urine samples from two cohorts, Shanxi (People's Republic of China) and Honolulu (USA). The results showed that the evaluation of the extracted information data using partial least square discriminant analysis (PLS-DA) provided a robust, predictive and transparent model for the metabolic differences between the two populations. The presented findings

  9. Atmospheric trace gas measurements with a new clean air sampling system

    International Nuclear Information System (INIS)

    The development of a new clean air sampling system for the Department of Energy's WB-57F aircraft has allowed the analysis of CCl3F (Fluorocarbon-11), CCl2F2 (Fluorocarbon-12), CHClF2 (Fluorocarbon-22), C2Cl3F3 (Fluorocarbon-113), CH4, CO, CO2, N2O, CH3Cl, CCl4, CH3CCl3, OCS and SF6 in tropospheric and stratospheric samples. Samples collected during the interception of the plume from the eruption of Mount St. Helens indicate that OCS was injected into the stratosphere during the eruption. A large CO2 gradient was found at 19.2 km on this flight

  10. Size selective isocyanate aerosols personal air sampling using porous plastic foams

    International Nuclear Information System (INIS)

    As part of a European project (SMT4-CT96-2137), various European institutions specialized in occupational hygiene (BGIA, HSL, IOM, INRS, IST, Ambiente e Lavoro) have established a program of scientific collaboration to develop one or more prototypes of European personal samplers for the collection of simultaneous three dust fractions: inhalable, thoracic and respirable. These samplers based on existing sampling heads (IOM, GSP and cassettes) use Polyurethane Plastic Foam (PUF) according to their porosity to support sampling and separator size of the particles. In this study, the authors present an original application of size selective personal air sampling using chemical impregnated PUF to perform isocyanate aerosols capturing and derivatizing in industrial spray-painting shops.

  11. Effect of sample digestion, air filter contamination, and post-adsorption on the analysis of trace elements in air particulate matter

    International Nuclear Information System (INIS)

    Inductively coupled plasma atomic emission spectrometry and inductively coupled plasma MS are the major analytical tools for trace elements in environmental matrices, however, the underestimate of certain trace elements in analysis of air particulate matter by these two techniques has long been observed. This has been attributed to incomplete sample digestion. Here, we demonstrate that the combined effects of sample digestion, air filter impurities, and post-adsorption of the analytes contribute to the interference of the analysis. Particular attention should be paid to post-adsorption of analytes onto air filters after acid digestion. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  12. Remote control of sample insertion and extraction to/from reactor rotary specimen rack

    International Nuclear Information System (INIS)

    Automation of sample insertion and extraction to/from reactor irradiation facilities and radiation dose reduction to reactor personnel were the aim of a multi-annual activity program at the L.E.N.A. TRIGA Mark II reactor of the University of Pavia. At the two previous European TRIGA Users Conferences, held in Vienna and in Heidelberg, in 1988 and 1990, respectively, the new automated storage pits for irradiated samples and a 'robot' type machine devoted to sample insertion and extraction, were presented and described. However the operation of the rotatory specimen rack (Lazy Susan), i.e. rotation switching on and position selection, had to be carried out by reactor personnel on the reactor top, an area where the maximum allowable radiation dose is quite often overcome. The present paper describes the last step in our automation program, i.e. the remote control of Lazy Susan operation and the coupling of the robot's performance and Lazy Susan rotation. Also it is stressed that in the present case all work from device design to construction has been carried out by the personnel of the electronic group of L.E.N.A. plant. (authors)

  13. New developments in the extraction and determination of parabens in cosmetics and environmental samples. A review

    International Nuclear Information System (INIS)

    Highlights: • The analysis of parabens in cosmetics and environmental samples is reviewed. • Literature in this field from 1980 to 2003 is briefly discussed. • Determination and extraction methods in the last decade are discussed in-depth. - Abstract: Parabens are a family of synthetic esters of p-hydroxibenzoic acid widely used as preservatives in cosmetics and health-care products, among other daily-use commodities. Recently, their potential endocrine disrupting effects have raised concerns about their safety and their potential effects as emerging pollutants, leading to the regulation of the presence of parabens in commercial products by national and trans-national organizations. Also, this has led to an interest in developing sensible and reliable methods for their determination in environmental samples, cosmetics and health-care products. This paper is a comprehensive up-to-date review of the literature concerning the determination of parabens in environmental samples and cosmetic and health-care products. A brief revision of the literature concerning the traditional determination of parabens (1980–2003) is included, followed by an in-depth revision of the recent developments in both measurement and extraction methods for parabens in the last years (2003–2013). Finally, possible future perspectives in this field are proposed

  14. New developments in the extraction and determination of parabens in cosmetics and environmental samples. A review

    Energy Technology Data Exchange (ETDEWEB)

    Ocaña-González, Juan Antonio; Villar-Navarro, Mercedes [Department of Analytical Chemistry, Faculty of Chemistry, Universidad de Sevilla, c/Prof. García González, s/n. 41012 Seville (Spain); Ramos-Payán, María [Department of Analytical Chemistry, Faculty of Chemistry, Universidad de Sevilla, c/Prof. García González, s/n. 41012 Seville (Spain); Department of Analytical Chemistry, Lineberguer Cancer Center, The University of North Carolina at Chapel Hill, NC (United States); Fernández-Torres, Rut [Department of Analytical Chemistry, Faculty of Chemistry, Universidad de Sevilla, c/Prof. García González, s/n. 41012 Seville (Spain); Research Centre of Health and Environment (CYSMA), University of Huelva (Spain); Bello-López, Miguel Angel, E-mail: mabello@us.es [Department of Analytical Chemistry, Faculty of Chemistry, Universidad de Sevilla, c/Prof. García González, s/n. 41012 Seville (Spain)

    2015-02-09

    Highlights: • The analysis of parabens in cosmetics and environmental samples is reviewed. • Literature in this field from 1980 to 2003 is briefly discussed. • Determination and extraction methods in the last decade are discussed in-depth. - Abstract: Parabens are a family of synthetic esters of p-hydroxibenzoic acid widely used as preservatives in cosmetics and health-care products, among other daily-use commodities. Recently, their potential endocrine disrupting effects have raised concerns about their safety and their potential effects as emerging pollutants, leading to the regulation of the presence of parabens in commercial products by national and trans-national organizations. Also, this has led to an interest in developing sensible and reliable methods for their determination in environmental samples, cosmetics and health-care products. This paper is a comprehensive up-to-date review of the literature concerning the determination of parabens in environmental samples and cosmetic and health-care products. A brief revision of the literature concerning the traditional determination of parabens (1980–2003) is included, followed by an in-depth revision of the recent developments in both measurement and extraction methods for parabens in the last years (2003–2013). Finally, possible future perspectives in this field are proposed.

  15. Accelerated solvent extraction for gas chromatographic analysis of nicotine and cotinine in meconium samples.

    Science.gov (United States)

    Sant'anna, Simone Gomes; Oliveira, Carolina Dizioli Rodrigues; Diniz, Edna Maria de Albuquerque; Yonamine, Mauricio

    2012-01-01

    Adverse effects associated with smoking during pregnancy are well documented. Although self-report surveys on drug consumption during pregnancy have been improved with new interviewing techniques, underreporting is still a concern. Therefore, a series of biological markers and specimens to diagnose fetal exposure to tobacco have been studied. In the present study, an analytical method was developed to detect nicotine and cotinine (the main nicotine metabolite) in meconium samples. Accelerated solvent extraction (ASE) followed by solid-phase extraction (SPE) were used as sample preparation techniques. The analytes were detected by gas-chromatography with nitrogen-phosphorus detection. The limits of detection were 3.0 and 30 ng/g for cotinine and nicotine, respectively. The method showed good linearity (r(2) > 0.98) in the concentration range studied (LOQ-500 ng/g). The intraday precision, given by the RSD of the method, was less than 15% for cotinine and nicotine. The method proved to be fast, practical, and sensitive. Smaller volumes of organic solvents are necessary compared to other chromatographic methods published in the scientific literature. This is the first report in which ASE was used as sample preparation technique in methods to detect xenobiotics in meconium. PMID:22290748

  16. Electromembrane extraction and spectrophotometric determination of As(V) in water samples.

    Science.gov (United States)

    Kamyabi, Mohammad Ali; Aghaei, Ali

    2016-12-01

    In this study, for the first time electromembrane extraction (EME) was used as a highly efficient sample pre-treatment method for the UV-VIS spectrophotometric determination of As(V) in water samples. The influences of experimental parameters during EME were investigated and optimized using one-variable-at-a-time methodology as follows: organic solvent: 1-octanol+2.5% (V/V) di-(2-ethylhexyl) phosphate, applied voltage: 70V, extraction time: 15min, pH of acceptor: 13, stirring rate: 750rpm. The method allowed the determination of As(V) in the range of 5-300ngmL(-1). The relative standard deviation was found to be within the range of 3.4-7.6%. The limit of detection, corresponding to a signal to noise ratio of three, was 1.5ngmL(-1). The proposed method was finally applied to the determination of As(V) in water samples and relative recoveries ranging from 95 to 102% were obtained. PMID:27374507

  17. Gas chromatographic determination of cholesterol from food samples using extraction/saponification method

    International Nuclear Information System (INIS)

    A simple and fast one-step extraction/saponification with Na/OH/KOH (Ethanolic, Sodium Hydroxide/Potassium Hydroxide was compared and validated for determination of cholesterol from locally available 10 edible oil and egg samples. The importance of the use of edible oils and eggs in routine diet is unquestionable, but presence of cholesterol is considered as a risk factor for coronary heart disease and hypertension. The lowering of cholesterol level in order to reduce the risk is widely accepted. The cholesterol in the edible oil and eggs was determined by gas chromatography, through elution from the column (2x3 mm i.d) packed with 3% OV-I01, on Chromosorb G/'NAW 80-100 mesh size at 250-300C with programmed heating rate of 3 degree C/min. Nitrogen gas flow rate was 40 ml/min. The cholesterol samples were run under the conditions after selective extraction in diethyl ether. The calibration was linear within 50-500 IJg/ml concentration range. The amount of cholesterol detected were from 12.92-18.05 mg/g in edible oil and 117.54-143.42 mg/g in egg samples with RSD 1.3-2.7%. (author)

  18. Radiological background levels found in glass fiber filters used for low-level environmental surveillance air sampling

    International Nuclear Information System (INIS)

    Environmental surveillance monitoring of low-level radioactive particles in air requires a thorough understanding of low-level techniques and air sample collection media. High-volume air sampling for radioactive particles around Lawrence Livermore National Laboratory (LLNL) currently employs glass-fiber filters that are analyzed for gross alpha and gross beta activity and for specific isotopes. This study was conducted to determine the activities of radionuclides contained in blank glass-fiber filters. Data from this study provided a partial explanation of differences between current reported concentrations of radionuclides in air and those reported historically when cellulose filters were used in the LLNL monitoring effort. (author)

  19. Radiological background levels found on glass fiber filters used for low-level environmental surveillance air sampling

    International Nuclear Information System (INIS)

    Environmental surveillance of low-level radioactive particles in air requires a thorough understanding of low-level techniques and air sample collection media. High-volume air sampling for radioactive particles around Lawrence Livermore National Laboratory (LLNL) employs glass-fiber filters that are analyzed for gross alpha and gross beta activity and for specific isotopes. This study was conducted to determine the activities of radionuclides contained in blank glass-fiber filters. Data from this study provided a partial explanation of differences between current reported concentrations of radionuclides in air and those reported historically when cellulose filters were used in the LLNL monitoring effort

  20. Zirconium(IV) functionalized magnetic nanocomposites for extraction of organophosphorus pesticides from environmental water samples.

    Science.gov (United States)

    Jiang, Li; Huang, Tengjun; Feng, Shun; Wang, Jide

    2016-07-22

    The widespread use of organophosphate pesticides (OPPs) in agriculture leads to residue accumulation in the environment which is dangerous to human health and disrupts the ecological balance. In this work, one nanocomposite immobilized zirconium (Zr, IV) was prepared and used as the affinity probes to quickly and selectively extract organophosphorus pesticides (OPPs) from water samples. The Fe3O4-ethylenediamine tetraacetic acid (EDTA)@Zr(IV) nanocomposites (NPs) were prepared by simply mixing Zr(IV) ions with Fe3O4-EDTA NPs synthesized by one-pot chemical co-precipitation method. The immobilized Zr(IV) ions were further utilized to capture OPPs based on their high affinity for the phosphate moiety in OPPs. Coupled with GC-MS, four OPPs were used as models to demonstrate the feasibility of this approach. Under the optimum conditions, the limits of detection for target OPPs were in the range of 0.10-10.30ngmL(-1) with relative standard deviations (RSDs) of 0.61-4.40% (n=3), respectively. The linear ranges were over three orders of magnitudes (correlation coefficients, R(2)>0.9995). The Fe3O4-EDTA@Zr(IV) NPs were successfully applied to extract OPPs samples with recoveries of 86.95-112.60% and RSDs of 1.20-10.42% (n=3) from two spiked real water. By the proposed method, the matrix interference could be effectively eliminated. We hope our finding can provide a promising alternative for the fast extraction of OPPs from complex real samples. PMID:27328881

  1. Detection of fissile materials in smeared or air filter samples by fission track registration technique

    International Nuclear Information System (INIS)

    The fission track registration technique was investigated for the detection of fissile materials in smeared and air filter samples. The filters taken directly from the nuclear facilities were applied onto the surface of Lexan plate for neutron irradiation in the HANARO research reactor. The fission tracks in the Lexan plate were observed under optical microscope. The optimal conditions for the neutron irradiation and chemical etching were established, where the total neutron irradiation dose was 300x1013n/cm2 and the chemical etching was done in 6.25 M-NaOH solution for 10 min., respectively

  2. Determination of Sr-90 in environmental samples using solid phase extraction disk

    International Nuclear Information System (INIS)

    A method is described for determination of Sr-90 in environmental samples using solid phase extraction disk (Empore TM Strontium Rad Disk) and GM counter. To determine the optimum condition for capacity of Empore TM Strontium Rad Disk, its characterization studies such as the effects Sr content, acidity (molarity) of acids, presence of Ca2+ and other major ions (Na+, Mg2+ etc), influence of interference (Pb and Bi) and others were carried out. An optimized the using of Empore TM Strontium Rad Disk for determination of Sr-90 was validated by application to environmental samples. Quantitative recoveries above 95%for Sr (stable) were recorded in 6M HCl condition. Typical environmental samples may contain an assortment of anionic and cationic species, but in general, Empore TM Strontium Rad Disk has enough capacity to effectively separate Sr for wide variety of aqueous solutions. Sr recovery in a matrix-free or the content of matrix less than 300 mg/sample is typically greater than 99% is reported in this research work. In particular, sample, which may contain interference such as Pb and Bi would require an addition separation step before processing to ensure an accurate measurement of Sr. In this research work, radiotracer 85Sr was used to monitor the behavior of Sr and calculation its recovery. For analytical methods that can count Y-90, the Sr-90 activity/concentration in environmental sample was calculated. The concentration of Sr-90 in ash sample (Quality Controled Sample) of 276 ± 18 Bq/kg ash was determined from Y-90 activity. The relative percent difference of 1.1% was achievable for Empore TM Sr-Rad Disk methods when compared to the conventional method (fumed-HNO3 method) - 279 ± 11 Bq/kg ash. (Author)

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

    Science.gov (United States)

    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. PMID:21570440

  4. Extraction method enhancement techniques for the analysis of PCDDS and PCDFS in meat sample

    Energy Technology Data Exchange (ETDEWEB)

    Jeong, Tae-Uk [Gyeonsang National Univ., Jinju (Korea). Division of Applied Life Science]|[National Veterinary Research and Quarantine Service (Korea). Busan Regional Office; Kwon, Jin-Wook [National Veterinary Research and Quarantine Service (Korea). Anyang city

    2004-09-15

    Dioxins are the most concerned persistent organic pollutants(POPs) to human beings and being fat soluble tend to accumulate in higher animals including humans. Dioxins has 75 congeners of PCDD and 135 congeners of PCDF, but generally only 7 congeners of PCDD and 10 congeners of PCDF are analyzed because of their toxicity, stability and so on. Since dioxins contamination is regarded as a global issue, a large amount of samples have been analyzed, and various methods for measuring dioxins have been developed and improved. Dioxins analysis needs very complicated analytical procedure including extraction, cleanup and instrument analysis. Because analytical procedure is very complicated and needs many steps, conventional analytical procedure are very time consuming and use large volumes of solvents. So current methods are time consuming and very expensive. In this study, speedy and cost reducing methods without reducing recovery and stability should be focused. So to present the new extraction method to simplify and stabilize of extraction method, the recovery and stability of 7 congeners of PCDD and 10 congeners of PCDF using soxhlet, forced convection dry oven and microwave oven were compared.

  5. Determination of Technetium-99 in Environmental Samples by Solvent Extraction at Controlled Valence

    DEFF Research Database (Denmark)

    Chen, Q.J.; Aarkrog, A.; Dahlgaard, H.;

    1989-01-01

    Distribution coefficients of technetium and ruthenium are determined under different conditions with CCl4, cyclohexanone, and 5% tri-isooctylamine (TIOA)/xylene. A method for analyzing 99Tc in environmental samples has been developed by solvent extraction in which the valences of technetium and...... subsequently separated by solvent extraction with cyclohexanone and 5% TIOA/xylene. The decontamination of the procedure is 1.35 .cntdot. 105 for 103Ru and 1.66 .cntdot. 105 for 110mAg. The chemical yield of technetium-99 is 55%....... ruthenium are controlled with H2O2 and NaClO. Technetium and ruthenium which are oxidized to TcO4- and RuO4- by NaClO are separated by extraction with CCl4 at pH 4. The RuO4- is reduced to low valence and technetium is kept in the TcO4- state with H2O2. Technetium, ruthenium, and other nuclides are...

  6. An Improved Method for High Quality Metagenomics DNA Extraction from Human and Environmental Samples

    Science.gov (United States)

    Bag, Satyabrata; Saha, Bipasa; Mehta, Ojasvi; Anbumani, D.; Kumar, Naveen; Dayal, Mayanka; Pant, Archana; Kumar, Pawan; Saxena, Shruti; Allin, Kristine H.; Hansen, Torben; Arumugam, Manimozhiyan; Vestergaard, Henrik; Pedersen, Oluf; Pereira, Verima; Abraham, Philip; Tripathi, Reva; Wadhwa, Nitya; Bhatnagar, Shinjini; Prakash, Visvanathan Gnana; Radha, Venkatesan; Anjana, R. M.; Mohan, V.; Takeda, Kiyoshi; Kurakawa, Takashi; Nair, G. Balakrish; Das, Bhabatosh

    2016-01-01

    To explore the natural microbial community of any ecosystems by high-resolution molecular approaches including next generation sequencing, it is extremely important to develop a sensitive and reproducible DNA extraction method that facilitate isolation of microbial DNA of sufficient purity and quantity from culturable and uncultured microbial species living in that environment. Proper lysis of heterogeneous community microbial cells without damaging their genomes is a major challenge. In this study, we have developed an improved method for extraction of community DNA from different environmental and human origin samples. We introduced a combination of physical, chemical and mechanical lysis methods for proper lysis of microbial inhabitants. The community microbial DNA was precipitated by using salt and organic solvent. Both the quality and quantity of isolated DNA was compared with the existing methodologies and the supremacy of our method was confirmed. Maximum recovery of genomic DNA in the absence of substantial amount of impurities made the method convenient for nucleic acid extraction. The nucleic acids obtained using this method are suitable for different downstream applications. This improved method has been named as the THSTI method to depict the Institute where the method was developed. PMID:27240745

  7. An Improved Method for High Quality Metagenomics DNA Extraction from Human and Environmental Samples.

    Science.gov (United States)

    Bag, Satyabrata; Saha, Bipasa; Mehta, Ojasvi; Anbumani, D; Kumar, Naveen; Dayal, Mayanka; Pant, Archana; Kumar, Pawan; Saxena, Shruti; Allin, Kristine H; Hansen, Torben; Arumugam, Manimozhiyan; Vestergaard, Henrik; Pedersen, Oluf; Pereira, Verima; Abraham, Philip; Tripathi, Reva; Wadhwa, Nitya; Bhatnagar, Shinjini; Prakash, Visvanathan Gnana; Radha, Venkatesan; Anjana, R M; Mohan, V; Takeda, Kiyoshi; Kurakawa, Takashi; Nair, G Balakrish; Das, Bhabatosh

    2016-01-01

    To explore the natural microbial community of any ecosystems by high-resolution molecular approaches including next generation sequencing, it is extremely important to develop a sensitive and reproducible DNA extraction method that facilitate isolation of microbial DNA of sufficient purity and quantity from culturable and uncultured microbial species living in that environment. Proper lysis of heterogeneous community microbial cells without damaging their genomes is a major challenge. In this study, we have developed an improved method for extraction of community DNA from different environmental and human origin samples. We introduced a combination of physical, chemical and mechanical lysis methods for proper lysis of microbial inhabitants. The community microbial DNA was precipitated by using salt and organic solvent. Both the quality and quantity of isolated DNA was compared with the existing methodologies and the supremacy of our method was confirmed. Maximum recovery of genomic DNA in the absence of substantial amount of impurities made the method convenient for nucleic acid extraction. The nucleic acids obtained using this method are suitable for different downstream applications. This improved method has been named as the THSTI method to depict the Institute where the method was developed. PMID:27240745

  8. Estimation of sampling error uncertainties in observed surface air temperature change in China

    Science.gov (United States)

    Hua, Wei; Shen, Samuel S. P.; Weithmann, Alexander; Wang, Huijun

    2016-06-01

    This study examines the sampling error uncertainties in the monthly surface air temperature (SAT) change in China over recent decades, focusing on the uncertainties of gridded data, national averages, and linear trends. Results indicate that large sampling error variances appear at the station-sparse area of northern and western China with the maximum value exceeding 2.0 K2 while small sampling error variances are found at the station-dense area of southern and eastern China with most grid values being less than 0.05 K2. In general, the negative temperature existed in each month prior to the 1980s, and a warming in temperature began thereafter, which accelerated in the early and mid-1990s. The increasing trend in the SAT series was observed for each month of the year with the largest temperature increase and highest uncertainty of 0.51 ± 0.29 K (10 year)-1 occurring in February and the weakest trend and smallest uncertainty of 0.13 ± 0.07 K (10 year)-1 in August. The sampling error uncertainties in the national average annual mean SAT series are not sufficiently large to alter the conclusion of the persistent warming in China. In addition, the sampling error uncertainties in the SAT series show a clear variation compared with other uncertainty estimation methods, which is a plausible reason for the inconsistent variations between our estimate and other studies during this period.

  9. Extreme 13C depletion of CCl2F2 in firn air samples from NEEM, Greenland

    Directory of Open Access Journals (Sweden)

    T. Blunier

    2012-07-01

    Full Text Available A series of 12 high volume air samples collected from the S2 firn core during the North Greenland Eemian Ice Drilling (NEEM 2009 campaign have been measured for mixing ratio and stable carbon isotope composition of the chlorofluorocarbon CFC-12 (CCl2F2. While the mixing ratio measurements compare favorably to other firn air studies, the isotope results show extreme 13C depletion at the deepest measurable depth (65 m, to values lower than δ13C = −80‰ vs. VPDB (the international stable carbon isotope scale, compared to present day surface tropospheric measurements near −40‰. Firn air modeling was used to interpret these measurements. Reconstructed atmospheric time series indicate even larger depletions (to −120‰ near 1950 AD, with subsequent rapid enrichment of the atmospheric reservoir of the compound to the present day value. Mass-balance calculations show that this change must have been caused by a large change in the isotopic composition of anthropogenic CFC-12 emissions, probably due to technological changes in the CFC production process over the last 80 yr. Propagating the mass-balance calculations into the future demonstrates that as emissions decrease to zero, isotopic fractionation by the stratospheric sinks will lead to continued 13C enrichment in atmospheric CFC-12.

  10. Extreme 13C depletion of CCl2F2 in firn air samples from NEEM, Greenland

    Directory of Open Access Journals (Sweden)

    T. Blunier

    2013-01-01

    Full Text Available A series of 12 high volume air samples collected from the S2 firn core during the North Greenland Eemian Ice Drilling (NEEM 2009 campaign have been measured for mixing ratio and stable carbon isotope composition of the chlorofluorocarbon CFC-12 (CCl2F2. While the mixing ratio measurements compare favorably to other firn air studies, the isotope results show extreme 13C depletion at the deepest measurable depth (65 m, to values lower than δ13C = −80‰ vs. VPDB (the international stable carbon isotope scale, compared to present day surface tropospheric measurements near −40‰. Firn air modeling was used to interpret these measurements. Reconstructed atmospheric time series indicate even larger depletions (to −120‰ near 1950 AD, with subsequent rapid enrichment of the atmospheric reservoir of the compound to the present day value. Mass-balance calculations show that this change is likely to have been caused by a large change in the isotopic composition of anthropogenic CFC-12 emissions, probably due to technological advances in the CFC production process over the last 80 yr, though direct evidence is lacking.

  11. Quantitative Detection of Trace Malachite Green in Aquiculture Water Samples by Extractive Electrospray Ionization Mass Spectrometry

    Science.gov (United States)

    Fang, Xiaowei; Yang, Shuiping; Chingin, Konstantin; Zhu, Liang; Zhang, Xinglei; Zhou, Zhiquan; Zhao, Zhanfeng

    2016-01-01

    Exposure to malachite green (MG) may pose great health risks to humans; thus, it is of prime importance to develop fast and robust methods to quantitatively screen the presence of malachite green in water. Herein the application of extractive electrospray ionization mass spectrometry (EESI-MS) has been extended to the trace detection of MG within lake water and aquiculture water, due to the intensive use of MG as a biocide in fisheries. This method has the advantage of obviating offline liquid-liquid extraction or tedious matrix separation prior to the measurement of malachite green in native aqueous medium. The experimental results indicate that the extrapolated detection limit for MG was ~3.8 μg·L−1 (S/N = 3) in lake water samples and ~0.5 μg·L−1 in ultrapure water under optimized experimental conditions. The signal intensity of MG showed good linearity over the concentration range of 10–1000 μg·L−1. Measurement of practical water samples fortified with MG at 0.01, 0.1 and 1.0 mg·L−1 gave a good validation of the established calibration curve. The average recoveries and relative standard deviation (RSD) of malachite green in lake water and Carassius carassius fish farm effluent water were 115% (6.64% RSD), 85.4% (9.17% RSD) and 96.0% (7.44% RSD), respectively. Overall, the established EESI-MS/MS method has been demonstrated suitable for sensitive and rapid (<2 min per sample) quantitative detection of malachite green in various aqueous media, indicating its potential for online real-time monitoring of real life samples. PMID:27529262

  12. Preparation and examination of monolithic in-needle extraction (MINE) device for the direct analysis of liquid samples

    International Nuclear Information System (INIS)

    Graphical abstract: -- Highlights: •MINE device for isolation of analytes from water samples. •Nine polymer poly(styrene-divinylbenzene) monoliths prepared in stainless steel needles. •High efficiency of in-needle extraction systems based on monolithic materials. •New possibilities in sample preparation area. -- Abstract: Combination of extraction and chromatographic techniques opens NEW possibilities in sample preparation area. Macroporous poly(styrene-divinylbenzene) (PS-DVB) monoliths were prepared by in situ polymerization in stainless steel needles. The surface of stainless steel needle was modified earlier by the silane coupling agent. Monolithic materials located inside needles were used as the in-needle extraction device. Scanning electron microscope (SEM) images were obtained for nine monoliths. Spectra of prepared materials were also performed with the use of two techniques: Attenuated Total Reflectance (ATR) and Fourier Transform Infrared Spectroscopy (FTIR). The new monolithic in-needle extraction (MINE) devices were used in the preparation of a series of test water samples for chromatographic analysis. The extraction of phenolic compounds from water samples was carried out by pumping liquid samples through the MINE device. Obtained results indicate a high efficiency of in-needle extraction systems based on monolithic materials. Breakthrough volume and the sorption efficiency of prepared monolithic in-needle extraction devices were determined experimentally. The achieved recovery was close to 90%, and determined LOQ values varied between 0.4 and 6 μg

  13. Preparation and examination of monolithic in-needle extraction (MINE) device for the direct analysis of liquid samples

    Energy Technology Data Exchange (ETDEWEB)

    Pietrzyńska, Monika, E-mail: monikapietrzynska@gmail.com; Voelkel, Adam; Bielicka-Daszkiewicz, Katarzyna

    2013-05-07

    Graphical abstract: -- Highlights: •MINE device for isolation of analytes from water samples. •Nine polymer poly(styrene-divinylbenzene) monoliths prepared in stainless steel needles. •High efficiency of in-needle extraction systems based on monolithic materials. •New possibilities in sample preparation area. -- Abstract: Combination of extraction and chromatographic techniques opens NEW possibilities in sample preparation area. Macroporous poly(styrene-divinylbenzene) (PS-DVB) monoliths were prepared by in situ polymerization in stainless steel needles. The surface of stainless steel needle was modified earlier by the silane coupling agent. Monolithic materials located inside needles were used as the in-needle extraction device. Scanning electron microscope (SEM) images were obtained for nine monoliths. Spectra of prepared materials were also performed with the use of two techniques: Attenuated Total Reflectance (ATR) and Fourier Transform Infrared Spectroscopy (FTIR). The new monolithic in-needle extraction (MINE) devices were used in the preparation of a series of test water samples for chromatographic analysis. The extraction of phenolic compounds from water samples was carried out by pumping liquid samples through the MINE device. Obtained results indicate a high efficiency of in-needle extraction systems based on monolithic materials. Breakthrough volume and the sorption efficiency of prepared monolithic in-needle extraction devices were determined experimentally. The achieved recovery was close to 90%, and determined LOQ values varied between 0.4 and 6 μg.

  14. Extraction of methylmercury from tissue and plant samples by acid leaching

    Energy Technology Data Exchange (ETDEWEB)

    Hintelmann, Holger; Nguyen, Hong T. [Trent University, Chemistry Department, Peterborough, ON (Canada)

    2005-01-01

    A simple and efficient extraction method based on acidic leaching has been developed for measurement of methylmercury (MeHg) in benthic organisms and plant material. Methylmercury was measured by speciated isotope-dilution mass spectrometry (SIDMS), using gas chromatography interfaced with inductively coupled plasma mass spectrometry (GC-ICP-MS). Reagent concentration and digestion temperature were optimized for several alkaline and acidic extractants. Recovery was evaluated by addition of MeHg enriched with CH{sub 3}{sup 201}Hg{sup +}. Certified reference materials (CRM) were used to evaluate the efficiency of the procedure. The final digestion method used 5 mL of 4 mol L{sup -1} HNO{sub 3} at 55 C to leach MeHg from tissue and plant material. The digest was further processed by aqueous phase ethylation, without interference with the ethylation step, resulting in 96{+-}7% recovery of CH{sub 3}{sup 201}Hg{sup +} from oyster tissue and 93{+-}7% from pine needles. Methylmercury was stable in this solution for at least 1 week and measured concentrations of MeHg in CRM were statistically not different from certified values. The method was applied to real samples of benthic invertebrates and inter-laboratory comparisons were conducted using lyophilized zooplankton, chironomidae, and notonectidae samples. (orig.)

  15. Single sample extraction protocol for the quantification of NAD and NADH redox states in Saccharomyces cerevisiae.

    Science.gov (United States)

    Sporty, Jennifer L; Kabir, Md Mohiuddin; Turteltaub, Kenneth W; Ognibene, Ted; Lin, Su-Ju; Bench, Graham

    2008-10-01

    A robust redox extraction protocol for quantitative and reproducible metabolite isolation and recovery has been developed for simultaneous measurement of nicotinamide adenine dinucleotide (NAD) and its reduced form, NADH, from Saccharomyces cerevisiae. Following culture in liquid media, yeast cells were harvested by centrifugation and then lysed under nonoxidizing conditions by bead blasting in ice-cold, nitrogen-saturated 50 mM ammonium acetate. To enable protein denaturation, ice cold nitrogen-saturated CH(3)CN/50 mM ammonium acetate (3:1 v/v) was added to the cell lysates. Chloroform extractions were performed on supernatants to remove organic solvent. Samples were lyophilized and resuspended in 50 mM ammonium acetate. NAD and NADH were separated by HPLC and quantified using UV-Vis absorbance detection. NAD and NADH levels were evaluated in yeast grown under normal (2% glucose) and calorie restricted (0.5% glucose) conditions. Results demonstrate that it is possible to perform a single preparation to reliably and robustly quantitate both NAD and NADH contents in the same sample. Robustness of the protocol suggests it will be (i) applicable to quantification of these metabolites in other cell cultures; and (ii) amenable to isotope labeling strategies to determine the relative contribution of specific metabolic pathways to total NAD and NADH levels in cell cultures. PMID:18763242

  16. Extraction of methylmercury from tissue and plant samples by acid leaching.

    Science.gov (United States)

    Hintelmann, Holger; Nguyen, Hong T

    2005-01-01

    A simple and efficient extraction method based on acidic leaching has been developed for measurement of methylmercury (MeHg) in benthic organisms and plant material. Methylmercury was measured by speciated isotope-dilution mass spectrometry (SIDMS), using gas chromatography interfaced with inductively coupled plasma mass spectrometry (GC-ICP-MS). Reagent concentration and digestion temperature were optimized for several alkaline and acidic extractants. Recovery was evaluated by addition of MeHg enriched with CH3 201Hg+. Certified reference materials (CRM) were used to evaluate the efficiency of the procedure. The final digestion method used 5 mL of 4 mol L(-1) HNO3 at 55 degrees C to leach MeHg from tissue and plant material. The digest was further processed by aqueous phase ethylation, without interference with the ethylation step, resulting in 96 +/- 7% recovery of CH3 201Hg+ from oyster tissue and 93+/-7% from pine needles. Methylmercury was stable in this solution for at least 1 week and measured concentrations of MeHg in CRM were statistically not different from certified values. The method was applied to real samples of benthic invertebrates and inter-laboratory comparisons were conducted using lyophilized zooplankton, chironomidae, and notonectidae samples. PMID:15662514

  17. Simulated radioactive decontamination of biological samples using a portable DNA extraction instrument for rapid DNA profiling.

    Science.gov (United States)

    Frégeau, Chantal J; Dalpé, Claude

    2016-02-01

    A portable DNA extraction instrument was evaluated for its ability to decontaminate blood and saliva samples deposited on different surfaces (metal, plastic and glass) contaminated with stable isotopes of cobalt (Co), cesium (Cs), and strontium (Sr) as equivalents to their radiogenic (60)Co, (137)Cs, and (90)Sr isotopes, respectively, that could be released during a nuclear weapon accident or a radiological dispersal device (RDD) detonation. Despite the very high contamination levels tested in this study, successful removal of greater than 99.996% of the Co, Cs, Sr contaminants was achieved based on inductively coupled plasma-mass spectrometry (ICP-MS) and neutron activation analyses carried out on all liquids (including DNA eluates) and solid waste produced during automated DNA extraction. The remaining amounts of Co, Cs and Sr in the DNA eluates, when converted to dose rates (corresponding to (60)Co, (137)Cs and (90)Sr), were determined to be below the recommended dose limits for the general public in most of the scenarios tested. The presence of Co, Cs and Sr contaminants in the cell lysates had no adverse impact on the binding of DNA onto the magnetic DNA IQ™ beads. DNA yields were similar to uncontaminated controls. The remaining Co, Cs and Sr in the DNA eluates did not interfere with real-time PCR DNA quantification. In addition, the quality of the AmpFlSTR(®) Identifiler(®) profiles derived in 26min using an accelerated protocol was very good and comparable to controls. This study emphasizes the use of an accelerated process involving a portable DNA extraction instrument to significantly reduce radioactive dose rates to allow contaminated samples to be processed safely in a forensic mobile laboratory to expedite the identification of individuals potentially involved in the dispersal of nuclear or other radioactive materials. PMID:26773226

  18. Single sample extraction and HPLC processing for quantification of NAD and NADH levels in Saccharomyces cerevisiae

    Energy Technology Data Exchange (ETDEWEB)

    Sporty, J; Kabir, M M; Turteltaub, K; Ognibene, T; Lin, S; Bench, G

    2008-01-10

    A robust redox extraction protocol for quantitative and reproducible metabolite isolation and recovery has been developed for simultaneous measurement of nicotinamide adenine dinucleotide (NAD) and its reduced form, NADH, from Saccharomyces cerevisiae. Following culture in liquid media, approximately 10{sup 8} yeast cells were harvested by centrifugation and then lysed under non-oxidizing conditions by bead blasting in ice-cold, nitrogen-saturated 50-mM ammonium acetate. To enable protein denaturation, ice cold nitrogen-saturated CH{sub 3}CN + 50-mM ammonium acetate (3:1; v:v) was added to the cell lysates. After sample centrifugation to pellet precipitated proteins, organic solvent removal was performed on supernatants by chloroform extraction. The remaining aqueous phase was dried and resuspended in 50-mM ammonium acetate. NAD and NADH were separated by HPLC and quantified using UV-VIS absorbance detection. Applicability of this procedure for quantifying NAD and NADH levels was evaluated by culturing yeast under normal (2% glucose) and calorie restricted (0.5% glucose) conditions. NAD and NADH contents are similar to previously reported levels in yeast obtained using enzymatic assays performed separately on acid (for NAD) and alkali (for NADH) extracts. Results demonstrate that it is possible to perform a single preparation to reliably and robustly quantitate both NAD and NADH contents in the same sample. Robustness of the protocol suggests it will be (1) applicable to quantification of these metabolites in mammalian and bacterial cell cultures; and (2) amenable to isotope labeling strategies to determine the relative contribution of specific metabolic pathways to total NAD and NADH levels in cell cultures.

  19. Measurement of gross alpha and beta in air filter samples by using liquid scintillation counter

    International Nuclear Information System (INIS)

    The determination of gross alpha and gross beta in particulate air filter samples was carried out by alpha, beta discrimination method using Liquid Scintillation Analyzer by setting the PSA value at 55 for 5 ml 0.1 HCl plus 15 ml of Ultima Gold AB cocktail by using 241Am and 90Sr/90Y sources. The standardized method was compared with the gross alpha and gross beta activity determined by conventional method of direct counting with end window G.M. counter and ZnS (Ag). The minimum detectable activity of LSA method was found to be 9.3 mBq and 17.7 mBq for gross alpha and gross beta respectively for 6000 sec compared to the conventional method of 9.8 mBq and 189 mBq respectively at the same counting time. The result of analysis by both method indicate that the alpha, beta discrimination set up of LSA method is highly effective in the determination of low level alpha, beta activity in air filter samples. (author)

  20. Comparison of DNA Extraction Methods from Small Samples of Newborn Screening Cards Suitable for Retrospective Perinatal Viral Research

    OpenAIRE

    McMichael, Gai L.; Highet, Amanda R.; Gibson, Catherine S; Goldwater, Paul N; O'Callaghan, Michael E.; Alvino, Emily R.; MacLennan, Alastair H

    2011-01-01

    Reliable detection of viral DNA in stored newborn screening cards (NSC) would give important insight into possible silent infection during pregnancy and around birth. We sought a DNA extraction method with sufficient sensitivity to detect low copy numbers of viral DNA from small punch samples of NSC. Blank NSC were spotted with seronegative EDTA-blood and seropositive EBV EDTA-blood. DNA was extracted with commercial and noncommercial DNA extraction methods and quantified on a spectrofluorome...

  1. Development and application of a solidphase extraction method for simultaneousdetermination of PAHs, oxy-PAHs andazaarenes in water samples

    OpenAIRE

    WANG Yu

    2012-01-01

    In this study, a solid phase extraction (SPE) method was developed that can be used to extract a wide range of polycyclic aromatic compounds (PACs), including polycyclic aromatic hydrocarbons (PAHs), oxygenated PAHs (oxy-PAHs) and azaarenes, from water samples. Three commercially available SPE materials, i.e. Oasis HLB, ISOLUTE C2/C18 (EC) and ISOLUTE PAH, were tested for their capability to accomplish the extraction, and two were chosen for further optimization. Several different combination...

  2. Determination of Organic Pollutants in Small Samples of Groundwaters by Liquid-Liquid Extraction and Capillary Gas Chromatography

    DEFF Research Database (Denmark)

    Harrison, I.; Leader, R.U.; Higgo, J.J.W.;

    1994-01-01

    A method is presented for the determination of 22 organic compounds in polluted groundwaters. The method includes liquid-liquid extraction of the base/neutral organics from small, alkaline groundwater samples, followed by derivatisation and liquid-liquid extraction of phenolic compounds after neu...... neutralisation. The extracts were analysed by capillary gas chromatography. Dual detection by flame Ionisation and electron capture was used to reduce analysis time....

  3. Methylmercury determination in biological samples using electrothermal atomic absorption spectrometry after acid leaching extraction

    Energy Technology Data Exchange (ETDEWEB)

    Saber-Tehrani, Mohammad; Hashemi-Moghaddam, Hamid; Givianrad, Mohammad Hadi; Abroomand-Azar, Parviz [Islamic Azad University, Department of Chemistry, Science and Research Branch, Tehran (Iran)

    2006-11-15

    An efficient and sensitive method for the determination of methylmercury in biological samples was developed based on acid leaching extraction of methylmercury into toluene. Methylmercury in the organic phase was determined by electrothermal atomic absorption spectrometry (ETAAS). The methylmercury signal was enhanced and the reproducibility increased by formation of certain complexes and addition of Pd-DDC modifier. The complex of methylmercury with DDC produced the optimum analytical signal in terms of sensitivity and reproducibility compared to complexes with dithizone, cysteine, 1,10-phenanthroline, and diethyldithiocarbamate. Method performance was optimized by modifying parameters such as temperature of mineralization, atomization, and gas flow rate. The limit of detection for methylmercury determination was 0.015 {mu}g g{sup -1} and the RSD of the whole procedure was 12% for human teeth samples (n=5) and 15.8% for hair samples (n=5). The method's accuracy was investigated by using NIES-13 and by spiking the samples with different amounts of methylmercury. The results were in good agreement with the certified values and the recoveries were 88-95%. (orig.)

  4. Sequential injection system incorporating a micro extraction column for automatic fractionation of metal ions in solid samples

    DEFF Research Database (Denmark)

    Chomchoei, Roongrat; Miró, Manuel; Hansen, Elo Harald;

    2005-01-01

    Recently a novel approach to perform sequential extractions (SE) of elements in solid samples was developed by this group, based upon the use of a sequential injection (SI) system incorporating a specially designed extraction microcolumn. Entailing a number of distinct advantages as compared to c...... CRM483 soil which exhibits inhomogeneity in the particle size distribution....

  5. Freezing fecal samples prior to DNA extraction affects the Firmicutes to Bacteroidetes ratio determined by downstream quantitative PCR analysis

    DEFF Research Database (Denmark)

    Bahl, Martin Iain; Bergström, Anders; Licht, Tine Rask

    2012-01-01

    Freezing stool samples prior to DNA extraction and downstream analysis is widely used in metagenomic studies of the human microbiota but may affect the inferred community composition. In this study, DNA was extracted either directly or following freeze storage of three homogenized human fecal...

  6. Freezing fecal samples prior to DNA extraction affects the Firmicutes to Bacteroidetes ratio determined by downstream quantitative PCR analysis

    DEFF Research Database (Denmark)

    Bahl, Martin Iain; Bergström, Anders; Licht, Tine Rask

    Freezing stool samples prior to DNA extraction and downstream analysis is widely used in metagenomic studies of the human microbiota but may affect the inferred community composition. In this study DNA was extracted either directly or following freeze storage of three homogenized human fecal...

  7. Subcritical water extraction of alkaloids in Sophora flavescens Ait. and determination by capillary electrophoresis with field-amplified sample stacking.

    Science.gov (United States)

    Wang, Haiyan; Lu, Yuchao; Chen, Jie; Li, Junchao; Liu, Shuhui

    2012-01-25

    The extraction and determination of cytisine, sophocarpine, matrine, sophoridine and oxymatrine in Sophora flavescens Ait. were performed using subcritical water extraction and capillary electrophoresis with field-amplified sample stacking. The effects of extraction temperature, pressure, time and cycle number on the extraction yields were investigated systematically for accelerated solvent extraction with ethanol (ASE) and accelerated solvent extraction with water (subcritical water extraction, SWE). The extraction yields obtained using SWE, ASE, water ultrasonic extraction and chloroform soaking extraction methods were compared. The electrophoresis separation buffer was monosodium phosphate (pH 3.0; 110 mM)-isopropanol (85:15, v/v). The effect of phosphoric acid added to the sample matrix on the reproducibility of the peak heights of the analytes was also examined. Cytisine, sophoridine and oxymatrine showed good linearity (R(2)>0.999) within 0.125-4.0 μg/mL, and sophocarpine and matrine exhibited good linearity (R(2)>0.998) within 0.0625-2.0 μg/mL, with the detection limits in the range of 0.004-0.0013 μg/mL. The five alkaloid contents in medicinal plants from different sources and Sophora instant granule were determined and compared. PMID:21996061

  8. Extraction of Water from Soil and Plant Samples for 18O/16O and D/H Isotope Ratio Measurements

    International Nuclear Information System (INIS)

    The need for a rapid, inexpensive technique for routine extraction of water from plant and soil samples for Oxygen-18/Oxygen-16 (18O/16O) and Hydrogen-2/Hydrogen-1 (D/H) isotope ratio measurements is increasing due to the greater demand for isotopic data in agroecological, soil water, evaporation and transpiration partitioning and hydrological studies. The common sample extraction technique is vacuum distillation. Most of the current techniques are laborious, time consuming and involve complicated setups with specially-made glass apparatus. In addition, liquid nitrogen or dry ice is needed to freeze and trap water vapour evaporated during extraction. Both of these cooling agents can be difficult to acquire in many developing countries. With water isotope analyses becoming cheaper, easier and faster (e.g. through the development of modern laser isotope analysers), the bottleneck in sample throughput is often the water extraction time from the soil and plant samples instead of the isotopic analysis of water

  9. Extraction of semivolatile organic compounds from high-efficiency particulate air (HEPA) filters by supercritical carbon dioxide

    International Nuclear Information System (INIS)

    Supercritical fluid extraction (SFE) using unmodified carbon dioxide has been explored as an alternative method for the extraction of semivolatile organic compounds from high-efficiency particulate air (HEPA) filters. HEPA filters provide the final stage of containment on many exhaust systems in US Department of Energy (DOE) facilities by preventing the escape of chemical and radioactive materials entrained in the exhausted air. The efficiency of the filters is tested by the manufacturer and DOE using dioctylphthalate (DOP), a substance regulated by the US Environmental Protection Agency under the Resource Conservation and Recovery Act. Therefore, the filters must be analyzed for semivolatile organics before disposal. Ninety-eight acid, base, and neutral semivolatile organics were spiked onto blank HEPA material and extracted using SFE, Soxhlet, automated Soxhlet, and sonication techniques. The SFE conditions were optimized using a Dionex SFE-703 instrument. Average recoveries for the 98 semivolatile compounds are 82.7% for Soxhlet, 74.0% for sonication, 70.2% for SFE, and 62.9% for Soxtec. Supercritical fluid extraction reduces the extraction solvent volume to 10--15 mL, a factor of 20--30 less than Soxhlet and more than 5 times less than Soxtec and sonication. Extraction times of 30--45 min are used compared to 16--18 h for Soxhlet extraction

  10. Extraction of semivolatile organic compounds from high-efficiency particulate air (HEPA) filters by supercritical carbon dioxide

    Energy Technology Data Exchange (ETDEWEB)

    Schilling, J.B.

    1997-09-01

    Supercritical fluid extraction (SFE) using unmodified carbon dioxide has been explored as an alternative method for the extraction of semivolatile organic compounds from high-efficiency particulate air (HEPA) filters. HEPA filters provide the final stage of containment on many exhaust systems in US Department of Energy (DOE) facilities by preventing the escape of chemical and radioactive materials entrained in the exhausted air. The efficiency of the filters is tested by the manufacturer and DOE using dioctylphthalate (DOP), a substance regulated by the US Environmental Protection Agency under the Resource Conservation and Recovery Act. Therefore, the filters must be analyzed for semivolatile organics before disposal. Ninety-eight acid, base, and neutral semivolatile organics were spiked onto blank HEPA material and extracted using SFE, Soxhlet, automated Soxhlet, and sonication techniques. The SFE conditions were optimized using a Dionex SFE-703 instrument. Average recoveries for the 98 semivolatile compounds are 82.7% for Soxhlet, 74.0% for sonication, 70.2% for SFE, and 62.9% for Soxtec. Supercritical fluid extraction reduces the extraction solvent volume to 10--15 mL, a factor of 20--30 less than Soxhlet and more than 5 times less than Soxtec and sonication. Extraction times of 30--45 min are used compared to 16--18 h for Soxhlet extraction.

  11. Solid phase speciation of arsenic by sequential extraction in standard reference materials and industrially contaminated soil samples

    Energy Technology Data Exchange (ETDEWEB)

    Herreweghe, Samuel van; Swennen, Rudy; Vandecasteele, Carlo; Cappuyns, Valerie

    2003-04-01

    Leaching experiments, a mineralogical survey and larger samples are preferred when arsenic is present as discrete mineral phases. - Availability, mobility, (phyto)toxicity and potential risk of contaminants is strongly affected by the manner of appearance of elements, the so-called speciation. Operational fractionation methods like sequential extractions have been applied for a long time to determine the solid phase speciation of heavy metals since direct determination of specific chemical compounds can not always be easily achieved. The three-step sequential extraction scheme recommended by the BCR and two extraction schemes based on the phosphorus-like protocol proposed by Manful (1992, Occurrence and Ecochemical Behaviours of Arsenic in a Goldsmelter Impacted Area in Ghana, PhD dissertation, at the RUG) were applied to four standard reference materials (SRM) and to a batch of samples from industrially contaminated sites, heavily contaminated with arsenic and heavy metals. The SRM 2710 (Montana soil) was found to be the most useful reference material for metal (Mn, Cu, Zn, As, Cd and Pb) fractionation using the BCR sequential extraction procedure. Two sequential extraction schemes were developed and compared for arsenic with the aim to establish a better fractionation and recovery rate than the BCR-scheme for this element in the SRM samples. The major part of arsenic was released from the heavily contaminated samples after NaOH-extraction. Inferior extraction variability and recovery in the heavily contaminated samples compared to SRMs could be mainly contributed to subsample heterogeneity.

  12. Solid phase speciation of arsenic by sequential extraction in standard reference materials and industrially contaminated soil samples

    International Nuclear Information System (INIS)

    Leaching experiments, a mineralogical survey and larger samples are preferred when arsenic is present as discrete mineral phases. - Availability, mobility, (phyto)toxicity and potential risk of contaminants is strongly affected by the manner of appearance of elements, the so-called speciation. Operational fractionation methods like sequential extractions have been applied for a long time to determine the solid phase speciation of heavy metals since direct determination of specific chemical compounds can not always be easily achieved. The three-step sequential extraction scheme recommended by the BCR and two extraction schemes based on the phosphorus-like protocol proposed by Manful (1992, Occurrence and Ecochemical Behaviours of Arsenic in a Goldsmelter Impacted Area in Ghana, PhD dissertation, at the RUG) were applied to four standard reference materials (SRM) and to a batch of samples from industrially contaminated sites, heavily contaminated with arsenic and heavy metals. The SRM 2710 (Montana soil) was found to be the most useful reference material for metal (Mn, Cu, Zn, As, Cd and Pb) fractionation using the BCR sequential extraction procedure. Two sequential extraction schemes were developed and compared for arsenic with the aim to establish a better fractionation and recovery rate than the BCR-scheme for this element in the SRM samples. The major part of arsenic was released from the heavily contaminated samples after NaOH-extraction. Inferior extraction variability and recovery in the heavily contaminated samples compared to SRMs could be mainly contributed to subsample heterogeneity

  13. Evaluation of sampling methods for toxicological testing of indoor air particulate matter.

    Science.gov (United States)

    Tirkkonen, Jenni; Täubel, Martin; Hirvonen, Maija-Riitta; Leppänen, Hanna; Lindsley, William G; Chen, Bean T; Hyvärinen, Anne; Huttunen, Kati

    2016-09-01

    There is a need for toxicity tests capable of recognizing indoor environments with compromised air quality, especially in the context of moisture damage. One of the key issues is sampling, which should both provide meaningful material for analyses and fulfill requirements imposed by practitioners using toxicity tests for health risk assessment. We aimed to evaluate different existing methods of sampling indoor particulate matter (PM) to develop a suitable sampling strategy for a toxicological assay. During three sampling campaigns in moisture-damaged and non-damaged school buildings, we evaluated one passive and three active sampling methods: the Settled Dust Box (SDB), the Button Aerosol Sampler, the Harvard Impactor and the National Institute for Occupational Safety and Health (NIOSH) Bioaerosol Cyclone Sampler. Mouse RAW264.7 macrophages were exposed to particle suspensions and cell metabolic activity (CMA), production of nitric oxide (NO) and tumor necrosis factor (TNFα) were determined after 24 h of exposure. The repeatability of the toxicological analyses was very good for all tested sampler types. Variability within the schools was found to be high especially between different classrooms in the moisture-damaged school. Passively collected settled dust and PM collected actively with the NIOSH Sampler (Stage 1) caused a clear response in exposed cells. The results suggested the higher relative immunotoxicological activity of dust from the moisture-damaged school. The NIOSH Sampler is a promising candidate for the collection of size-fractionated PM to be used in toxicity testing. The applicability of such sampling strategy in grading moisture damage severity in buildings needs to be developed further in a larger cohort of buildings. PMID:27569522

  14. Mutagenic potency in Salmonella typhimurium of organic extracts of soil samples originating from urban, suburban, agricultural, forest and natural areas.

    Science.gov (United States)

    Courty, Benoit; Le Curieux, Frank; Belkessam, Laurence; Laboudigue, Agnès; Marzin, Daniel

    2008-05-31

    The purpose of the present work was to assess the mutagenic potency of soil samples presumably not contaminated by industrial wastes and discharges. A set of 51 soil samples was collected from areas considered as not contaminated by a known industrial activity: 11 urban samples (collected in cities), 15 suburban samples (collected in villages), 7 agricultural samples, and 18 forest or natural samples. Each soil sample was collected at the surface (0-5cm deep), dried, sieved (2mm), homogenized before organic extraction (dichloromethane/acetone 1/1 (v/v), 37 degrees C, 4h, soil/solvent ratio 1/2, m/v), solvent exchange to DMSO and sterilizing filtration. The micro-method adaptation of the standard bacterial mutagenicity test on Salmonella typhimurium strain TA98 was performed with and without a metabolic activation system (rat-liver homogenate S9), and thus detected the effect of pro-mutagens and direct mutagens, respectively. The use of a pre-incubation method increased the sensitivity of the assay. The results obtained showed a wide range of effect levels, from no effect to clear mutagenicity. In particular, the extract of all 11 urban soil samples demonstrated mutagenic activity, while the extracts of 10 of the 15 suburban samples showed mutagenicity. On the other hand, the extract of only one of the 7 agricultural samples studied induced mutations, and none of the 18 natural or forest-soil samples investigated produced mutagenic extracts. These findings seem to indicate the crucial influence of the diffuse pollution originating from different human activities on the mutagenic potency of urban soil samples. These findings make it possible to classify the soils according to their mutagenic potency. No clear correlation was found between the mutagenicity detected in soil extracts and the measured polycyclic aromatic hydrocarbon (PAH) content of the soils investigated. PMID:18440855

  15. Effect of DNA Extraction Methods and Sampling Techniques on the Apparent Structure of Cow and Sheep Rumen Microbial Communities

    OpenAIRE

    Gemma Henderson; Faith Cox; Sandra Kittelmann; Vahideh Heidarian Miri; Michael Zethof; Noel, Samantha J.; Garry C Waghorn; Janssen, Peter H.

    2013-01-01

    Molecular microbial ecology techniques are widely used to study the composition of the rumen microbiota and to increase understanding of the roles they play. Therefore, sampling and DNA extraction methods that result in adequate yields of microbial DNA that also accurately represents the microbial community are crucial. Fifteen different methods were used to extract DNA from cow and sheep rumen samples. The DNA yield and quality, and its suitability for downstream PCR amplifications varied co...

  16. Air-assisted liquid–liquid microextraction by solidifying the floating organic droplets for the rapid determination of seven fungicide residues in juice samples

    Energy Technology Data Exchange (ETDEWEB)

    You, Xiangwei [Tobacco Research Institute, Chinese Academy of Agricultural Sciences, Qingdao 266101 (China); College of Science, China Agricultural University, Beijing 100193 (China); Xing, Zhuokan [College of Science, China Agricultural University, Beijing 100193 (China); Liu, Fengmao, E-mail: liufengmao@cau.edu.cn [College of Science, China Agricultural University, Beijing 100193 (China); Zhang, Xu [College of Science, China Agricultural University, Beijing 100193 (China)

    2015-05-22

    Highlights: • A novel AALLME-SFO method was firstly reported for pesticide residue analysis. • Solvent with low density and proper melting point was used as extraction solvent. • The formation of “cloudy solvent” with a syringe only. • The new method avoided the use of organic dispersive solvent. - Abstract: A novel air assisted liquid–liquid microextraction using the solidification of a floating organic droplet method (AALLME-SFO) was developed for the rapid and simple determination of seven fungicide residues in juice samples, using the gas chromatography with electron capture detector (GC-ECD). This method combines the advantages of AALLME and dispersive liquid–liquid microextraction based on the solidification of floating organic droplets (DLLME-SFO) for the first time. In this method, a low-density solvent with a melting point near room temperature was used as the extraction solvent, and the emulsion was rapidly formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent for ten times repeatedly using a 10-mL glass syringe. After centrifugation, the extractant droplet could be easily collected from the top of the aqueous samples by solidifying it at a temperature lower than the melting point. Under the optimized conditions, good linearities with the correlation coefficients (γ) higher than 0.9959 were obtained and the limits of detection (LOD) varied between 0.02 and 0.25 μg L{sup −1}. The proposed method was applied to determine the target fungicides in juice samples and acceptable recoveries ranged from 72.6% to 114.0% with the relative standard deviations (RSDs) of 2.3–13.0% were achieved. Compared with the conventional DLLME method, the newly proposed method will neither require a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly.

  17. Air-assisted liquid–liquid microextraction by solidifying the floating organic droplets for the rapid determination of seven fungicide residues in juice samples

    International Nuclear Information System (INIS)

    Highlights: • A novel AALLME-SFO method was firstly reported for pesticide residue analysis. • Solvent with low density and proper melting point was used as extraction solvent. • The formation of “cloudy solvent” with a syringe only. • The new method avoided the use of organic dispersive solvent. - Abstract: A novel air assisted liquid–liquid microextraction using the solidification of a floating organic droplet method (AALLME-SFO) was developed for the rapid and simple determination of seven fungicide residues in juice samples, using the gas chromatography with electron capture detector (GC-ECD). This method combines the advantages of AALLME and dispersive liquid–liquid microextraction based on the solidification of floating organic droplets (DLLME-SFO) for the first time. In this method, a low-density solvent with a melting point near room temperature was used as the extraction solvent, and the emulsion was rapidly formed by pulling in and pushing out the mixture of aqueous sample solution and extraction solvent for ten times repeatedly using a 10-mL glass syringe. After centrifugation, the extractant droplet could be easily collected from the top of the aqueous samples by solidifying it at a temperature lower than the melting point. Under the optimized conditions, good linearities with the correlation coefficients (γ) higher than 0.9959 were obtained and the limits of detection (LOD) varied between 0.02 and 0.25 μg L−1. The proposed method was applied to determine the target fungicides in juice samples and acceptable recoveries ranged from 72.6% to 114.0% with the relative standard deviations (RSDs) of 2.3–13.0% were achieved. Compared with the conventional DLLME method, the newly proposed method will neither require a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly

  18. Dynamic fractionation of trace metals in soil and sediment samples using rotating coiled column extraction and sequential injection microcolumn extraction: a comparative study.

    Science.gov (United States)

    Rosende, Maria; Savonina, Elena Yu; Fedotov, Petr S; Miró, Manuel; Cerdà, Víctor; Wennrich, Rainer

    2009-09-15

    Dynamic fractionation has been recognized as an appealing alternative to conventional equilibrium-based sequential extraction procedures (SEPs) for partitioning of trace elements (TE) in environmental solid samples. This paper reports the first attempt for harmonization of flow-through dynamic fractionation using two novel methods, the so-called sequential injection microcolumn (SIMC) extraction and rotating coiled column (RCC) extraction. In SIMC extraction, a column packed with the solid sample is clustered in a sequential injection system, while in RCC, the particulate matter is retained under the action of centrifugal forces. In both methods, the leachants are continuously pumped through the solid substrates by the use of either peristaltic or syringe pumps. A five-step SEP was selected for partitioning of Cu, Pb and Zn in water soluble/exchangeable, acid-soluble, easily reducible, easily oxidizable and moderately reducible fractions from 0.2 to 0.5 g samples at an extractant flow rate of 1.0 mL min(-1) prior to leachate analysis by inductively coupled plasma-atomic emission spectrometry. Similarities and discrepancies between both dynamic approaches were ascertained by fractionation of TE in certified reference materials, namely, SRM 2711 Montana Soil and GBW 07311 sediment, and two real soil samples as well. Notwithstanding the different extraction conditions set by both methods, similar trends of metal distribution were in generally found. The most critical parameters for reliable assessment of mobilizable pools of TE in worse-case scenarios are the size-distribution of sample particles, the density of particles, the content of organic matter and the concentration of major elements. For reference materials and a soil rich in organic matter, the extraction in RCC results in slightly higher recoveries of environmentally relevant fractions of TE, whereas SIMC leaching is more effective for calcareous soils. PMID:19615513

  19. Establishing a novel automated magnetic bead-based method for the extraction of DNA from a variety of forensic samples.

    Science.gov (United States)

    Witt, Sebastian; Neumann, Jan; Zierdt, Holger; Gébel, Gabriella; Röscheisen, Christiane

    2012-09-01

    Automated systems have been increasingly utilized for DNA extraction by many forensic laboratories to handle growing numbers of forensic casework samples while minimizing the risk of human errors and assuring high reproducibility. The step towards automation however is not easy: The automated extraction method has to be very versatile to reliably prepare high yields of pure genomic DNA from a broad variety of sample types on different carrier materials. To prevent possible cross-contamination of samples or the loss of DNA, the components of the kit have to be designed in a way that allows for the automated handling of the samples with no manual intervention necessary. DNA extraction using paramagnetic particles coated with a DNA-binding surface is predestined for an automated approach. For this study, we tested different DNA extraction kits using DNA-binding paramagnetic particles with regard to DNA yield and handling by a Freedom EVO(®)150 extraction robot (Tecan) equipped with a Te-MagS magnetic separator. Among others, the extraction kits tested were the ChargeSwitch(®)Forensic DNA Purification Kit (Invitrogen), the PrepFiler™Automated Forensic DNA Extraction Kit (Applied Biosystems) and NucleoMag™96 Trace (Macherey-Nagel). After an extensive test phase, we established a novel magnetic bead extraction method based upon the NucleoMag™ extraction kit (Macherey-Nagel). The new method is readily automatable and produces high yields of DNA from different sample types (blood, saliva, sperm, contact stains) on various substrates (filter paper, swabs, cigarette butts) with no evidence of a loss of magnetic beads or sample cross-contamination. PMID:22310206

  20. Magnetic mixed hemimicelles solid-phase extraction coupled with high-performance liquid chromatography for the extraction and rapid determination of six fluoroquinolones in environmental water samples.

    Science.gov (United States)

    Wang, Li; Yuan, Qiuxiang; Liang, Guoxi; Shi, Longbiao; Zhan, Qian

    2015-03-01

    In this study, a mixed hemimicelle solid-phase extraction method based on Fe3 O4 nanoparticles coated with sodium dodecyl sulfate was applied for the preconcentration and fast isolation of six fluoroquinolones in environmental water samples before high-performance liquid chromatography determination. The main factors affecting the extraction efficiency of the analytes, such as amount of surfactant, amount of Fe3 O4 nanoparticles, extraction time, sample volume, sample pH, ionic strength, and desorption conditions, were investigated and optimized. The method has detection limits from 0.05 to 0.1 ng/mL and good linearity (r ≥ 09948) in the range 0.1-200 ng/mL depending on the fluoroquinolone. The enrichment factor is ∼200. The recoveries (at spiked levels of 1, 5, and 50 ng/mL) are in the range of 79-120%. PMID:25581496

  1. Accelerated solvent extraction followed by on-line solid-phase extraction coupled to ion trap LC/MS/MS for analysis of benzalkonium chlorides in sediment samples

    Science.gov (United States)

    Ferrer, I.; Furlong, E.T.

    2002-01-01

    Benzalkonium chlorides (BACs) were successfully extracted from sediment samples using a new methodology based on accelerated solvent extraction (ASE) followed by an on-line cleanup step. The BACs were detected by liquid chromatography/ion trap mass spectrometry (LC/MS) or tandem mass spectrometry (MS/MS) using an electrospray interface operated in the positive ion mode. This methodology combines the high efficiency of extraction provided by a pressurized fluid and the high sensitivity offered by the ion trap MS/MS. The effects of solvent type and ASE operational variables, such as temperature and pressure, were evaluated. After optimization, a mixture of acetonitrile/water (6:4 or 7:3) was found to be most efficient for extracting BACs from the sediment samples. Extraction recoveries ranged from 95 to 105% for C12 and C14 homologues, respectively. Total method recoveries from fortified sediment samples, using a cleanup step followed by ASE, were 85% for C12BAC and 79% for C14-BAC. The methodology developed in this work provides detection limits in the subnanogram per gram range. Concentrations of BAC homologues ranged from 22 to 206 ??g/kg in sediment samples from different river sites downstream from wastewater treatment plants. The high affinity of BACs for soil suggests that BACs preferentially concentrate in sediment rather than in water.

  2. Triphenylphosphine oxide as a feasible extractant for Uranium (VI) and its application for the determination of Uranium in geological samples

    International Nuclear Information System (INIS)

    Triphenylphosphine oxide (TPO) was chosen as an extractant for uranium from nitric acid medium. Different procedures and parameters were systemized to judge its feasibility. The executed experiments were carried out testing the following variables: TPO and nitric acid concentration, time of shaking, temperature, ph, different diluents, aqueous to organic phase ratio (A/O) and the different interfering ions. The factors studied were followed by investigation related to apply the extraction system of TPO to extract and determine uranium content from certain International and Reference geologic samples with application on local igneous and sedimentary samples. The final results indicate that the method is fast and selective

  3. Air-deployable oil spill sampling devices review phase 2 testing. Volume 1

    International Nuclear Information System (INIS)

    SAIC Canada tested air deployable oil sampling devices for the Emergencies Science and Technology Division of Environment Canada in order to determine the applicability and status of these devices. The 3 devices tested were: Canada's SABER (sampling autonomous buoy for evidence recovery), the United States' POPEIE (probe for oil pollution evidence in the environment); and, Sweden's SAR Floatation 2000. They were tested for buoyancy properties, drift behaviour and sampler sorbent pickup ratios. The SAR and SABER both had lesser draft and greater freeboard, while the POPEIE had much greater draft than freeboard. All 3 devices could be used for oil sample collection in that their drift characteristics would allow for the SABER and SAR devices to be placed upwind of the slick while the POPEIE device could be placed downwind of an oil spill. The sorbent testing revealed that Sefar sorbent and Spectra sorbent used in the 3 devices had negative pickup ratios for diesel but performance improved as oil viscosity increased. Both sorbents are inert and capable of collecting oil in sufficient volumes for consistent fingerprinting analysis. 10 refs., 8 tabs., 8 figs

  4. Unmanned platform for long-range remote analysis of volatile compounds in air samples.

    Science.gov (United States)

    da Costa, Eric T; Neves, Carlos A; Hotta, Guilherme M; Vidal, Denis T R; Barros, Marcelo F; Ayon, Arturo A; Garcia, Carlos D; do Lago, Claudimir Lucio

    2012-09-01

    This paper describes a long-range remotely controlled CE system built on an all-terrain vehicle. A four-stroke engine and a set of 12-V batteries were used to provide power to a series of subsystems that include drivers, communication, computers, and a capillary electrophoresis module. This dedicated instrument allows air sampling using a polypropylene porous tube, coupled to a flow system that transports the sample to the inlet of a fused-silica capillary. A hybrid approach was used for the construction of the analytical subsystem combining a conventional fused-silica capillary (used for separation) and a laser machined microfluidic block, made of PMMA. A solid-state cooling approach was also integrated in the CE module to enable controlling the temperature and therefore increasing the useful range of the robot. Although ultimately intended for detection of chemical warfare agents, the proposed system was used to analyze a series of volatile organic acids. As such, the system allowed the separation and detection of formic, acetic, and propionic acids with signal-to-noise ratios of 414, 150, and 115, respectively, after sampling by only 30 s and performing an electrokinetic injection during 2.0 s at 1.0 kV. PMID:22965708

  5. Results of Inspection and Cleaning of Two Radionuclide Air-Sampling Systems Based on the Requirements of ANSI/HPS N13.1-1999

    International Nuclear Information System (INIS)

    The Pacific Northwest National Laboratory (PNNL) conducted inspection and cleaning activities at two radionuclide air-sampling systems that continuously monitor radioactive air emissions from research and development (RandD) facilities. The inspection and cleaning was performed to evaluate effective methods and potential cost impacts of maintenance requirements in the revised American National Standard Institute (ANSI) standard Sampling and Monitoring Releases of Airborne Radioactive Substances from the Stacks and Ducts of Nuclear Facilities (ANSI/HPS N13.1-1999). The standard requires at least annual inspections of sampling systems followed by cleaning if deposits are visible. During 2001 and 2002, inspections were performed leaving the sampling systems in place and inserting videoscope cables into different access points to allow viewing of the inside and outside of sampling manifolds and transport lines. Cleaning was performed on one of the systems by disconnecting and extracting the sampling manifold, then washing it with de-ionized water and scrub brushes. The wash water was analyzed for radioactivity and solids. Results of the inspection showed greater deposition in one of the systems than would be expected by a High Efficiency Particulate Air (HEPA) filtered exhaust stream; the second system was also downstream of HEPA filters and appeared much cleaner. The videoscope was a useful and cost-effective tool and provided a better view than could be obtained with the naked eye. However, because even small amounts of deposition were made visible with the videoscope, clarification is needed in defining when probe washing is merited, particularly in existing sampling systems whose design is not conducive to easy removal and cleaning

  6. Molecularly imprinted solid-phase extraction of glutathione from urine samples

    Energy Technology Data Exchange (ETDEWEB)

    Song, Renyuan, E-mail: songrenyuan0726@163.com; Hu, Xiaoling; Guan, Ping; Li, Ji; Zhao, Na; Wang, Qiaoli

    2014-11-01

    Molecularly imprinted polymer (MIP) particles for glutathione were synthesized through iniferter-controlled living radical precipitation polymerization (IRPP) under ultraviolet radiation at ambient temperature. Static adsorption, solid-phase extraction, and high-performance liquid chromatography were carried out to evaluate the adsorption properties and selective recognition characteristics of the polymers for glutathione and its structural analogs. The obtained IRPP-MIP particles exhibited a regularly spherical shape, rapid binding kinetics, high imprinting factor, and high selectivity compared with the MIP particles prepared using traditional free-radical precipitation polymerization. The selective separation and enrichment of glutathione from the mixture of glycyl-glycine and glutathione disulfide could be achieved on the IRPP-MIP cartridge. The recoveries of glutathione, glycyl-glycine, and glutathione disulfide were 95.6% ± 3.65%, 29.5% ± 1.26%, and 49.9% ± 1.71%, respectively. The detection limit (S/N = 3) of glutathione was 0.5 mg·L{sup −1}. The relative standard deviations (RSDs) for 10 replicate detections of 50 mg·L{sup −1} of glutathione were 5.76%, and the linear range of the calibration curve was 0.5 mg·L{sup −1} to 200 mg·L{sup −1} under optimized conditions. The proposed approach was successfully applied to determine glutathione in spiked human urine samples with recoveries of 90.24% to 96.20% and RSDs of 0.48% to 5.67%. - Highlights: • Imprinted polymer particles were prepared by IRPP at ambient temperature. • High imprinting factor, high selectivity, and rapid binding kinetics were achieved. • Selective solid-phase extraction of glutathione from human urine samples.

  7. Sampling of power plant stacks for air toxic emissions: Topical report for Phases 1 and 2

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1995-02-21

    Under contract with the US Department of Energy (DE-AC22-92PCO0367), Pittsburgh Energy Technology Center, Radian Corporation has conducted a test program to collect and analyze size-fractionated stack gas particulate samples for selected inorganic hazardous air pollutants (HAPS). Specific goals of the program are (1) the collection of one-gram quantities of size-fractionated stack gas particulate matter for bulk (total) and surface chemical charactization, and (2) the determination of the relationship between particle size, bulk and surface (leachable) composition, and unit load. The information obtained from this program identifies the effects of unit load, particle size, and wet FGD system operation on the relative toxicological effects of exposure to particulate emissions.

  8. Molecular beam mass spectrometric sampling of minor species from coal dust-air flames

    International Nuclear Information System (INIS)

    It has been demonstrated that unaugmented, unconfined, premixed coal dust-air flames can be stabilized on small conical or flat, Meeker type burners. Since these flames are laminar, they can be used to study the kinetics of various processes in coal combustion and related areas such as understanding mechanisms of fireside corrosion and of flame and explosive inhibition. Some of the current work with these flames is directed toward identification and measurement of minor alkali metal and other species responsible for fireside corrosion. In order to make these measurements, molecular beam mass spectrometric sampling techniques have been adpated for use with these heterogeneous flames. In this paper, the equipment and techniques used are reviewed and some preliminary results presented

  9. Extraction of fatty acids from dried freshwater algae using accelerated solvent extraction

    Science.gov (United States)

    A high temperature/pressure extraction method (accelerated solvent extraction)(ASE) and a manual extraction method (modified Folch extraction) were compared with regard to their ability to extract total fat from three samples of air-dried filamentous algae and determine the fatty acid (FA) profile o...

  10. GUIDE TO CALCULATING TRANSPORT EFFICIENCY OF AEROSOLS IN OCCUPATIONAL AIR SAMPLING SYSTEMS

    Energy Technology Data Exchange (ETDEWEB)

    Hogue, M.; Hadlock, D.; Thompson, M.; Farfan, E.

    2013-11-12

    This report will present hand calculations for transport efficiency based on aspiration efficiency and particle deposition losses. Because the hand calculations become long and tedious, especially for lognormal distributions of aerosols, an R script (R 2011) will be provided for each element examined. Calculations are provided for the most common elements in a remote air sampling system, including a thin-walled probe in ambient air, straight tubing, bends and a sample housing. One popular alternative approach would be to put such calculations in a spreadsheet, a thorough version of which is shared by Paul Baron via the Aerocalc spreadsheet (Baron 2012). To provide greater transparency and to avoid common spreadsheet vulnerabilities to errors (Burns 2012), this report uses R. The particle size is based on the concept of activity median aerodynamic diameter (AMAD). The AMAD is a particle size in an aerosol where fifty percent of the activity in the aerosol is associated with particles of aerodynamic diameter greater than the AMAD. This concept allows for the simplification of transport efficiency calculations where all particles are treated as spheres with the density of water (1g cm-3). In reality, particle densities depend on the actual material involved. Particle geometries can be very complicated. Dynamic shape factors are provided by Hinds (Hinds 1999). Some example factors are: 1.00 for a sphere, 1.08 for a cube, 1.68 for a long cylinder (10 times as long as it is wide), 1.05 to 1.11 for bituminous coal, 1.57 for sand and 1.88 for talc. Revision 1 is made to correct an error in the original version of this report. The particle distributions are based on activity weighting of particles rather than based on the number of particles of each size. Therefore, the mass correction made in the original version is removed from the text and the calculations. Results affected by the change are updated.

  11. Sample preparation of Mycobacterium tuberculosis extracts for nuclear magnetic resonance metabolomic studies.

    Science.gov (United States)

    Zinniel, Denise K; Fenton, Robert J; Halouska, Steven; Powers, Robert; Barletta, Raul G

    2012-01-01

    Mycobacterium tuberculosis is a major cause of mortality in human beings on a global scale. The emergence of both multi- (MDR) and extensively-(XDR) drug-resistant strains threatens to derail current disease control efforts. Thus, there is an urgent need to develop drugs and vaccines that are more effective than those currently available. The genome of M. tuberculosis has been known for more than 10 years, yet there are important gaps in our knowledge of gene function and essentiality. Many studies have since used gene expression analysis at both the transcriptomic and proteomic levels to determine the effects of drugs, oxidants, and growth conditions on the global patterns of gene expression. Ultimately, the final response of these changes is reflected in the metabolic composition of the bacterium including a few thousand small molecular weight chemicals. Comparing the metabolic profiles of wild type and mutant strains, either untreated or treated with a particular drug, can effectively allow target identification and may lead to the development of novel inhibitors with anti-tubercular activity. Likewise, the effects of two or more conditions on the metabolome can also be assessed. Nuclear magnetic resonance (NMR) is a powerful technology that is used to identify and quantify metabolic intermediates. In this protocol, procedures for the preparation of M. tuberculosis cell extracts for NMR metabolomic analysis are described. Cell cultures are grown under appropriate conditions and required Biosafety Level 3 containment, harvested, and subjected to mechanical lysis while maintaining cold temperatures to maximize preservation of metabolites. Cell lysates are recovered, filtered sterilized, and stored at ultra-low temperatures. Aliquots from these cell extracts are plated on Middlebrook 7H9 agar for colony-forming units to verify absence of viable cells. Upon two months of incubation at 37 °C, if no viable colonies are observed, samples are removed from the

  12. Embryotoxicity of organic extracts from airborne particulates in ambient air in the chicken embryo

    Energy Technology Data Exchange (ETDEWEB)

    Matsumoto, H.; Kashimoto, T.

    1986-07-01

    A fraction containing polycyclic aromatic hydrocarbons (PAHs), prepared from an organic extract of airborne particulate matter, was separated into nine subfractions by high pressure liquid chromatography (HPLC). The embryotoxicity of each of these fractions was investigated and analysis for PAHs by capillary gas chromatography-mass spectrometry (GC-MS) was performed. The ninth subfraction, with coronene as its main component, had the strongest toxic effects on chicken embryos per m/sup 3/ of air. Of the remaining eight subfractions, three had the greatest toxicity: the second fraction with benzofluoranthenes and benzo(e)pyrene as the main components, the fourth fraction having PAH-estimated compounds in small amounts, and the fifth fraction with indeno(1,2,3-cd)pyrene and benzo(ghi)perylene as the main ingredients had the greatest toxicity. These findings indicate PAHs to be responsible for embryotoxicity but the total amounts were not necessarily proportional to it. For further characterization of toxicity, the effects of each PAH and/or quantification of other embryotoxic compounds possibly present in small amounts should be investigated.

  13. Preparation and evaluation of molecularly imprinted solid-phase micro-extraction fibers for selective extraction of phthalates in an aqueous sample

    International Nuclear Information System (INIS)

    A novel molecularly imprinted polymer (MIP) that was applied to a solid-phase micro-extraction (SPME) device, which could be coupled directly to gas chromatograph and mass spectrometer (GC/MS), was prepared using dibutyl phthalate (DBP) as the template molecule. The characteristics and application of this fiber were investigated. Electron microscope images indicated that the MIP-coated solid-phase micro-extraction (MI-SPME) fibers were homogeneous and porous. The extraction yield of DBP with the MI-SPME fibers was higher than that of the non-imprinted polymer (NIP)-coated SPME (NI-SPME) fibers. The MI-SPME fibers had a higher selectivity to other phthalates that had similar structures as DBP. A method was developed for the determination of phthalates using MI-SPME fibers coupled with GC/MS. The extraction conditions were optimized. Detection limits for the phthalate samples were within the range of 2.17-20.84 ng L-1. The method was applied to five kinds of phthalates dissolved in spiked aqueous samples and resulted in recoveries of up to 94.54-105.34%, respectively. Thus, the MI-SPME fibers are suitable for the extraction of trace phthalates in complicated samples.

  14. Preparation and evaluation of molecularly imprinted solid-phase micro-extraction fibers for selective extraction of phthalates in an aqueous sample

    Energy Technology Data Exchange (ETDEWEB)

    He Juan, E-mail: juanhe@haut.edu.cn [School of Chemistry and Chemical Engineering, Henan University of, Technology, LianHua Road, Zhengzhou 450051 (China); Lv Ruihe; Zhan Haijun; Wang Huizhi; Cheng Jie; Lu Kui; Wang Fengcheng [School of Chemistry and Chemical Engineering, Henan University of, Technology, LianHua Road, Zhengzhou 450051 (China)

    2010-07-26

    A novel molecularly imprinted polymer (MIP) that was applied to a solid-phase micro-extraction (SPME) device, which could be coupled directly to gas chromatograph and mass spectrometer (GC/MS), was prepared using dibutyl phthalate (DBP) as the template molecule. The characteristics and application of this fiber were investigated. Electron microscope images indicated that the MIP-coated solid-phase micro-extraction (MI-SPME) fibers were homogeneous and porous. The extraction yield of DBP with the MI-SPME fibers was higher than that of the non-imprinted polymer (NIP)-coated SPME (NI-SPME) fibers. The MI-SPME fibers had a higher selectivity to other phthalates that had similar structures as DBP. A method was developed for the determination of phthalates using MI-SPME fibers coupled with GC/MS. The extraction conditions were optimized. Detection limits for the phthalate samples were within the range of 2.17-20.84 ng L{sup -1}. The method was applied to five kinds of phthalates dissolved in spiked aqueous samples and resulted in recoveries of up to 94.54-105.34%, respectively. Thus, the MI-SPME fibers are suitable for the extraction of trace phthalates in complicated samples.

  15. A high-precision measurement system for carbon and hydrogen isotopic ratios of atmospheric methane and its application to air samples collected in the western pacific region

    International Nuclear Information System (INIS)

    In order to study temporal and spatial variations of atmospheric CH4 quantitatively, we originally improved a measurement system for carbon and hydrogen isotopic ratios (δ13C and δD) of CH4 to attain high-precision measurements. By analyzing 100 mL aliquots of an ambient air sample, the precision of our system is 0.08 per mille for δ13C and 2.2 per mille for δD (1σ), which are one of the highest precisions reported so far. The system consists mainly of a CH4 preconcentration device and a continuous-flow gas chromatograph isotope ratio mass spectrometer equipped with a combustion furnace and a pyrolysis furnace for measurements of δ13C and δD. The preconcentration trap temperature was maintained at -130 ±1degC during collection of CH4 from the air sample by passing it through the trap, then at -83 ± 1degC while remaining air components such as N2 and O2 except for CH4 escaped, and finally at 100±1degC for CH4 elusion. The isotopic values are measured on a mass spectrometer, relative to respective reference gases. For this study, the δ13C and δD values of the reference gases were calibrated against our primary standards provided by the IAEA: our δ13C primary standards is NBS18, whereas our δD primary standards are V-SMOW and SLAP. To ensure the long-term stability and reproducibility of our measurement system, a calibrated whole air stored in a high-pressure cylinder, which was called 'test gas', was measured at least twice on each day when sample measurements were made. To measure small air samples, such as those extracted from ice cores, we also examined the relation between the sample size and the measured value of δ13C and δD: gradual enrichment of the δ13C occurred with decreasing CH4 content less than 8 nmol whereas no such effect could be seen for the δD. Furthermore, preliminary results of latitudinal distributions of δ13C and δD were discussed along with CH4 concentrations obtained by our shipboard air-sampling program. (author)

  16. A molecularly imprinted polymer for the selective solid-phase extraction of dimethomorph from ginseng samples.

    Science.gov (United States)

    Xu, Xuanwei; Liang, Shuang; Meng, Xinxin; Zhang, Min; Chen, Ying; Zhao, Dan; Li, Yueru

    2015-04-15

    A molecularly imprinted polymer (MIP) was synthesized and evaluated to selectively extract dimethomorph from ginseng samples. Dimethomorph molecularly imprinted polymers with template to monomer molar ratios were contrived and developed via precipitation polymerization employing methacrylic acid as functional monomer, ethylene dimethacrylate as cross-linker and butanone:N-heptane (7:3, v:v)as porogen. The LOD (limit of detection) of this method was 0.002 mg kg(-1), and the LOQ (limit of quantification) was 0.005 mg kg(-1). The different spiked level of ginseng was 0.1 mg kg(-1), 1.0 mg kg(-1), 5.0 mg kg(-1), and the average recovery of dimethomrph was 89.2-91.6%. Under the optimized condition, good linearity was obtained from 0.01 to 5 mg kg(-1) (r(2) ≥ 0.9997) with the relative standard deviations of less than 3.20%. This proposed MISPE-GC procedure eliminated the effect of template leakage on quantitative analysis and could be applied to direct determination of dimethomrph in ginseng samples. PMID:25795323

  17. Precise determination of 13C/12C and CO2 concentration in small samples of soil air by mass spectrometry

    International Nuclear Information System (INIS)

    Studies of soil CO2 concentration and its isotopic composition have been carried out. The sample size of soil air was about 100 cm3 only. The isotope analysis of such small CO2 samples were performed by a dynamic flow mass spectrometer. The air samples were taken from the depth of 10 to 75 cm at two points of a grass field at a distance of a few meters. The measured δ13C values were very consistent for both points ranging from -21.53 to -22.37 per mill, while the corresponding CO2 concentration ranged from 0.24 to 0.55%. (author)

  18. The determination of americium, curium and californium in biological samples by combined solvent extraction-liquid scintillation counting

    International Nuclear Information System (INIS)

    A method has been developed to extract Am, Cm and Cf from ashed biological samples dissolved in 8 M LiN03-10-2 M HN03 into a liquid/scintillation cocktail. This new method reduces tissue and instrument background and allows use of a larger sample for analysis than when using a commercial gelling cocktail. The extractant cocktail is 20% N,N,N-trioctyl-N-methylammonium chloride dissolved in toluene containing the scintillators p-terphenyl and 1,4-bis-2-(5-phenyl-oxazolyl)-benzene. Several different types of biological samples were analyzed and radionuclide recoveries greater than 90% were obtained in all cases. (author)

  19. Determination of 15 isomers of chlorobenzoic acid in soil samples using accelerated sample extraction followed by liquid chromatography

    Czech Academy of Sciences Publication Activity Database

    Křesinová, Zdena; Muzikář, Milan; Olšovská, Jana; Cajthaml, Tomáš

    2011-01-01

    Roč. 84, č. 4 (2011), s. 1141-1147. ISSN 0039-9140 R&D Projects: GA MŠk 2B06156; GA ČR GA525/09/1058 Institutional research plan: CEZ:AV0Z50200510 Keywords : Chlorobenzoic acid * hplc * Accelerated solvent extraction Subject RIV: EE - Microbiology, Virology Impact factor: 3.794, year: 2011

  20. Hollow-fiber micro-extraction combined with HPLC for the determination of sitagliptin in urine samples

    Directory of Open Access Journals (Sweden)

    Rezaee Raheme

    2015-01-01

    Full Text Available This study successfully developed a three-phase hollow-fiber liquid phase micro extraction coupled with high performance liquid chromatography for determination of trace levels of an anti-diabetic drug, sitagliptin (STG, in urine samples. Sitagliptin was extracted from 15 mL of the basic sample solution with a pH of 8.5 into an organic extracting solvent (n-octanol impregnated in the pores of a hollow fiber and then back extracted into an acidified aqueous solution in the lumen of the hollow fiber with a pH of 3. After extraction, 20 µL of the acceptor phase was injected into HPLC. In order to obtain high extraction efficiency, the parameters affecting the HF-LPME including pH of the source and receiving phases, type of organic phase, ionic strength, stirring rate, extraction time, the volume ratio of donor phase to acceptor phase and temperature were studied and optimized. Under the optimized conditions, enrichment factors up to 88 were achieved and the relative standard deviation of the method was in the range of 3 % to 6%. The results indicated that HF-LPME method has an excellent clean-up capacity and a high preconcentration factor and can serve as a simple and sensitive method for monitoring the drug in the urine samples.

  1. Uncertainties in Air Exchange using Continuous-Injection, Long-Term Sampling Tracer-Gas Methods

    Energy Technology Data Exchange (ETDEWEB)

    Sherman, Max H.; Walker, Iain S.; Lunden, Melissa M.

    2013-12-01

    The PerFluorocarbon Tracer (PFT) method is a low-cost approach commonly used for measuring air exchange in buildings using tracer gases. It is a specific application of the more general Continuous-Injection, Long-Term Sampling (CILTS) method. The technique is widely used but there has been little work on understanding the uncertainties (both precision and bias) associated with its use, particularly given that it is typically deployed by untrained or lightly trained people to minimize experimental costs. In this article we will conduct a first-principles error analysis to estimate the uncertainties and then compare that analysis to CILTS measurements that were over-sampled, through the use of multiple tracers and emitter and sampler distribution patterns, in three houses. We find that the CILTS method can have an overall uncertainty of 10-15percent in ideal circumstances, but that even in highly controlled field experiments done by trained experimenters expected uncertainties are about 20percent. In addition, there are many field conditions (such as open windows) where CILTS is not likely to provide any quantitative data. Even avoiding the worst situations of assumption violations CILTS should be considered as having a something like a ?factor of two? uncertainty for the broad field trials that it is typically used in. We provide guidance on how to deploy CILTS and design the experiment to minimize uncertainties.

  2. Sampling of power plant stacks for air toxic emissions: Final report for Phases 1 and 2

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1995-04-28

    A test program to collect and analyze size-fractionated stack gas particulate samples for selected inorganic hazardous air pollutants (HAPs) was conducted . Specific goals of the program are (1) the collection of one-gram quantities of size-fractionated stack gas particulate matter for bulk (total) and surface chemical characterization, and (2) the determination of the relationship between particle size, bulk and surface (leachable) composition, and unit load. The information obtained from this program identifies the effects of unit load, particle size, and wet FGD system operation on the relative toxicological effects of exposure to particulate emissions. Field testing was conducted in two phases. The Phase I field program was performed over the period of August 24 through September 20, 1992, at the Tennessee Valley Authority Widows Creek Unit 8 Power Station, located near Stevenson (Jackson County), Alabama, on the Tennessee River. Sampling activities for Phase II were conducted from September 11 through October 14, 1993. Widows Creek Unit 8 is a 575-megawatt plant that uses bituminous coal averaging 3.7% sulfur and 13% ash. Downstream of the boiler, a venture wet scrubbing system is used for control of both sulfur dioxide and particulate emissions. There is no electrostatic precipitator (ESP) in this system. This system is atypical and represents only about 5% of the US utility industry. However, this site was chosen for this study because of the lack of information available for this particulate emission control system.

  3. Sample preparation of sewage sludge and soil samples for the determination of polycyclic aromatic hydrocarbons based on one-pot microwave-assisted saponification and extraction.

    Science.gov (United States)

    Pena, M Teresa; Pensado, Luis; Casais, M Carmen; Mejuto, M Carmen; Cela, Rafael

    2007-04-01

    A microwave-assisted sample preparation (MASP) procedure was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sewage sludge and soil samples. The procedure involved the simultaneous microwave-assisted extraction of PAHs with n-hexane and the hydrolysis of samples with methanolic potassium hydroxide. Because of the complex nature of the samples, the extracts were submitted to further cleaning with silica and Florisil solid-phase extraction cartridges connected in series. Naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[e]pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene, benzo[g,h,i]perylene, and indeno[1,2,3-cd]pyrene, were considered in the study. Quantification limits obtained for all of these compounds (between 0.4 and 14.8 microg kg(-1) dry mass) were well below of the limits recommended in the USA and EU. Overall recovery values ranged from 60 to 100%, with most losses being due to evaporation in the solvent exchange stages of the procedure, although excellent extraction recoveries were obtained. Validation of the accuracy was carried out with BCR-088 (sewage sludge) and BCR-524 (contaminated industrial soil) reference materials. PMID:17268774

  4. Sample preparation of sewage sludge and soil samples for the determination of polycyclic aromatic hydrocarbons based on one-pot microwave-assisted saponification and extraction

    Energy Technology Data Exchange (ETDEWEB)

    Pena, M.T.; Pensado, Luis; Casais, M.C.; Mejuto, M.C.; Cela, Rafael [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia. Instituto de Investigacion y Analisis Alimentario, Santiago de Compostela (Spain)

    2007-04-15

    A microwave-assisted sample preparation (MASP) procedure was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sewage sludge and soil samples. The procedure involved the simultaneous microwave-assisted extraction of PAHs with n-hexane and the hydrolysis of samples with methanolic potassium hydroxide. Because of the complex nature of the samples, the extracts were submitted to further cleaning with silica and Florisil solid-phase extraction cartridges connected in series. Naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[e]pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene, benzo[g,h,i]perylene, and indeno[1,2,3-cd]pyrene, were considered in the study. Quantification limits obtained for all of these compounds (between 0.4 and 14.8 {mu}g kg{sup -1} dry mass) were well below of the limits recommended in the USA and EU. Overall recovery values ranged from 60 to 100%, with most losses being due to evaporation in the solvent exchange stages of the procedure, although excellent extraction recoveries were obtained. Validation of the accuracy was carried out with BCR-088 (sewage sludge) and BCR-524 (contaminated industrial soil) reference materials. (orig.)

  5. A nanoparticle-based solid-phase extraction procedure followed by spectrofluorimetry to determine carbaryl in different water samples

    Energy Technology Data Exchange (ETDEWEB)

    Tabrizi, Ahad Bavili, E-mail: a.bavili@tbzmed.ac.ir, E-mail: abavilitabrizia@gmail.com [Biotechnology Research Center, Tabriz University of Medical Sciences, Tabriz (Iran, Islamic Republic of); Rashidi, Mohammad Reza [Research Center for Pharmaceutical Nanotechnology, Tabriz University of Medical Sciences, Tabriz, (Iran, Islamic Republic of); Ostadi, Hadi [Department of Chemistry, Payam-e-noor University, Ardabil Branch, Ardabil (Iran, Islamic Republic of)

    2014-04-15

    In this study, a new method based on Fe{sub 3}O{sub 4} magnetite nanoparticles (MNPs) has been developed for the extraction, preconcentration and determination of trace amounts of carbaryl from environmental water samples. Fe{sub 3}O{sub 4} MNPs were synthesized and modified by the surfactant sodium dodecyl sulfate (SDS), then successfully applied for the extraction of carbaryl and its determination by spectrofluorimetry. Main factors affecting the adsolubilization of carbaryl such as the amount of SDS, pH value, standing time, desorption solvent and maximal extraction volume were optimized. Under the selected conditions, carbaryl could be quantitatively extracted. Acceptable recoveries (84.5-91.9%) and relative standard deviations (6.2%) were achieved in analyzing spiked water samples. A concentration factor of 20 was achieved by the extraction of 100 mL of environmental water samples. The limit of detection and quantification were found to be 2.1 and 6.9 μg L{sup -1}, respectively. The proposed method was successfully applied for the extraction and determination of carbaryl in environmental water samples. (author)

  6. A nanoparticle-based solid-phase extraction procedure followed by spectrofluorimetry to determine carbaryl in different water samples

    International Nuclear Information System (INIS)

    In this study, a new method based on Fe3O4 magnetite nanoparticles (MNPs) has been developed for the extraction, preconcentration and determination of trace amounts of carbaryl from environmental water samples. Fe3O4 MNPs were synthesized and modified by the surfactant sodium dodecyl sulfate (SDS), then successfully applied for the extraction of carbaryl and its determination by spectrofluorimetry. Main factors affecting the adsolubilization of carbaryl such as the amount of SDS, pH value, standing time, desorption solvent and maximal extraction volume were optimized. Under the selected conditions, carbaryl could be quantitatively extracted. Acceptable recoveries (84.5-91.9%) and relative standard deviations (6.2%) were achieved in analyzing spiked water samples. A concentration factor of 20 was achieved by the extraction of 100 mL of environmental water samples. The limit of detection and quantification were found to be 2.1 and 6.9 μg L-1, respectively. The proposed method was successfully applied for the extraction and determination of carbaryl in environmental water samples. (author)

  7. Summertime PAH assembly in Mediterranean air: the Herceg Novi sampling station as an example

    Directory of Open Access Journals (Sweden)

    VLADIMIR Z. JOVANOVIC

    2007-02-01

    Full Text Available The results of an analysis of the total suspended particles (TSP, total solvent organic extracts (TSOE, and polycyclic aromatic hydrocarbons (PAHs in aerosol samples collected from the atmosphere of Herceg Novi from 17th June to 15th September in 1998 and 1999 are presented. The TSP and TSOE concentrations were determined by the standard gravimetric method, whereas the PAHs from the organic part of the aerosol were analysed by the GC-MS method. The difference found in the TSP and TSOE contents between the two consecutive years (before and after the bombing of Yugoslavia was attributed to changes in the intensity and origin of emissions from dominant sources, specific to the summer period of this region. The content and nature of the PAHs identified in the samples of 1998 and 1999 were also different, indicating the significance of traffic as the source of PAHs, which was of significantly lower intensity in 1999 (immediately after the war due to the lower influx of tourists. Factor analysis showed that the PAH distribution at the measuring site in 1999 was largely determined by meteorological parameters, mainly by the average daily temperature and wind direction. In 1998, the dominant impact on the PAH distribution was attributed to traffic, both local and from a wider region, without an explicit impact of meteorological parameters.

  8. Passive air sampler as a tool for long-term air pollution monitoring: Part 2. Air genotoxic potency screening assessment

    International Nuclear Information System (INIS)

    The capability of passive air sampling to be employed in the evaluation of direct genotoxicity of ambient air samples was assessed. Genotoxic effects of the total extracts from the polyurethane foam filters exposed for 28 days during a regional passive air sampling campaign were investigated. Twenty sampling sites were selected in Brno city on the area of approximately 20 x 20 km in October and November 2004. Brno is the second largest city of the Czech Republic, highly industrialized with approximately 370,000 of permanent inhabitants. The levels of PAHs, PCBs, and chlorinated pesticides were determined in all samples. Fraction of each extract was also assayed in the bacterial genotoxicity test using Escherichia coli sulA::lacZ. Complete dose-response relationships of the air extracts were determined. The statistical analysis showed significant correlation between observed biological effects and PAHs concentrations in samples. - Extracts from passive air samples can be used to assess genotoxic potency

  9. Optimization and evaluation of metabolite extraction protocols for untargeted metabolic profiling of liver samples by UPLC-MS.

    Science.gov (United States)

    Masson, Perrine; Alves, Alexessander Couto; Ebbels, Timothy M D; Nicholson, Jeremy K; Want, Elizabeth J

    2010-09-15

    A series of six protocols were evaluated for UPLC-MS based untargeted metabolic profiling of liver extracts in terms of reproducibility and number of metabolite features obtained. These protocols, designed to extract both polar and nonpolar metabolites, were based on (i) a two stage extraction approach or (ii) a simultaneous extraction in a biphasic mixture, employing different volumes and combinations of extraction and resuspension solvents. A multivariate statistical strategy was developed to allow comparison of the multidimensional variation between the methods. The optimal protocol for profiling both polar and nonpolar metabolites was found to be an aqueous extraction with methanol/water followed by an organic extraction with dichloromethane/methanol, with resuspension of the dried extracts in methanol/water before UPLC-MS analysis. This protocol resulted in a median CV of feature intensities among experimental replicates of data demonstrate the robustness of the proposed protocol for extracting metabolites from liver samples and make it well suited for untargeted liver profiling in studies exploring xenobiotic hepatotoxicity and clinical investigations of liver disease. The generic nature of this protocol facilitates its application to other tissues, for example, brain or lung, enhancing its utility in clinical and toxicological studies. PMID:20715759

  10. Cryogenic separation of oxygen-argon mixture in natural air samples for isotopic and molecular ratios

    Science.gov (United States)

    Habeeb Rahman, Keedakkadan; Abe, Osamu

    2014-05-01

    The discovery of mass independent isotope fractionation in oxygen during the formation of ozone in the stratosphere has initiated a wide application in isotope geochemistry field. Separation of oxygen-argon mixture has become the foundation of high precision analysis of Δ17O and δ(O2/Ar) for geochemical applications. Here we present precise and simplified cryogenic separation of argon oxygen mixture from the atmospheric and dissolved air using 30/60 mesh 5A molecular sieve zeolite. A pioneer study of this method was conducted by Thiemens and Meagher in 1984. The column which is made of glass tube contains about 1.1 grams of molecular sieve zeolite and both ends of column was filled with glass wools. The experimental set up was tested for different combination of molecular sieves and slurry temperatures. We found the most efficient condition for the separation was at a column temperature of -103°C. For complete transfer of O2 and Ar mixture usually takes in 15-20 minutes time. The isotopic ratios of oxygen were analyzed using mass spectrometer (Thermo Fischer Delta Plus) relative to reference oxygen-argon mixture at 3V of m/z 32 for both sample and reference side. The signals of m/z 28, 32, and 40 were measured by dynamically to determine oxygen -argon ratio and to check nitrogen contamination. Repeated measurements of atmospheric air yielded a reproducibility (SE n=80) of 0.006, 0.004 and 0.19‰ for δ17O, δ18O and δO2/Ar respectively. The isotopic and molecular fractionation of argon- oxygen mixture during gas adsorption and desorption while using molecular sieve under liquid nitrogen temperature was studied. We have established a linear relationship governing the effect of 13X and 5A molecular sieves on molecular fractionation. And suggested the use of single 1/8" pellet 13X molecular sieve provided a negligible fractionation.

  11. Feasibility of corona discharge ion mobility spectrometry for direct analysis of samples extracted by dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Jafari, Mohammad T; Riahi, Farhad

    2014-05-23

    The capability of corona discharge ionization ion mobility spectrometry (CD-IMS) for direct analysis of the samples extracted by dispersive liquid-liquid microextraction (DLLME) was investigated and evaluated, for the first time. To that end, an appropriate new injection port was designed and constructed, resulting in possibility of direct injection of the known sample volume, without tedious sample preparation steps (e.g. derivatization, solvent evaporation, and re-solving in another solvent…). Malathion as a test compound was extracted from different matrices by a rapid and convenient DLLME method. The positive ion mobility spectra of the extracted malathion were obtained after direct injection of carbon tetrachloride or methanol solutions. The analyte responses were compared and the statistical results revealed the feasibility of direct analysis of the extracted samples in carbon tetrachloride, resulting in a convenient methodology. The coupled method of DLLME-CD-IMS was exhaustively validated in terms of sensitivity, dynamic range, recovery, and enrichment factor. Finally, various real samples of apple, river and underground water were analyzed, all verifying the feasibility and success of the proposed method for the easy extraction of the analyte using DLLME separation before the direct analysis by CD-IMS. PMID:24742534

  12. Indoor Air Quality in Selected Samples of Primary Schools in Kuala Terengganu, Malaysia

    OpenAIRE

    Marzuki Ismail

    2010-01-01

    Studies have found out that indoor air quality affects human especially children and the elderly more compared to ambient atmospheric air. This study aims to investigate indoor air pollutants concentration in selected vernacular schools with different surrounding human activities in Kuala Terengganu, the administrative and commercial center of Terengganu state. Failure to identify and establish indoor air pollution status can increase the chance of long-term and short-term health problems for...

  13. Occurrence and quantitative microbial risk assessment of Cryptosporidium and Giardia in soil and air samples

    Directory of Open Access Journals (Sweden)

    Ana Paola Balderrama-Carmona

    2014-09-01

    Conclusions: Soil and air inhalation and/or ingestion are important vehicles for these parasites. To our knowledge, the results obtained in the present study represent the first QMRAs for cryptosporidiosis and giardiasis due to soil and air inhalation/ingestion in Mexico. In addition, this is the first evidence of the microbial air quality around these parasites in rural zones.

  14. Characterization of citrus pectin samples extracted under different conditions: influence of acid type and pH of extraction

    OpenAIRE

    Kaya, Merve; Sousa, Antonio G.; Crepeau, Marie-Jeanne; Sorensen, Susanne O.; Ralet, Marie-Christine

    2014-01-01

    Background and Aims Pectin is a complex macromolecule, the fine structure of which is influenced by many factors. It is used as a gelling, thickening and emulsifying agent in a wide range of applications, from food to pharmaceutical products. Current industrial pectin extraction processes are based on fruit peel, a waste product from the juicing industry, in which thousands of tons of citrus are processed worldwide every year. This study examines how pectin components vary in relation to the ...

  15. Utilizing the partitioning properties of silicone for the passive sampling of polychlorinated biphenyls (PCBs) in indoor air.

    Science.gov (United States)

    Vorkamp, Katrin; Odsbjerg, Lisbeth; Langeland, Majbrith; Mayer, Philipp

    2016-10-01

    The former use of polychlorinated biphenyls (PCBs) in construction materials can lead to elevated indoor air concentrations. We studied the partitioning of PCB congeners between indoor air and silicone with a view to establish passive sampling of PCBs. The release of PCB congeners from silicone followed first order kinetics and confirmed air-side rate-limited mass transfer. Logarithmic elimination rate constants decreased linearly with the logKOA values of the PCB congeners, but varied in a non-linear way with air velocity. Linear uptake of PCBs was found for silicone disks (0.5 mm thickness) in a petri dish, while PCBs reached equilibrium in silicone-coated paper sheets (0.001 mm silicone on each side) exposed to indoor air for 1-2 weeks. The ratios of equilibrium concentrations in silicone and conventionally measured air concentrations were roughly comparable with silicone-air partition coefficients, but further research is required for the determination of silicone-air partition coefficients. Avoiding performance reference compounds (PRCs) because of the indoor setting, the two formats were calibrated against conventional active measurements. Comparisons of air concentrations derived from active and kinetic passive sampling showed a divergence by factors of 2.4 and 2.0 (median values) for the petri dishes and the silicone-coated paper, respectively. With promising results for sensitivity and precision, the calibration of kinetic passive samplers remains the main challenge and will need suitable, non-hazardous PRCs. Equilibrium sampling indicated promising alternatives. PMID:27389945

  16. Arsenic fractionation by sequential extractions in standard reference materials and industrially contaminated soil samples: Applicability and drawbacks

    Energy Technology Data Exchange (ETDEWEB)

    Herreweghe, S. van; Swennen, R. [Fysico-Chemische Geologie, Heverlee (Belgium)

    2003-07-01

    Availability mobility (phyto)toxycity and potential risk of contaminants is strongly affected by the manner of appearance of elements, the so-called speciation. Operational fractionation methods like sequential extractions have been applied for a long time to determine the solid phase speciation of heavy metals since direct determination of specific chemical compounds can not always be easily achieved. The aim of this research was to assess the applicability of sequential extractions on highly contaminated soils where arsenic is also present as discrete As-bearing minerals. Sequential extractions are mostly developed to fractionate heavy metals occurring in trace amounts and their applicability on highly contaminated samples remains insufficiently studied. There was, furthermore, a need to evaluate sequential extraction schemes specifically focussing on metalloid element extraction such as arsenic. (orig.)

  17. Solid-phase extraction of flavonoids in honey samples using carbamate-embedded triacontyl-modified silica sorbent.

    Science.gov (United States)

    Liu, Houmei; Zhang, Mingliang; Guo, Yong; Qiu, Hongdeng

    2016-08-01

    In this study, carbamate-embedded triacontyl-modified silica (Sil-CBM-C30) is successfully prepared and used as an efficient sorbent for solid-phase extraction. The extraction performance of the resultant sorbent is evaluated with five flavonoids including myricetin, quercetin, luteolin, kaempferol and isorhamnetin. Main parameters, which affect extraction efficiencies, are carefully investigated and optimized. Comparative experiments between Sil-CBM-C30 and commercial C18 sorbents indicate that the extraction efficiencies of the former one surpass the latter one. The modification of carbamate-embedded triacontyl group on surface of silica causes analytes extracted by hydrophobic, hydrogen bonding and π-π interactions. Under optimal conditions, good linearities and satisfied LODs and LOQs are achieved. The SPE-HPLC-DAD method is successfully developed and applied for the honey sample analysis. PMID:26988475

  18. Performance verification of the Maxwell 16 Instrument and DNA IQ Reference Sample Kit for automated DNA extraction of known reference samples.

    Science.gov (United States)

    Krnajski, Z; Geering, S; Steadman, S

    2007-12-01

    Advances in automation have been made for a number of processes conducted in the forensic DNA laboratory. However, because most robotic systems are designed for high-throughput laboratories batching large numbers of samples, smaller laboratories are left with a limited number of cost-effective options for employing automation. The Maxwell 16 Instrument and DNA IQ Reference Sample Kit marketed by Promega are designed for rapid, automated purification of DNA extracts from sample sets consisting of sixteen or fewer samples. Because the system is based on DNA capture by paramagnetic particles with maximum binding capacity, it is designed to generate extracts with yield consistency. The studies herein enabled evaluation of STR profile concordance, consistency of yield, and cross-contamination performance for the Maxwell 16 Instrument. Results indicate that the system performs suitably for streamlining the process of extracting known reference samples generally used for forensic DNA analysis and has many advantages in a small or moderate-sized laboratory environment. PMID:25869266

  19. Determination of Antioxidant Flavonoids in Sudanese Honey Samples by Solid Phase Extraction and High Performance Liquid Chromatography

    OpenAIRE

    Suzan Zein Alabdeen Makawi; Elrasheed Ahmed Gadkariem; Saad Mohamed Hussein Ayoub

    2009-01-01

    Flavonoids were extracted by solid phase extraction (SPE) from seven floral honey samples of different botanical origin from different regions of Sudan. The flavonoids were determined by high performance liquid chromatography (HPLC) technique using photo diode array detector (PDA). An isocratic and gradient systems for the resolution, identification and quantification of five flavonoids, namely; quercetin, kaempferol, apigenin, hesperetin and isorhamnetin, were developed. Although the isocrat...

  20. Aircraft Cabin Air Sampling Study; Part 2 of the Final Report

    OpenAIRE

    Crump, Derrick; Harrison, Paul; Walton, Christopher

    2011-01-01

    This is the second part of the report on aircraft cabin air quality prepared by Cranfield University for the Department for Transport. The study was set up in light of concerns about possible adverse impacts on the health and well-being of air crew resulting from exposure to substances in cabin air. Part 1 of the report describes in detail the methodology used in the study, summarises the results obtained and assesses cabin air quality against available exposure limits and the quality of air ...

  1. Magnetic nanoparticles with hydrophobicity and hydrophilicity for solid-phase extraction of polycyclic aromatic hydrocarbons from environmental water samples.

    Science.gov (United States)

    Xue, Shu-Wen; Tang, Min-Qiong; Xu, Li; Shi, Zhi-guo

    2015-09-11

    Magnetic nanoparticles (MNPs) featured with divinylbenzene (DVB) and sulfonate functionalities (Fe3O4-DVB-SO3(-)) were prepared via "thiol-ene" click chemistry. The hydrophobic DVB moieties were dedicated for extraction while the hydrophilic sulfonate groups were designed for dispersing the MNPs in aqueous sample solution. Thus, the specially designed material could ensure operational convenience and improve reproducibility during extraction. The application of the material was demonstrated by the extraction of polycyclic aromatic hydrocarbons (PAHs) from environmental water samples followed by gas chromatography-mass spectrometric analysis. The main factors influencing the extraction, including the type of the desorption solvent, the agitation mode, the amount of MNPs, extraction and desorption time and salt addition in sample solution, were investigated in detail. Under the optimized conditions, the proposed method showed satisfactory reproducibility with intra-day and inter-day relative standard deviations less than 16.5% and 21.2%, and low limits of detection of 1.1pgmL(-1), 0.8pgmL(-1), 1.1pgmL(-1), 1.4pgmL(-1), 0.6pgmL(-1), 2.1pgmL(-1) and 0.7pgmL(-1) for naphthalene, acenaphthene, fluorine, phenanthrene, anthracene, fluoranthene and pyrene, respectively. The developed method was also successfully used for determination of the PAHs in genuine lake and river environmental water samples by standard addition method. All the studied PAHs were detected in these waters with comparable results by the standard liquid-liquid extraction method. The developed MNPs with dual property of hydrophobicity and hydrophilicity were suitable for the treatment of water samples. The magnetic solid phase extraction based on this material was reliable and convenient. It has great potential in the preconcentration of trace analytes in complex matrix. PMID:26260841

  2. Determination of vanadium in steel and geological samples by its extraction and spectrophotometric determination using 2,3-dihydroxynaphthalene

    International Nuclear Information System (INIS)

    A new and simple method for extraction and spectrophotometric determination of vanadium has been described. Iron has been removed from the sample solution by its prior extraction with MIBK from concentrated HCl medium (∼6 M). Vanadium has been determined in the form of a colored complex with 2,3-dihydroxynaphthalene after its extraction into MIBK. The method is at least 5 fold more sensitive to BPHA method. The molar absorptivity of the complex at 530 nm being 1.5 x 104 Lmol-1 cm-1. For samples having >5 fold excess concentration of TiO2, a prior separation of TiO2 as its (Ti (OH) (HND)3) complex is a must. The method has been successfully applied to different rock, soil and steel samples. (author)

  3. Determination of Chlorophenols in Water Samples Using Solid-Phase Extraction Enrichment Procedure and Gas Chromatography Analysis.

    Science.gov (United States)

    Ben Hassine, S; Hammami, B; Touil, S; Driss, M R

    2015-11-01

    Solid-phase extraction (SPE) procedure followed by derivatization and gas chromatography electron capture detection was evaluated for the determination of trace amounts of chlorophenols (CPs) in waters samples. Different parameters affecting extraction efficiency such as, volume of elution solvent, volume and pH of water sample, quantity of sorbent phase were studied and optimized. SPE was carried out on polystyrene-divinylbenzene (Bond Elut ENV) and high recoveries were obtained using 1000 mg of this cartridge for the treatment of 500 mL of acidified water sample. The described method was then tested on spiked tap, mineral, ground and surface water samples. The overall procedure provided limits of detection lower than 20 ng L(-1), recoveries of 70%-106% and an enrichment factor of 500 for the examined CPs in 500 mL water samples. Among the studied compounds, pentachlorophenol was detected in tap water at a concentration level of 0.06 µg L(-1). PMID:26067701

  4. Fluorometric determination of nonylphenol in water samples enriched with zirconium doped titanium dioxide nanotubes solid phase extraction

    Institute of Scientific and Technical Information of China (English)

    Xian Fa Su; Xin Ning Zhao; Guo Hong Xie; Qing Xiang Zhou

    2012-01-01

    This paper developed a fluorometric method for the sensitive determination of nonylphenol in water samples by preconcentration with zirconium doped titanium dioxide nanotubes solid phase extraction.The parameters on extraction that would influence the enrichment performance such as the kind and volume of eluent,sample pH,sample flow rate,and sample volume were optimized in detail.Under the optimal conditions,the proposed method provided an excellent linear range of 1-150 μg/L and good LOD of 0.076 μg/L.The relative standard deviation (RSD,n =6) was 2.8%.Proposed method was also used for the analysis of real water samples and the spiked recoveries were satisfied in the range of 98.7-103%.

  5. Determination of cadmium in real water samples by flame atomic absorption spectrometry after cloud point extraction

    International Nuclear Information System (INIS)

    Water pollution is a global threat and it is the leading world wide cause of death and diseases. The awareness of the potential danger posed by heavy metals to the ecosystems and in particular to human health has grown tremendously in the past decades. Separation and preconcentration procedures are considered of great importance in analytical and environmental chemistry. Cloud point is one of the most reliable and sophisticated separation methods for determination of traces quantities of heavy metals. Cloud point methodology was successfully employed for preconcentration of trace quantities of cadmium prior to their determination by flame atomic absorption spectrometry (FAAS). The metals react with 8-hydroxquinoline in a surfactant Triton X-114 medium. The following parameters such as pH, concentration of the reagent and Triton X-114, equilibrating temperature and centrifuging time were evaluated and optimized to enhance the sensitivity and extraction efficiency of the proposed method. Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation and the cadmium content was measured by FAAS. The validation of the procedure was carried out by spiking addition methods. The method was applied for determination of Cd in water samples of different ecosystems (lake and river). (author)

  6. Training in metabolomics research. I. Designing the experiment, collecting and extracting samples and generating metabolomics data

    Science.gov (United States)

    Barnes, Stephen; Benton, H. Paul; Casazza, Krista; Cooper, Sara J.; Cui, Xiangqin; Du, Xiuxia; Engler, Jeffrey; Kabarowski, Janusz H.; Li, Shuzhao; Pathmasiri, Wimal; Prasain, Jeevan K.; Renfrow, Matthew B.; Tiwari, Hemant K.

    2016-01-01

    The study of metabolism has had a long history. Metabolomics, a systems biology discipline representing analysis of known and unknown pathways of metabolism, has grown tremendously over the past 20 years. Because of its comprehensive nature, metabolomics requires careful consideration of the question(s) being asked, the scale needed to answer the question(s), collection and storage of the sample specimens, methods for extraction of the metabolites from biological matrices, the analytical method(s) to be employed and the quality control of the analyses, how collected data are correlated, the statistical methods to determine metabolites undergoing significant change, putative identification of metabolites and the use of stable isotopes to aid in verifying metabolite identity and establishing pathway connections and fluxes. The National Institutes of Health Common Fund Metabolomics Program was established in 2012 to stimulate interest in the approaches and technologies of metabolomics. To deliver one of the program’s goals, the University of Alabama at Birmingham has hosted an annual 4-day short course in metabolomics for faculty, postdoctoral fellows and graduate students from national and international institutions. This paper is the first part of a summary of the training materials presented in the course to be used as a resource for all those embarking on metabolomics research. PMID:27434804

  7. Training in metabolomics research. I. Designing the experiment, collecting and extracting samples and generating metabolomics data.

    Science.gov (United States)

    Barnes, Stephen; Benton, H Paul; Casazza, Krista; Cooper, Sara J; Cui, Xiangqin; Du, Xiuxia; Engler, Jeffrey; Kabarowski, Janusz H; Li, Shuzhao; Pathmasiri, Wimal; Prasain, Jeevan K; Renfrow, Matthew B; Tiwari, Hemant K

    2016-07-01

    The study of metabolism has had a long history. Metabolomics, a systems biology discipline representing analysis of known and unknown pathways of metabolism, has grown tremendously over the past 20 years. Because of its comprehensive nature, metabolomics requires careful consideration of the question(s) being asked, the scale needed to answer the question(s), collection and storage of the sample specimens, methods for extraction of the metabolites from biological matrices, the analytical method(s) to be employed and the quality control of the analyses, how collected data are correlated, the statistical methods to determine metabolites undergoing significant change, putative identification of metabolites and the use of stable isotopes to aid in verifying metabolite identity and establishing pathway connections and fluxes. The National Institutes of Health Common Fund Metabolomics Program was established in 2012 to stimulate interest in the approaches and technologies of metabolomics. To deliver one of the program's goals, the University of Alabama at Birmingham has hosted an annual 4-day short course in metabolomics for faculty, postdoctoral fellows and graduate students from national and international institutions. This paper is the first part of a summary of the training materials presented in the course to be used as a resource for all those embarking on metabolomics research. The complete set of training materials including slide sets and videos can be viewed at http://www.uab.edu/proteomics/metabolomics/workshop/workshop_june_2015.php. Copyright © 2016 John Wiley & Sons, Ltd. PMID:27434804

  8. Development of a Cloud-Point Extraction Method for Cobalt Determination in Natural Water Samples

    Directory of Open Access Journals (Sweden)

    Mohammad Reza Jamali

    2013-01-01

    Full Text Available A new, simple, and versatile cloud-point extraction (CPE methodology has been developed for the separation and preconcentration of cobalt. The cobalt ions in the initial aqueous solution were complexed with 4-Benzylpiperidinedithiocarbamate, and Triton X-114 was added as surfactant. Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation, and the cobalt content was measured by flame atomic absorption spectrometry. The main factors affecting CPE procedure, such as pH, concentration of ligand, amount of Triton X-114, equilibrium temperature, and incubation time were investigated and optimized. Under the optimal conditions, the limit of detection (LOD for cobalt was 0.5 μg L-1, with sensitivity enhancement factor (EF of 67. Calibration curve was linear in the range of 2–150 μg L-1, and relative standard deviation was 3.2% (c=100 μg L-1; n=10. The proposed method was applied to the determination of trace cobalt in real water samples with satisfactory analytical results.

  9. Sequential extraction of platinum, cisplatin and carboplatin from environmental samples and pre-concentration/separation using vesicular coacervative extraction and determination by continuum source ETAAS.

    Science.gov (United States)

    Meeravali, Noorbasha N; Madhavi, K; Manjusha, R; Kumar, Sunil Jai

    2014-01-01

    A sequential extraction procedure is developed for the separation of trace levels of hexachloroplatinate, cisplatin and carboplatin from soil, which are then, pre-concentrated using a vesicular coacervative cloud point extraction method prior to their determination as platinum by continuum source ETAAS. Sequential extraction of carboplatin, cisplatin and hexachloroplatinate from a specific red soil is achieved by using the 20% HCl, aqua regia at room temperature and by combination of aqua regia and HF with microwave digestion, respectively. The pre-concentration of these species from the extracted solutions is based on the formation of extractable hydrophobic complexes of PtCl₆(2-) anionic species with free cationic head groups solubilizing sites of the Triton X-114 co-surfactant stabilized TOMAC (tri-octyl methyl ammonium chloride) vesicles through electrostatic attraction. This process separates the platinum from bulk aqueous solution into a small vesicular rich phase. The parameters affecting the extraction procedures are optimized. Under the optimized conditions, the achieved pre-concentration factor is 20 and detection limit is 0.5 ng g(-1) for soil and 0.02 ng mL(-1) for water samples. The spiked recoveries of hexachloroplatinate, cisplatin and carboplatin in water and soil extracts in the vesicular coacervative extraction are in the range of 96-102% at 0.5-1 ng mL(-1) with relative standard deviation of 1-3%. The accuracy of the method for platinum determination is evaluated by analyzing CCRMP PTC-1a copper-nickel sulfide concentrate and BCR 723 road dust certified reference materials and the obtained results agreed with the certified values with 95% confidence level of student t-test. The results were also compared to mixed-micelle (MM)-CPE method reported in the literature. PMID:24274268

  10. Air sampling procedures to evaluate microbial contamination: a comparison between active and passive methods in operating theatres

    Directory of Open Access Journals (Sweden)

    Napoli Christian

    2012-08-01

    Full Text Available Abstract Background Since air can play a central role as a reservoir for microorganisms, in controlled environments such as operating theatres regular microbial monitoring is useful to measure air quality and identify critical situations. The aim of this study is to assess microbial contamination levels in operating theatres using both an active and a passive sampling method and then to assess if there is a correlation between the results of the two different sampling methods. Methods The study was performed in 32 turbulent air flow operating theatres of a University Hospital in Southern Italy. Active sampling was carried out using the Surface Air System and passive sampling with settle plates, in accordance with ISO 14698. The Total Viable Count (TVC was evaluated at rest (in the morning before the beginning of surgical activity and in operational (during surgery. Results The mean TVC at rest was 12.4 CFU/m3 and 722.5 CFU/m2/h for active and passive samplings respectively. The mean in operational TVC was 93.8 CFU/m3 (SD = 52.69; range = 22-256 and 10496.5 CFU/m2/h (SD = 7460.5; range = 1415.5-25479.7 for active and passive samplings respectively. Statistical analysis confirmed that the two methods correlate in a comparable way with the quality of air. Conclusion It is possible to conclude that both methods can be used for general monitoring of air contamination, such as routine surveillance programs. However, the choice must be made between one or the other to obtain specific information.

  11. Inorganic fractions in extracellular polymeric substance extracted from activated sludge and biofilm samples by different methods.

    Science.gov (United States)

    Zhang, Leiyan; Geng, Jinju; Ding, Lili; Ren, Hongqiang

    2012-01-01

    This study highlighted the inorganic fractions in the extracellular polymeric substance (EPS) extract from two activated sludges and one biofilm. Nine EPS extraction methods (centrifugation, sonication, cation exchange resin (CER) + sonication, CER, heating, formaldehyde + heating, formaldehyde + NaOH, ethanol and EDTA) were used in the study. The EPS extracts had large inorganic fractions, which ranged from 28% to 94% of the EPS dry weight. The EPS inorganic fraction was dependent on the source of the sludge and wastewater, the kinds of bacteria and the extraction method. The EPS extracts obtained by heating and sonication had smaller inorganic fractions than those obtained by centrifugation. The compositions of the inorganic fraction of EPS extracts obtained with CER and sonication + CER showed similar trends. The chemical extraction methods could contaminate the inorganic composition of EPS extracts by impurities, carrying over of the extractant itself or by changing the pH of the solution. Ethanol was the most effective extractant for obtaining inorganic ions. PMID:22828296

  12. Comparison of halocarbon measurements in an atmospheric dry whole air sample

    Directory of Open Access Journals (Sweden)

    George C. Rhoderick

    2015-11-01

    Full Text Available Abstract The growing awareness of climate change/global warming, and continuing concerns regarding stratospheric ozone depletion, will require continued measurements and standards for many compounds, in particular halocarbons that are linked to these issues. In order to track atmospheric mole fractions and assess the impact of policy on emission rates, it is necessary to demonstrate measurement equivalence at the highest levels of accuracy for assigned values of standards. Precise measurements of these species aid in determining small changes in their atmospheric abundance. A common source of standards/scales and/or well-documented agreement of different scales used to calibrate the measurement instrumentation are key to understanding many sets of data reported by researchers. This report describes the results of a comparison study among National Metrology Institutes and atmospheric research laboratories for the chlorofluorocarbons (CFCs dichlorodifluoromethane (CFC-12, trichlorofluoromethane (CFC-11, and 1,1,2-trichlorotrifluoroethane (CFC-113; the hydrochlorofluorocarbons (HCFCs chlorodifluoromethane (HCFC-22 and 1-chloro-1,1-difluoroethane (HCFC-142b; and the hydrofluorocarbon (HFC 1,1,1,2-tetrafluoroethane (HFC-134a, all in a dried whole air sample. The objective of this study is to compare calibration standards/scales and the measurement capabilities of the participants for these halocarbons at trace atmospheric levels. The results of this study show agreement among four independent calibration scales to better than 2.5% in almost all cases, with many of the reported agreements being better than 1.0%.

  13. The impact of different methods of DNA extraction on microbial community measures of BALF samples based on metagenomic data

    Science.gov (United States)

    Wen, Yan; Xiao, Fei; Wang, Chen; Wang, Zhen

    2016-01-01

    Purpose: It is a challenge to find a better microorganisms DNA extraction method for samples taken from the lower airways for metagenomic sequencing, as the concentrations of bacteria in the alveoli and small airways are likely considerably less than that of the mouth or lower digestive tract. Background DNA from the host, and extraction biases can significantly interfere with microbiota assessment and increase the cost of sequencing. This study aimed to develop an optimized DNA extraction method, which would enable a higher concentration of microbial DNA to be extracted from the samples. Methods: We compared the microbiota profiles of the lower airway communities in twelve individuals with IIP. DNA was extracted using three different extraction methods: QIAamp UCP PurePathogen Blood Kit named kit3 in this study, QIAamp UCP Pathogen Mini Kit named kit2, and QIAamp DNA Microbiome Kit named kit1. DNA libraries were constructed according to the manufacturer’s instructions (Illumina). The same workflows from Illumina were used to perform cluster generation, template hybridization, isothermal amplification, linearization, blocking, denaturing, and hybridization of the sequencing primers. Raw data was uploaded to MG-RAST v3 and analyzed. Results: A great number of bacterium inhabits the lower airways of patients with IIP, though there is no airway infection. More bacterium was found in mouth or upper airway. DNA concentrations of DNA samples isolated with kit1 with Benzonase were significantly lower than those isolated with the other two kits for BALF and mouthwash samples. Moreover, the ratio of human genome in clean reads of samples isolated with kit1 with Benzonase was remarkably smaller than those isolated with kit2 and kit3. The relative abundance of total bacteria, the total number of taxa, and the relative abundance of taxa in BALF samples as opposed to mouthwash samples with kit1 were significantly higher than for those extracted the other kits. Conclusion: A

  14. Optimization of the in-needle extraction device for the direct flow of the liquid sample through the sorbent layer.

    Science.gov (United States)

    Pietrzyńska, Monika; Voelkel, Adam

    2014-11-01

    In-needle extraction was applied for preparation of aqueous samples. This technique was used for direct isolation of analytes from liquid samples which was achieved by forcing the flow of the sample through the sorbent layer: silica or polymer (styrene/divinylbenzene). Specially designed needle was packed with three different sorbents on which the analytes (phenol, p-benzoquinone, 4-chlorophenol, thymol and caffeine) were retained. Acceptable sampling conditions for direct analysis of liquid sample were selected. Experimental data collected from the series of liquid samples analysis made with use of in-needle device showed that the effectiveness of the system depends on various parameters such as breakthrough volume and the sorption capacity, effect of sampling flow rate, solvent effect on elution step, required volume of solvent for elution step. The optimal sampling flow rate was in range of 0.5-2 mL/min, the minimum volume of solvent was at 400 µL level. PMID:25127610

  15. Development of ultrasound-assisted extraction for mercury speciation studies in biological samples using HPLC-ID-ICP-MS

    International Nuclear Information System (INIS)

    An efficient and simple ultrasound-assisted extraction method has been developed to determine inorganic and methyl mercury in biological samples by high performance liquid chromatography coupled with isotope dilution inductively coupled plasma mass spectrometry (HPLC-ID- ICP-MS). The operational parameters of ultrasound-assisted extraction, such as extractant composition, sonication time and extraction temperature, were optimized. The interconversion between CH3198Hg+ and 198Hg2+ during the operation was monitored by isotopic mercury-198 tracer technique. The efficiency of the extraction of inorganic and methyl mercury in biological samples was evaluated by total mercury determination using inductively coupled plasmas mass spectrometry. The best optimal extraction parameters are 30 minutes at 50 degree C for sonication using 0.05% (m/v) cysteine and 0.05% (v/v) 2-mercaptoethanol as extractant. The recovery of inorganic and methyl mercury was validated by four certified reference materials, including IAEA MA-B-3/TM tuna fish, NIST 1566a bovine liver, IAEA 350 fish mussel and GBW 07601 human hair. As for speciation study, a key point is that the original elemental speciation should be kept during the processing. Therefore, the above four certified reference materials spiked with CH3198Hg+ and 198Hg2+ were used to investigate the interconversion of methyl mercury into inorganic mercury or vice versa during the extraction. The CH3198Hg+ and 198Hg2+ were determined by high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry. The data show that the interconversion between CH3198Hg+ and 198Hg2+ during the operation is negligible. This extraction method is more simple and convenient than the common used ones and is more suitable for simultaneous determination of inorganic and methyl mercury by HPLC-ICP-MS technique.

  16. Comparison of DNA extraction methods for microbial community profiling with an application to pediatric bronchoalveolar lavage samples.

    Directory of Open Access Journals (Sweden)

    Dana Willner

    Full Text Available Barcoded amplicon sequencing is rapidly becoming a standard method for profiling microbial communities, including the human respiratory microbiome. While this approach has less bias than standard cultivation, several steps can introduce variation including the type of DNA extraction method used. Here we assessed five different extraction methods on pediatric bronchoalveolar lavage (BAL samples and a mock community comprised of nine bacterial genera to determine method reproducibility and detection limits for these typically low complexity communities. Additionally, using the mock community, we were able to evaluate contamination and select a relative abundance cut-off threshold based on the geometric distribution that optimizes the trade off between detecting bona fide operational taxonomic units and filtering out spurious ones. Using this threshold, the majority of genera in the mock community were predictably detected by all extraction methods including the hard-to-lyse Gram-positive genus Staphylococcus. Differences between extraction methods were significantly greater than between technical replicates for both the mock community and BAL samples emphasizing the importance of using a standardized methodology for microbiome studies. However, regardless of method used, individual patients retained unique diagnostic profiles. Furthermore, despite being stored as raw frozen samples for over five years, community profiles from BAL samples were consistent with historical culturing results. The culture-independent profiling of these samples also identified a number of anaerobic genera that are gaining acceptance as being part of the respiratory microbiome. This study should help guide researchers to formulate sampling, extraction and analysis strategies for respiratory and other human microbiome samples.

  17. Sample preparation for avian and porcine influenza virus cDNA amplification simplified: Boiling vs. conventional RNA extraction.

    Science.gov (United States)

    Fereidouni, Sasan R; Starick, Elke; Ziller, Mario; Harder, Timm C; Unger, Hermann; Hamilton, Keith; Globig, Anja

    2015-09-01

    RNA extraction and purification is a fundamental step that allows for highly sensitive amplification of specific RNA targets in PCR applications. However, commercial extraction kits that are broadly used because of their robustness and high yield of purified RNA are expensive and labor-intensive. In this study, boiling in distilled water or a commercial lysis buffer of different sample matrices containing avian or porcine influenza viruses was tested as an alternative. Real-time PCR (RTqPCR) for nucleoprotein gene fragment was used as read out. Results were compared with freshly extracted RNA by use of a commercial extraction kit. Different batches of virus containing materials, including diluted virus positive allantoic fluid or cell culture supernatant, and avian faecal, cloacal or oropharyngeal swab samples were used in this study. Simple boiling of samples without any additional purification steps can be used as an alternative RNA preparation method to detect influenza A virus nucleoprotein RNA in oropharyngeal swab samples, allantoic fluid or cell-culture supernatant. The boiling method is not applicable for sample matrices containing faecal material. PMID:25929989

  18. Sample preparation for avian and porcine influenza virus cDNA amplification simplified: Boilign vs. conventional RNA extraction

    International Nuclear Information System (INIS)

    Full text: RNA extraction and purification is a fundamental step that allows for highly sensitive amplification of specific RNA targets in PCR applications. However, commercial extraction kits that are broadly used because of their robustness and high yield of purified RNA are expensive and labor-intensive. In this study, boiling in distilled water or a commerical lysis buffer of different sample matrices containing avian or porcine influenza viruses was tested as an alternative. Real-time PCR (RTaPCR) for nucleoprotein gene fragment was used as read out. Results were compared with freshly extracted RNA by use of a commercial extraction kit. Different batches of virus containing material materials, including diluted virus positive allontoic fluid or cell culture supernatnat, and avian faecal, cloacal or oropharyngeal swab samples were used in this study. Simple boiling of samples without any additional purification steps can be used as an alternative RNA preparation method to detect influenza A virus nucleoprotein RNA in oropharyngeal swab samples, allantoic fluid or cell-culture supernatant. The boiling method is not applicable for sample matrices containing faecal material. (author)

  19. Estimating Sampling Biases and Measurement Uncertainties of AIRS-AMSU-A Temperature and Water Vapor Observations Using MERRA Reanalysis

    Science.gov (United States)

    Hearty, Thomas J.; Savtchenko, Andrey K.; Tian, Baijun; Fetzer, Eric; Yung, Yuk L.; Theobald, Michael; Vollmer, Bruce; Fishbein, Evan; Won, Young-In

    2014-01-01

    We use MERRA (Modern Era Retrospective-Analysis for Research Applications) temperature and water vapor data to estimate the sampling biases of climatologies derived from the AIRS/AMSU-A (Atmospheric Infrared Sounder/Advanced Microwave Sounding Unit-A) suite of instruments. We separate the total sampling bias into temporal and instrumental components. The temporal component is caused by the AIRS/AMSU-A orbit and swath that are not able to sample all of time and space. The instrumental component is caused by scenes that prevent successful retrievals. The temporal sampling biases are generally smaller than the instrumental sampling biases except in regions with large diurnal variations, such as the boundary layer, where the temporal sampling biases of temperature can be +/- 2 K and water vapor can be 10% wet. The instrumental sampling biases are the main contributor to the total sampling biases and are mainly caused by clouds. They are up to 2 K cold and greater than 30% dry over mid-latitude storm tracks and tropical deep convective cloudy regions and up to 20% wet over stratus regions. However, other factors such as surface emissivity and temperature can also influence the instrumental sampling bias over deserts where the biases can be up to 1 K cold and 10% wet. Some instrumental sampling biases can vary seasonally and/or diurnally. We also estimate the combined measurement uncertainties of temperature and water vapor from AIRS/AMSU-A and MERRA by comparing similarly sampled climatologies from both data sets. The measurement differences are often larger than the sampling biases and have longitudinal variations.

  20. Comparison of Air Impaction and Electrostatic Dust Collector Sampling Methods to Assess Airborne Fungal Contamination in Public Buildings.

    Science.gov (United States)

    Normand, Anne-Cécile; Ranque, Stéphane; Cassagne, Carole; Gaudart, Jean; Sallah, Kankoé; Charpin, Denis-André; Piarroux, Renaud

    2016-03-01

    Many ailments can be linked to exposure to indoor airborne fungus. However, obtaining a precise measurement of airborne fungal levels is complicated partly due to indoor air fluctuations and non-standardized techniques. Electrostatic dust collector (EDC) sampling devices have been used to measure a wide range of airborne analytes, including endotoxins, allergens, β-glucans, and microbial DNA in various indoor environments. In contrast, viable mold contamination has only been assessed in highly contaminated environments such as farms and archive buildings. This study aimed to assess the use of EDCs, compared with repeated air-impactor measurements, to assess airborne viable fungal flora in moderately contaminated indoor environments. Indoor airborne fungal flora was cultured from EDCs and daily air-impaction samples collected in an office building and a daycare center. The quantitative fungal measurements obtained using a single EDC significantly correlated with the cumulative measurement of nine daily air impactions. Both methods enabled the assessment of fungal exposure, although a few differences were observed between the detected fungal species and the relative quantity of each species. EDCs were also used over a 32-month period to monitor indoor airborne fungal flora in a hospital office building, which enabled us to assess the impact of outdoor events (e.g. ground excavations) on the fungal flora levels on the indoor environment. In conclusion, EDC-based measurements provided a relatively accurate profile of the viable airborne flora present during a sampling period. In particular, EDCs provided a more representative assessment of fungal levels compared with single air-impactor sampling. The EDC technique is also simpler than performing repetitive air-impaction measures over the course of several consecutive days. EDC is a versatile tool for collecting airborne samples and was efficient for measuring mold levels in indoor environments. PMID:26491105

  1. Sources of pre-analytical variations in yield of DNA extracted from blood samples: analysis of 50,000 DNA samples in EPIC.

    Directory of Open Access Journals (Sweden)

    Elodie Caboux

    Full Text Available The European Prospective Investigation into Cancer and nutrition (EPIC is a long-term, multi-centric prospective study in Europe investigating the relationships between cancer and nutrition. This study has served as a basis for a number of Genome-Wide Association Studies (GWAS and other types of genetic analyses. Over a period of 5 years, 52,256 EPIC DNA samples have been extracted using an automated DNA extraction platform. Here we have evaluated the pre-analytical factors affecting DNA yield, including anthropometric, epidemiological and technical factors such as center of subject recruitment, age, gender, body-mass index, disease case or control status, tobacco consumption, number of aliquots of buffy coat used for DNA extraction, extraction machine or procedure, DNA quantification method, degree of haemolysis and variations in the timing of sample processing. We show that the largest significant variations in DNA yield were observed with degree of haemolysis and with center of subject recruitment. Age, gender, body-mass index, cancer case or control status and tobacco consumption also significantly impacted DNA yield. Feedback from laboratories which have analyzed DNA with different SNP genotyping technologies demonstrate that the vast majority of samples (approximately 88% performed adequately in different types of assays. To our knowledge this study is the largest to date to evaluate the sources of pre-analytical variations in DNA extracted from peripheral leucocytes. The results provide a strong evidence-based rationale for standardized recommendations on blood collection and processing protocols for large-scale genetic studies.

  2. Optimum Method to Determine Gamma Activity in Large Boxes of Radioactive Material - In-toto Measurement vs. Sample Extraction

    International Nuclear Information System (INIS)

    During the operations of nuclear facilities and during the environmental remediation and decommissioning of nuclear facilities, radioactive waste is generated which must be assayed. To save on labor and transportation costs, this material is commonly placed in large containers of typically several cubic meters in size [e.g. B-25]. The most common choices of assay are to either extract a representative sample of the contents for laboratory assay, or to use in-situ gamma spectroscopy of the total container. Both of these methods have strengths and weaknesses. In Situ methods determine container activity directly and typically quantify gamma emitters which are then correlated to total activity. Gamma measurement accuracy can suffer from an inadequate efficiency calibration, which can be caused by variations in container size, shape, matrix fill height, or matrix density, but primarily by non-homogeneous distribution of the radioactivity. Laboratory assay methods using a small sample extracted from the container are generally quite accurate for the sample analyzed; but the determination of total container activity requires the assumption that the sample analyzed in the laboratory is truly representative of the total container, which is also heavily influenced by the non-homogeneous distribution of the radioactivity. This evaluation attempts to determine the best way to estimate the activity within the container and gives quantitative estimates of measurement uncertainty for various conditions of radioactivity contained within the container and for various in-toto and sampling strategies. A new feature of the ISOCS [In-Situ Object Counting System] software called IUE [ISOCS Uncertainty Estimator] was used. First, the various parameters were examined which cause uncertainty in the in-toto measurement to evaluate those which are the major contributors and to asses the measurement uncertainty for a uniformly distributed sample. Next, a series of levels of non

  3. Studies on radioactivities of dust samples in the air at high altitudes [Boeisho Gijutsu Kenkyu Honbu Giho, no.7169

    International Nuclear Information System (INIS)

    The radioactivity concentrations of airborne dust samples were studied. The samples had been collected at high altitude by the Japan Air Self-Defense Force from April 2013 to March 2014. The obtained data were used for gross beta radioactivity analysis and gamma nuclide analysis. It is shown that cesium 137 was mainly detected at the 10 km and 3 km altitude of central area of Japan in several samples. Gaseous radioiodine was not detected in all the samples. Radioactive xenon was detected but the concentration did not show significant difference to the background level. (author)

  4. Online recovery of radiocesium from soil, cellulose and plant samples by supercritical fluid extraction employing crown ethers and calix-crown derivatives as extractants

    International Nuclear Information System (INIS)

    Two crown ethers (CEs) viz. dibenzo18crown6, and dibenzo12crown7 and three calix-crown derivatives viz. (octyloxy)calix[4]arene-mono-crown-6 (CMC), calix[4]arene-bis(o-benzocrown-6) (CBC), and calix[4]arene-bis(naphthocrown-6) (CNC) were evaluated for the recovery of 137Cs from synthetic soil, cellulose (tissue paper), and plant samples by supercritical fluid extraction (SFE) route. CEs showed poor extraction of 137Cs from soil matrix. SFE experiments using 1 × 10-3 M solutions of CMC, CBC and CNC in acetonitrile at 3 M HNO3 as modifiers displayed better extraction of 137Cs, viz. 21(±2) % (CMC), 16.5(±3) % (CBC), and 4(±1) % (CNC). It was not possible to recover 137Cs quantitatively from soil matrix. The inefficient extraction of 137Cs from soil matrix was attributed to its incorporation into the interstitial sites. Experiments on tissue papers using CMC showed near quantitative 137Cs recovery. On the other hand, recovery from plant samples varied between 50(±5) % (for stems) and 75(±5) % (for leaves). (author)

  5. Sequential automated fusion/extraction chromatography methodology for the dissolution of uranium in environmental samples for mass spectrometric determination

    International Nuclear Information System (INIS)

    An improved methodology has been developed, based on dissolution by automated fusion followed by extraction chromatography for the detection and quantification of uranium in environmental matrices by mass spectrometry. A rapid fusion protocol (2/LiBr melts were used. The use of a M4 fusion unit also improved repeatability in sample preparation over muffle furnace fusion. Instrumental issues originating from the presence of high salt concentrations in the digestate after lithium metaborate fusion was also mitigated using an extraction chromatography (EXC) protocol aimed at removing lithium and interfering matrix constituants prior to the elution of uranium. The sequential methodology, which can be performed simultaneously on three samples, requires less than 20 min per sample for fusion and separation. It was successfully coupled to inductively coupled plasma mass spectrometry (ICP-MS) achieving detection limits below 100 pg kg-1 for 5-300 mg of sample.

  6. MICROBIOLOGICAL SURVEILLANCE OF AIR QUALITY IN OPE RATION THEATRES - COMPARISON OF THE CONVENTIONAL SETTLE PL ATE TECHNIQUES VS USE OF AN AIR SAMPLING DEVICE.

    Directory of Open Access Journals (Sweden)

    Prathab

    2012-10-01

    Full Text Available ABSTRACT: BACKGROUND: Air as a means of nosocomial transmission has alw ays remained as a cause of concern for health care providers and especially personnel involved in infection control activities. Although there are no uniform c onsensus on either the standards for surveillance, methodology for monitoring or the lev els of acceptable contamination, it still remains a fact that we need to have some criteria t o monitor air quality in atleast the critical care areas like the operation theatres. METHODOLOGY: Air quality surveillance in the operation theatres was performed simultaneously usin g the settle plate technique and an air sampling device. A total of 9 operation theatres were subjected to 4 surveillance cycles with a minimum of 2 recordings in each theatre following standard protocols and accepted method used to calculate bioburden. RESULTS: A comparison was made between the two methods using the data available with 72 recordings . In th e settle plate technique, the mean cfu /mm3 was found to be 17.11 and 22cfu/mm3 at less than 30 cm and at a point more than 30cms of the operating table where as the corresponding means usi ng the air sampler was137.83 and 164.11cfu/mm3 respectively which showed considerable statistical significance . CONCLUSION : The use of an air sampler would be more appropriate in monitoring the air quality in critical care areas ensuring a more stringent method of qual ity check without compromising on the the standard accepted norms and addressing the issue of patient safety with reference to infection prevention

  7. Double-salting out assisted liquid-liquid extraction (SALLE) HPLC method for estimation of temozolomide from biological samples.

    Science.gov (United States)

    Jain, Darshana; Athawale, Rajani; Bajaj, Amrita; Shrikhande, Shruti

    2014-11-01

    The role of temozolomide (TMZ) in treatment of high grade gliomas, melanomas and other malignancies is being defined by the current clinical developmental trials. Temozolomide belongs to the group of alkylating agents and is prescribed to patients suffering from most aggressive forms of brain tumors. The estimation techniques for temozolomide from the extracted plasma or biological samples includes high-performance liquid chromatography with UV detection (HPLC-UV), micellar electrokinetic capillary chromatography (MKEC) and liquid chromatography coupled to mass spectroscopy (LC-MS). These methods suffer from disadvantages like low resolution, low sensitivity, low recovery or cost involvement. An analytical method possessing capacity to estimate low quantities of TMZ in plasma samples with high extraction efficiency (%) and high resolution with cost effectiveness needs to be developed. Cost effective, robust and low plasma component interfering HPLC method using salting out liquid-liquid extraction (SALLE) technique was developed and validated for estimation of drug from plasma samples. The extraction efficiency (%) with conventional LLE technique with methanol, ethyl acetate, dichloromethane and acetonitrile was found to be 5.99±2.45, 45.39±4.56, 46.04±1.14 and 46.23±3.67 respectively. Extraction efficiency (%) improved with SALLE where sodium chloride was used as an electrolyte and was found to be 6.80±5.56, 52.01±3.13, 62.69±2.11 and 69.20±1.18 with methanol, ethyl acetate, dichloromethane and acetonitrile as organic solvent. Upon utilization of two salts for extraction (double salting liquid-liquid extraction) the extraction efficiency (%) was further improved and was twice of LLE. It was found that double salting liquid-liquid extraction technique yielded extraction efficiency (%) of 11.71±5.66, 55.62±3.44, 77.28±2.89 and 87.75±0.89. Hence a method based on double SALLE was developed for quantification of TMZ demonstrating linearity in the range of

  8. 3D Air Quality and the Clean Air Interstate Rule: Lagrangian Sampling of CMAQ Model Results to Aid Regional Accountability Metrics

    Science.gov (United States)

    Fairlie, T. D.; Szykman, Jim; Pierce, Robert B.; Gilliland, A. B.; Engel-Cox, Jill; Weber, Stephanie; Kittaka, Chieko; Al-Saadi, Jassim A.; Scheffe, Rich; Dimmick, Fred; Tikvart, Joe

    2008-01-01

    The Clean Air Interstate Rule (CAIR) is expected to reduce transport of air pollutants (e.g. fine sulfate particles) in nonattainment areas in the Eastern United States. CAIR highlights the need for an integrated air quality observational and modeling system to understand sulfate as it moves in multiple dimensions, both spatially and temporally. Here, we demonstrate how results from an air quality model can be combined with a 3d monitoring network to provide decision makers with a tool to help quantify the impact of CAIR reductions in SO2 emissions on regional transport contributions to sulfate concentrations at surface monitors in the Baltimore, MD area, and help improve decision making for strategic implementation plans (SIPs). We sample results from the Community Multiscale Air Quality (CMAQ) model using ensemble back trajectories computed with the NASA Langley Research Center trajectory model to provide Lagrangian time series and vertical profile information, that can be compared with NASA satellite (MODIS), EPA surface, and lidar measurements. Results are used to assess the regional transport contribution to surface SO4 measurements in the Baltimore MSA, and to characterize the dominant source regions for low, medium, and high SO4 episodes.

  9. Comparative Assessment of Automated Nucleic Acid Sample Extraction Equipment for Biothreat Agents

    OpenAIRE

    Kalina, Warren Vincent; Douglas, Christina Elizabeth; Coyne, Susan Rajnik; Minogue, Timothy Devin

    2014-01-01

    Magnetic beads offer superior impurity removal and nucleic acid selection over older extraction methods. The performances of nucleic acid extraction of biothreat agents in blood or buffer by easyMAG, MagNA Pure, EZ1 Advanced XL, and Nordiag Arrow were evaluated. All instruments showed excellent performance in blood; however, the easyMAG had the best precision and versatility.

  10. The use of supercritical fluid extraction as a sample preparation technique for soils

    International Nuclear Information System (INIS)

    Using off-line supercritical fluid extraction (SFE), polynuclear aromatic hydrocarbons (PAHs) were extracted at different levels from various soil and sediment matrices. Based upon GC/MS measurements a number of SFE operational parameters including pressure, temperature and flow rate, were optimized to yield the highest efficiencies with the best precision

  11. ASSESSMENT OF A SEQUENTIAL EXTRACTION PROCEDURE FOR PERTURBED LEAD CONTAMINATED SAMPLES WITH AND WITHOUT PHOSPHORUS AMENDMENTS

    Science.gov (United States)

    Sequential extraction procedures (SEP) attempt to determine the solid-phase association of elements in natural matrices. However, a major obstacle confronting SEP is species alteration of extracted metals before separation of solids from solution. The objectives of this study w...

  12. Stir-bar supported micro-solid-phase extraction for the determination of polychlorinated biphenyl congeners in serum samples.

    Science.gov (United States)

    Sajid, Muhammad; Basheer, Chanbasha

    2016-07-15

    In present work, a new configuration of micro-solid phase extraction was introduced and termed as stir-bar supported micro-solid-phase extraction (SB-μ-SPE). A tiny stir-bar was packed inside the porous polypropylene membrane along with sorbent material and the edges of membrane sheet were heat sealed to secure the contents. The packing of stir-bar inside the μ-SPE device does not allow the device to stick with the wall or any corner of the sample vial during extraction, which is, however, a frequent observation in routine μ-SPE. Moreover, it enhances effective surface area of the sorbent exposed to sample solution through continuous agitation (motion and rotation). It also completely immerses the SB-μ-SPE device in the sample solution even for non-polar sorbents. Polychlorinated biphenyls (PCBs) were selected as model compounds and the method performance was evaluated in human serum samples. After extraction, samples were analyzed by gas chromatography mass spectrometry (GC-MS). The factors that affect extraction efficiency of SB-μ-SPE were optimized. Under optimum conditions, a good linearity (0.1-100ngmL(-1)) with coefficients of determinations ranging from 0.9868 to 0.9992 was obtained. Limits of detections were ranged between 0.003 and 0.047ngmL(-1). Acceptable values for inter-day (3.2-9.1%) and intra-day (3.1-7.2%) relative standard deviations were obtained. The optimized method was successfully applied to determine the concentration of PCB congeners in human serum samples. PMID:27291862

  13. Comparative Study of the Effect of Sample Pretreatment and Extraction on the Determination of Flavonoids from Lemon (Citrus limon)

    OpenAIRE

    Carlos A Ledesma-Escobar; Priego-Capote, Feliciano; Luque de Castro, María D.

    2016-01-01

    Background Flavonoids have shown to exert multiple beneficial effects on human health, being also appreciated by both food and pharmaceutical industries. Citrus fruits are a key source of flavonoids, thus promoting studies to obtain them. Characteristics of these studies are the discrepancies among sample pretreatments and among extraction methods, and also the scant number of comparative studies developed so far. Objective Evaluate the effect of both the sample pretreatment and the extractio...

  14. Integrated targeted and non-targeted analysis of water sample extracts with micro-scale UHPLC–MS

    OpenAIRE

    Dominik Deyerling; Karl-Werner Schramm

    2015-01-01

    A sensitive method is introduced to detect selected pharmaceutical residues and polar pesticides with UHPLC–MS in water samples of different origin. Active or passive water sampling was combined with a laboratory solid-phase extraction cleanup and stable isotope dilution analysis. Recovery experiments demonstrated that the internal standard correction performed well for the compensation of matrix effects. Besides, the original targeted analysis approach was expanded by non-target analysis of ...

  15. Evaluation of sample extraction methods for proteomics analysis of green algae Chlorella vulgaris.

    Science.gov (United States)

    Gao, Yan; Lim, Teck Kwang; Lin, Qingsong; Li, Sam Fong Yau

    2016-05-01

    Many protein extraction methods have been developed for plant proteome analysis but information is limited on the optimal protein extraction method from algae species. This study evaluated four protein extraction methods, i.e. direct lysis buffer method, TCA-acetone method, phenol method, and phenol/TCA-acetone method, using green algae Chlorella vulgaris for proteome analysis. The data presented showed that phenol/TCA-acetone method was superior to the other three tested methods with regards to shotgun proteomics. Proteins identified using shotgun proteomics were validated using sequential window acquisition of all theoretical fragment-ion spectra (SWATH) technique. Additionally, SWATH provides protein quantitation information from different methods and protein abundance using different protein extraction methods was evaluated. These results highlight the importance of green algae protein extraction method for subsequent MS analysis and identification. PMID:26935773

  16. Neutron activitation analysis of an air-dust sample using a high-flux 14 Mev neutron generator

    International Nuclear Information System (INIS)

    The 14 MeV neutron activation analysis technique is illustrated for multielement analysis of a Milanese air-dust sample. The neutron generator and electronic system, the efficiency and flux calibration, the γ-ray background, the sample preparation and the peak analysis used are described. After careful corrections of all possible interferences and error calculations, the results of 24 elemental concentrations are compared with those of other analytical techniques in the scope of an interlaboratory test. (orig.)

  17. SAMPLING AND ANALYSIS FOR POLYCHLORINATED DIBENZO-P-DIOXINS AND DIBENZOFURANS IN AMBIENT AIR

    Science.gov (United States)

    A short-term study for determination of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) in ambient air in Green Bay, Wisconsin, has been completed. eneral Metals Works PS-1 air samplers equipped with particle filters and polyurethane foam (PUF)...

  18. Knoellia aerolata sp. nov., isolated from an air sample in Korea.

    Science.gov (United States)

    Weon, Hang-Yeon; Kim, Byung-Yong; Schumann, Peter; Kroppenstedt, Reiner M; Noh, Hyung-Jun; Park, Chan-Won; Kwon, Soon-Wo

    2007-12-01

    An aerobic, Gram-positive, non-motile, non-spore-forming, rod-coccus-shaped bacterium, strain 5317S-21(T), was isolated from an air sample from Suwon city, Republic of Korea. The isolate was able to grow within a pH range of 5.0-9.0 and a temperature range of 5-35 degrees C and it tolerated up to 2 % (w/v) NaCl. The cell-wall peptidoglycan contained meso-diaminopimelic acid as diagnostic diamino acid. The predominant isoprenoid quinone was MK-8(H(4)). The major polar lipids were phosphatidylinositol, phosphatidylethanolamine and diphosphatidylglycerol; phosphatidylglycerol and several unknown phospholipids were also detected. Mycolic acids were absent. The only whole-cell sugar was glucose. The major cellular fatty acids were iso-C(16 : 0), C(17 : 1)omega8c and iso-C(15 : 0). 16S rRNA gene sequence analysis indicated that strain 5317S-21(T) was related phylogenetically to members of the genus Knoellia, with 97.4 % sequence similarity to the type strains of Knoellia sinensis and Knoellia subterranea. The G+C content of the genomic DNA of strain 5317S-21(T) was 73 mol%. Levels of DNA-DNA relatedness between strain 5317S-21(T) and the type strains of Knoellia sinensis and Knoellia subterranea were 37 and 41 %, respectively. It was concluded that strain 5317S-21(T) represents a novel species of the genus Knoellia, for which the name Knoellia aerolata sp. nov. is proposed. The type strain is 5317S-21(T) (=KACC 20583(T) =DSM 18566(T)). PMID:18048739

  19. Supercritical fluid extraction and ultra performance liquid chromatography of respiratory quinones for microbial community analysis in environmental and biological samples.

    Science.gov (United States)

    Hanif, Muhammad; Atsuta, Yoichi; Fujie, Koichi; Daimon, Hiroyuki

    2012-01-01

    Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE) and ultra performance liquid chromatography (UPLC) method for the analysis of bacterial respiratory quinones (RQ) in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA) detector was successfully applied to the simultaneous determination of ubiquinones (UQ) and menaquinones (MK) without tedious pretreatment. Supercritical carbon dioxide (scCO(2)) extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost) and biological samples (swine and Japanese quail feces). PMID:22391598

  20. Supercritical Fluid Extraction and Ultra Performance Liquid Chromatography of Respiratory Quinones for Microbial Community Analysis in Environmental and Biological Samples

    Directory of Open Access Journals (Sweden)

    Koichi Fujie

    2012-03-01

    Full Text Available Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE and ultra performance liquid chromatography (UPLC method for the analysis of bacterial respiratory quinones (RQ in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA detector was successfully applied to the simultaneous determination of ubiquinones (UQ and menaquinones (MK without tedious pretreatment. Supercritical carbon dioxide (scCO2 extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost and biological samples (swine and Japanese quail feces.

  1. Evaluation of micro-colorimetric lipid determination method with samples prepared using sonication and accelerated solvent extraction methods

    Science.gov (United States)

    Two common laboratory extraction techniques were evaluated for routine use with the micro-colorimetric lipid determination method developed by Van Handel (1985) [E. Van Handel, J. Am. Mosq. Control Assoc. 1(1985) 302] and recently validated for small samples by Inouye and Lotufo ...

  2. A hybrid DNA extraction method for the qualitative and quantitative assessment of bacterial communities from poultry production samples

    Science.gov (United States)

    The efficacy of DNA extraction protocols can be highly dependent upon both the type of sample being investigated and the types of downstream analyses performed. Considering that the use of new bacterial community analysis techniques (e.g., microbiomics, metagenomics) is becoming more prevalent in th...

  3. EFFECTIVE METHOD TO EXTRACT DNA FROM ENVIRONMENTAL SAMPLES FOR POLYMERASE CHAIN REACTION AMPLIFICATION AND DNA FINGERPRINT ANALYSIS

    Science.gov (United States)

    A rapid direct-extraction method was used to obtain DNA from environmental soil samples. eat, enzymes, and guanidine isothiocyanate were utilized to lyse cells. he DNA was purified by agarose gel electrophoresis, amplified with 16S based primers by use of the polymerase chain rea...

  4. Early detection of foot-and-mouth disease virus from infected cattle using a dry filter air sampling system

    Science.gov (United States)

    Foot-and-mouth disease (FMD) is a highly contagious livestock disease of high economic impact. Early detection of FMD virus (FMDV) is fundamental for rapid outbreak control. Air sampling collection has been demonstrated as a useful technique for detection of FMDV RNA in infected animals, related to ...

  5. Detection of Campylobacter Bacteria in Air Samples for Continuous Real-Time Monitoring of Campylobacter Colonization in Broiler Flocks

    DEFF Research Database (Denmark)

    Olsen, Katja Nyholm; Lund, Marianne; Skov, J.;

    2009-01-01

    Improved monitoring tools are important for the control of Campylobacter bacteria in broiler production. In this study, we compare the sensitivities of detection of Campylobacter by PCR with feces, dust, and air samples during the lifetimes of broilers in two poultry houses and conclude that the ...

  6. Development of hyperbranched polymers with non-covalent interactions for extraction and determination of aflatoxins in cereal samples.

    Science.gov (United States)

    Liu, Xiaoyan; Li, Huihui; Xu, Zhigang; Peng, Jialin; Zhu, Shuqiang; Zhang, Haixia

    2013-10-01

    A novel approach for assembling homogeneous hyperbranched polymers based on non-covalent interactions with aflatoxins was developed; the polymers were used to evaluate the extraction of aflatoxins B1, B2, G1 and G2 (AFB1, AFB2, AFG1 and AFG2) in simulant solutions. The results showed that the extraction efficiencies of three kinds of synthesized polymers for the investigated analytes were not statistically different; as a consequence, one of the representative polymers (polymer I) was used as the solid-phase extraction (SPE) sorbent to evaluate the influences of various parameters, such as desorption conditions, pH, ionic strength, concentration of methanol in sample solutions, and the mass of the sorbent on the extraction efficiency. In addition, the extraction efficiencies for these aflatoxins were compared between the investigated polymer and the traditional sorbent C18. The results showed that the investigated polymer had superior extraction efficiencies. Subsequently, the proposed polymer for the SPE packing material was employed to enrich and analyze four aflatoxins in the cereal powder samples. The limits of detection (LODs) at a signal-to-noise (S/N) ratio of 3 were in the range of 0.012-0.120 ng g(-1) for four aflatoxins, and the limits of quantification (LOQs) calculated at S/N=10 were from 0.04 to 0.40 ng g(-1) for four aflatoxins. The recoveries of four aflatoxins from cereal powder samples were in the range of 82.7-103% with relative standard deviations (RSDs) lower than 10%. The results demonstrate the suitability of the SPE approach for the analysis of trace aflatoxins in cereal powder samples. PMID:24050668

  7. Solvent-assisted dispersive solid-phase extraction: A sample preparation method for trace detection of diazinon in urine and environmental water samples.

    Science.gov (United States)

    Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

    2016-09-01

    In this research, a sample preparation method termed solvent-assisted dispersive solid-phase extraction (SA-DSPE) was applied. The used sample preparation method was based on the dispersion of the sorbent into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was received by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the diazinon, the cloudy solution was centrifuged and diazinon in the sediment phase dissolved in ethanol and determined by gas chromatography-flame ionization detector. Under the optimized conditions (pH of solution=7.0, Sorbent: benzophenone, 2%, Disperser solvent: ethanol, 500μL, Centrifuge: centrifuged at 4000rpm for 3min), the method detection limit for diazinon was 0.2, 0.3, 0.3 and 0.3μgL(-1) for distilled water, lake water, waste water and urine sample, respectively. Furthermore, the pre-concentration factor was 363.8, 356.1, 360.7 and 353.38 in distilled water, waste water, lake water and urine sample, respectively. SA-DSPE was successfully used for trace monitoring of diazinon in urine, lake and waste water samples. PMID:27495366

  8. Effective removal of co-purified inhibitors from extracted DNA samples using synchronous coefficient of drag alteration (SCODA) technology.

    Science.gov (United States)

    Schmedes, Sarah; Marshall, Pamela; King, Jonathan L; Budowle, Bruce

    2013-07-01

    Various types of biological samples present challenges for extraction of DNA suitable for subsequent molecular analyses. Commonly used extraction methods, such as silica membrane columns and phenol-chloroform, while highly successful may still fail to provide a sufficiently pure DNA extract with some samples. Synchronous coefficient of drag alteration (SCODA), implemented in Boreal Genomics' Aurora Nucleic Acid Extraction System (Boreal Genomics, Vancouver, BC), is a new technology that offers the potential to remove inhibitors effectively while simultaneously concentrating DNA. In this initial study, SCODA was tested for its ability to remove various concentrations of forensically and medically relevant polymerase chain reaction (PCR) inhibitors naturally found in tissue, hair, blood, plant, and soil samples. SCODA was used to purify and concentrate DNA from intentionally contaminated DNA samples containing known concentrations of hematin, humic acid, melanin, and tannic acid. The internal positive control (IPC) provided in the Quantifiler™ Human DNA Quantification Kit (Life Technologies, Foster City, CA) and short tandem repeat (STR) profiling (AmpFℓSTR® Identifiler® Plus PCR Amplification Kit; Life Technologies, Foster City, CA) were used to measure inhibition effects and hence purification. SCODA methodology yielded overall higher efficiency of purification of highly contaminated samples compared with the QIAquick® PCR Purification Kit (Qiagen, Valencia, CA). SCODA-purified DNA yielded no cycle shift of the IPC for each sample and yielded greater allele percentage recovery and relative fluorescence unit values compared with the QIAquick® purification method. The Aurora provided an automated, minimal-step approach to successfully remove inhibitors and concentrate DNA from challenged samples. PMID:23254459

  9. Estimation of iron in fruit samples by substoichiometric extraction with malonic anilide

    International Nuclear Information System (INIS)

    A radiochemical solvent extraction method for the determination of iron(III) employing extractant malonic anilide (MA), synthesized in the laboratory, has been described. Effects of different parameters on the extraction of iron(III) from 2M hydrochloric acid into a mixed organic solvent (methyl isobutyl ketone (TIBK) and diethyl ether) have been studied in detail. The method was applied for the estimation of iron content in several fruits using the principle of substoichiometric isotope dilution analysis. (author) 18 refs.; 1 fig.; 7 tabs

  10. Indoor Air Quality in Selected Samples of Primary Schools in Kuala Terengganu, Malaysia

    Directory of Open Access Journals (Sweden)

    Marzuki Ismail

    2010-01-01

    Full Text Available Studies have found out that indoor air quality affects human especially children and the elderly more compared to ambient atmospheric air. This study aims to investigate indoor air pollutants concentration in selected vernacular schools with different surrounding human activities in Kuala Terengganu, the administrative and commercial center of Terengganu state. Failure to identify and establish indoor air pollution status can increase the chance of long-term and short-term health problems for these young students and staff; reduction in productivity of teachers; and degrade the youngsters learning environment and comfort. Indoor air quality (IAQ parameters in three primary schools were conducted during the monsoon season of November 2008 for the purposes of assessing ventilation rates, levels of particulate matter (PM10 and air quality differences between schools. In each classroom, carbon monoxide (CO, CO2, air velocity, relative humidity and temperature were performed during school hours, and a complete walkthrough survey was completed. Results show a statistically significant difference for the five IAQ parameters between the three schools at the 95.0% confidence level. We conclude our findings by confirming the important influence of surrounding human activities on indoor concentrations of pollutants in selected vernacular schools in Kuala Terengganu.

  11. Application of Synergistic Solvent Extraction by Formation of Ternary Complex for Determination of Trace Zn(II) in Water Samples

    International Nuclear Information System (INIS)

    The application of a synergistic solvent extraction by the formation of ternary complex with pyrocatechol violet (PV) and benzalkonium chloride (BC) was studied for determination of trace Zn(II) in water samples. The pH of sample solution and the amount of PV and BC added were optimized for the formation of the stable complex, a proper solvent was selected for the effective extraction, and the concentration of nitric acid was fixed for the back extraction of the complex from the solvent. After the ionic strength of 100 mL sample solution was adjusted to 0.1 M by adding NaCl and the pH was fixed at 9 with a carbonate buffer, 1.0 mL of 2% PV solution was added to form Zn(II)-PV complex then the Zn(II)-PV/BC ternary complex was made by adding 1.0 mL of 10% BC solution. The ternary complex was extracted into 10 mL of MIBK. And the ternary complex was backextracted with 10 mL of 1.0 mol/L nitric acid to determine Zn(II) by a flame atomic absorption spectrophotometer (flame-AAS). The interference of concomitant ions on the extraction of Zn(II) was investigated. This procedure was applied to the analysis of three real samples such as Dalbang-dam water, laboratory tap water and Jungnajin seawater. The recoveries of Zn(II) in spiked samples were 86.58-104.1%

  12. Supercritical fluid extraction for some carbamate insecticides in potatoes samples with HPLC/flourescence determination and HPLC/mass spectrometry confirmation

    OpenAIRE

    Gilvanda Silva Nunes; Santos, Teresa Cristina R.; Damiá Barceló; Alexandre Santos Pimenta; Maria Lúcia Ribeiro

    2002-01-01

    Six supercritical fluid extraction (SFE) methods were tested, by varying the following operational parameters: CO2 pressure, time and temperature of extraction, type and proportion of static modifier, and Hydromatrix®/sample rate into cell. Firstly, insecticide carbamates were extracted from spiked potatoes samples (fortification level of 0,5 mg.Kg-1) by using SPE procedures, and then final extracts were analyzed HPLC/fluorescence. Good performance was observed with SFE methods that operated ...

  13. A spatial multicriteria model for determining air pollution at sample locations.

    Science.gov (United States)

    Réquia Júnior, Weeberb João; Roig, Henrique Llacer; Koutrakis, Petros

    2015-02-01

    Atmospheric pollution in urban centers has been one of the main causes of human illness related to the respiratory and circulatory system. Efficient monitoring of air quality is a source of information for environmental management and public health. This study investigates the spatial patterns of atmospheric pollution using a spatial multicriteria model that helps target locations for air pollution monitoring sites. The main objective was to identify high-priority areas for measuring human exposures to air pollutants as they relate to emission sources. The method proved to be viable and flexible in its application to various areas. PMID:25947058

  14. An improved protocol for DNA extraction from alkaline soil and sediment samples for constructing metagenomic libraries.

    Science.gov (United States)

    Verma, Digvijay; Satyanarayana, T

    2011-09-01

    An improved single-step protocol has been developed for extracting pure community humic substance-free DNA from alkaline soils and sediments. The method is based on direct cell lysis in the presence of powdered activated charcoal and polyvinylpolypyrrolidone followed by precipitation with polyethyleneglycol and isopropanol. The strategy allows simultaneous isolation and purification of DNA while minimizing the loss of DNA with respect to other available protocols for metagenomic DNA extraction. Moreover, the purity levels are significant, which are difficult to attain with any of the methods reported in the literature for DNA extraction from soils. The DNA thus extracted was free from humic substances and, therefore, could be processed for restriction digestion, PCR amplification as well as for the construction of metagenomic libraries. PMID:21519906

  15. Sample preparation for an optimized extraction of localized metabolites in lichens: Application to Pseudevernia furfuracea.

    Science.gov (United States)

    Komaty, Sarah; Letertre, Marine; Dang, Huyen Duong; Jungnickel, Harald; Laux, Peter; Luch, Andreas; Carrié, Daniel; Merdrignac-Conanec, Odile; Bazureau, Jean-Pierre; Gauffre, Fabienne; Tomasi, Sophie; Paquin, Ludovic

    2016-04-01

    Lichens are symbiotic organisms known for producing unique secondary metabolites with attractive cosmetic and pharmacological properties. In this paper, we investigated three standard methods of preparation of Pseudevernia furfuracea (blender grinding, ball milling, pestle and mortar). The materials obtained were characterized by electronic microscopy, nitrogen adsorption and compared from the point of view of extraction. Their microscopic structure is related to extraction efficiency. In addition, it is shown using thalline reactions and mass spectrometry mapping (TOF-SIMS) that these metabolites are not evenly distributed throughout the organism. Particularly, atranorin (a secondary metabolite of interest) is mainly present in the cortex of P. furfuracea. Finally, using microwave assisted extraction (MAE) we obtained evidence that an appropriate preparation can increase the extraction efficiency of atranorin by a factor of five. PMID:26838439

  16. Supercritical fluid extraction of uranium from unsintered/sintered oxides samples using tri-n-butyl phosphate and N,N-dihexyloctanamide

    International Nuclear Information System (INIS)

    Direct extraction of different uranium oxide samples (unsintered UO3 and U3O8 and sintered UO2) was carried out using supercritical carbon dioxide modified with methanol solutions of extractants (30% v/v) such as tri-n-butyl phosphate (TBP) and/or, N-dihexyloctanamide (DHOA) in dynamic as well as static modes of extraction. Whereas near quantitative (> 95%) uranium extraction was observed in static mode, only partial extraction was observed in dynamic mode of extraction. This method holds promise for the direct assay of uranium from ores/different oxide samples without the tedious chemical methods. (author)

  17. Biases during DNA extraction of activated sludge samples revealed by high throughput sequencing

    OpenAIRE

    Guo, Feng; Zhang, Tong

    2012-01-01

    Standardization of DNA extraction is a fundamental issue of fidelity and comparability in investigations of environmental microbial communities. Commercial kits for soil or feces are often adopted for studies of activated sludge because of a lack of specific kits, but they have never been evaluated regarding their effectiveness and potential biases based on high throughput sequencing. In this study, seven common DNA extraction kits were evaluated, based on not only yield/purity but also seque...

  18. Application of copolymer coated frits for solid-phase extraction of poly cyclic aromatic hydrocarbons in water samples.

    Science.gov (United States)

    Rahimi, M; Noroozian, E

    2014-07-11

    A conducting copolymer of pyrrole and phenol was electrochemically synthesized on steel frits as a sorbent. The applicability of the frit was assessed for the solid-phase extraction of trace amounts of polycyclic aromatic hydrocarbons (PAHs) in aqueous samples followed by HPLC-UV. The coating produced was very adherent and the scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and FTIR spectrum for the coated frit were studied. The effects of various parameters on the efficiency of the solid-phase extraction process, such as the sample loading rate, elution solvent type, salt effect, volume and flow rate of sample and elution solvent were investigated. Under the optimal conditions, the calibration curves were obtained in the range of 0.1-500ngmL(-1) (r(2)>0.98) and the LODs (S/N=3) were obtained in the range of 0.01-0.08ngmL(-1). Relative standard deviations (RSDs) for intra- and inter-day precision were 2.7-10.2% and 3.6-11.4%, respectively. The recoveries (8 and 40ngmL(-1)) ranged from 79% to 115%. The simplicity of experimental procedure, short sample analysis, high extraction efficiency, and the use of low-cost adsorbent show the potential of this method for routine analysis of PAHs in real samples. PMID:24974869

  19. Microcystin accumulation in cladocerans: first evidence of MC uptake from aqueous extracts of a natural bloom sample.

    Science.gov (United States)

    Ferrão-Filho, Aloysio S; Herrera, Natalia A; Echeverri, Luis Fernando

    2014-09-01

    Bioaccumulation of microcystins (MC) in zooplankton has been shown in several studies, mainly in field samples. A few studies, however, have demonstrated MC bioaccumulation in laboratory experiments. Although ingestion of cell-bound MC is considered the main route of MC accumulation, another important source is the MC from the dissolved fraction (DMC). This study reports the accumulation of DMC from aqueous extracts of natural bloom samples in three cladoceran species: Moina micrura, Daphnia laevis and Daphnia similis. Animals were exposed for 96 h to aqueous extracts of lyophilized matter from two bloom samples from Colombian reservoirs in different concentrations (25-1000 mg DW L(-1)). Analysis by HPLC-MS detected MC-LR in these samples at concentrations of 434-538 μg g(-1). For the analysis of MC in animal tissues the samples were homogenized and sonicated in methanol:water (75%) and analyzed by ELISA. Results showed that the animals uptake of MC increased with increasing exposure concentrations of aqueous extracts, with M. micrura and D. laevis clones presenting the highest MC concentrations in their tissues (up to 1170-1260 μg g(-1)) while D. similis the lowest (184 μg g(-1)). This study shows, for the first time, that MC uptake from dissolved fraction by zooplankton is possible, not only from the ingestion of seston or cell-bound MC as previously demonstrated. PMID:24880137

  20. Scheduling whole-air samples above the Trade Wind Inversion from SUAS using real-time sensors

    Science.gov (United States)

    Freer, J. E.; Greatwood, C.; Thomas, R.; Richardson, T.; Brownlow, R.; Lowry, D.; MacKenzie, A. R.; Nisbet, E. G.

    2015-12-01

    Small Unmanned Air Systems (SUAS) are increasingly being used in science applications for a range of applications. Here we explore their use to schedule the sampling of air masses up to 2.5km above ground using computer controlled bespoked Octocopter platforms. Whole-air sampling is targeted above, within and below the Trade Wind Inversion (TWI). On-board sensors profiled the TWI characteristics in real time on ascent and, hence, guided the altitudes at which samples were taken on descent. The science driver for this research is investigation of the Southern Methane Anomaly and, more broadly, the hemispheric-scale transport of long-lived atmospheric tracers in the remote troposphere. Here we focus on the practical application of SUAS for this purpose. Highlighting the need for mission planning, computer control, onboard sensors and logistics in deploying such technologies for out of line-of-sight applications. We show how such a platform can be deployed successfully, resulting in some 60 sampling flights within a 10 day period. Challenges remain regarding the deployment of such platforms routinely and cost-effectively, particularly regarding training and support. We present some initial results from the methane sampling and its implication for exploring and understanding the Southern Methane Anomaly.

  1. Radiostrontium separation and measurement in a single step using plastic scintillators plus selective extractants. Application to aqueous sample analysis

    Energy Technology Data Exchange (ETDEWEB)

    Bagan, H.; Tarancon, A.; Rauret, G. [Departament de Quimica Analitica, Universitat de Barcelona, Diagonal 647, E-08028 Barcelona (Spain); Garcia, J.F., E-mail: jfgarcia@ub.edu [Departament de Quimica Analitica, Universitat de Barcelona, Diagonal 647, E-08028 Barcelona (Spain)

    2011-02-07

    This study describes a new protocol for {sup 90}Sr determination in water samples based on the use of a selective extractant (DtBuCH18C6) and plastic scintillator microspheres. The proposed procedure unifies chemical separation and sample measurement preparation in a single step to reduce the effort, time and reagents required for analysis. In addition, the final measurement does not produce mixed waste. The minimum activity detectable for 10 mL of sample solution is 0.46 Bq L{sup -1}. Relative errors for the determination of {sup 90}Sr activity in drinking, sea and river waters are less than 4%.

  2. Radiostrontium separation and measurement in a single step using plastic scintillators plus selective extractants. Application to aqueous sample analysis

    International Nuclear Information System (INIS)

    This study describes a new protocol for 90Sr determination in water samples based on the use of a selective extractant (DtBuCH18C6) and plastic scintillator microspheres. The proposed procedure unifies chemical separation and sample measurement preparation in a single step to reduce the effort, time and reagents required for analysis. In addition, the final measurement does not produce mixed waste. The minimum activity detectable for 10 mL of sample solution is 0.46 Bq L-1. Relative errors for the determination of 90Sr activity in drinking, sea and river waters are less than 4%.

  3. The contents of fifteen essential, trace and toxic elements in some green tea samples and in their aqueous extracts

    International Nuclear Information System (INIS)

    The content of fifteen elements such as Ca, Mg, Na, K, Mn, Zn, Co, Cu, Cr, Ni, Pd, Cd, Ba and Al were determined in Green Tea samples imported from different countries such as India, China, Kenya and Bangladesh in packets and without packets were purchased from authorized tea dealers in Peshawar. Wet ashing procedures were employed for decomposing the organic matter in the tea samples. Aqueous extract of each green tea sample was also prepared by heating with de-ionized water at 80 /sup o/C on electric heating plates. (author)

  4. APPLICATION OF STIR BAR SORPTIVE EXTRACTION TO ANALYSIS OF VOLATILE AND SEMIVOLATILE ORGANIC CHEMICALS OF POTENTIAL CONCERN IN SOLIDS AND AQUEOUS SAMPLES FROM THE HANFORD SITE

    Energy Technology Data Exchange (ETDEWEB)

    FRYE JM; KUNKEL JM

    2009-03-05

    Stir bar sorptive extraction was applied to aqueous and solid samples for the extraction and analysis of organic compounds from the Hanford chemicals of potential concern list, as identified in the vapor data quality objectives. The 222-S Laboratory analyzed these compounds from vapor samples on thermal desorption tubes as part of the Hanford Site industrial hygiene vapor sampling effort.

  5. Review of Methods for Calculating Pressure Profiles of Explosive Air Blast and its Sample Application

    OpenAIRE

    Chock, Jeffrey Mun Kong

    1999-01-01

    Blast profiles and two primary methods of determining them were reviewed for use in the creation of a computer program for calculating blast pressures which serves as a design tool to aid engineers or analysts in the study of structures subjected to explosive air blast. These methods were integrated into a computer program, BLAST.F, to generate air blast pressure profiles by one of these two differing methods. These two methods were compared after the creation of the program and can conserv...

  6. A Predictive Model for Vehicle Air Exchange Rates based on a Large, Representative Sample

    OpenAIRE

    Fruin, Scott A.; Hudda, Neelakshi; Sioutas, Constantinos; Delfino, Ralph J.

    2011-01-01

    The in-vehicle microenvironment is an important route of exposure to traffic-related pollutants, particularly ultrafine particles. However, significant particle losses can occur under conditions of low air exchange rate (AER) when windows are closed and air is recirculating. AERs are lower for newer vehicles and at lower speeds. Despite the importance of AER in affecting in-vehicle particle exposures, few studies have characterized AER and all have tested only a small number of cars. One reas...

  7. Evaluation of DNA extraction techniques for detecting Mycobacterium tuberculosis complex organisms in Asian elephant trunk wash samples.

    Science.gov (United States)

    Kay, Meagan K; Linke, Lyndsey; Triantis, Joni; Salman, M D; Larsen, R Scott

    2011-02-01

    Rapid and sensitive diagnostic assays for the detection of tuberculous mycobacteria in elephants are lacking. DNA extraction with PCR analysis is useful for tuberculosis screening in many species but has not been validated on elephant trunk wash samples. We estimated the analytical sensitivity and specificity of three DNA extraction methods to detect Mycobacterium tuberculosis complex organisms in trunk wash specimens. A ZR soil microbe DNA kit (ZR) and a traditional salt and ethanol precipitation (TSEP) approach were evaluated under three different treatment conditions: heat treatment, phenol treatment, and contamination with Mycobacterium avium. A third approach, using a column filtration method, was evaluated for samples contaminated with soil. Trunk wash samples from uninfected elephants were spiked with various concentrations of M. bovis cells and subjected to the described treatment conditions prior to DNA extraction. Extracted DNA was amplified using IS6110-targeted PCR analysis. The ZR and TSEP methods detected as low as 1 to 5 M. bovis cells and 10 M. bovis cells, respectively, per 1.5 ml of trunk wash under all three conditions. Depending on the amount of soil present, the column filtration method detected as low as 5 to 50 M. bovis cells per 1.5 ml of trunk wash. Analytical specificity was assessed by DNA extraction from species of nontuberculous mycobacteria and amplification using the same PCR technique. Only M. bovis DNA was amplified, indicating 100% analytical specificity of this PCR technique. Our results indicate that these DNA extraction techniques offer promise as useful tests for detection of M. tuberculosis complex organisms in elephant trunk wash specimens. PMID:21159933

  8. Automated on-line liquid-liquid extraction system for temporal mass spectrometric analysis of dynamic samples.

    Science.gov (United States)

    Hsieh, Kai-Ta; Liu, Pei-Han; Urban, Pawel L

    2015-09-24

    Most real samples cannot directly be infused to mass spectrometers because they could contaminate delicate parts of ion source and guides, or cause ion suppression. Conventional sample preparation procedures limit temporal resolution of analysis. We have developed an automated liquid-liquid extraction system that enables unsupervised repetitive treatment of dynamic samples and instantaneous analysis by mass spectrometry (MS). It incorporates inexpensive open-source microcontroller boards (Arduino and Netduino) to guide the extraction and analysis process. Duration of every extraction cycle is 17 min. The system enables monitoring of dynamic processes over many hours. The extracts are automatically transferred to the ion source incorporating a Venturi pump. Operation of the device has been characterized (repeatability, RSD = 15%, n = 20; concentration range for ibuprofen, 0.053-2.000 mM; LOD for ibuprofen, ∼0.005 mM; including extraction and detection). To exemplify its usefulness in real-world applications, we implemented this device in chemical profiling of pharmaceutical formulation dissolution process. Temporal dissolution profiles of commercial ibuprofen and acetaminophen tablets were recorded during 10 h. The extraction-MS datasets were fitted with exponential functions to characterize the rates of release of the main and auxiliary ingredients (e.g. ibuprofen, k = 0.43 ± 0.01 h(-1)). The electronic control unit of this system interacts with the operator via touch screen, internet, voice, and short text messages sent to the mobile phone, which is helpful when launching long-term (e.g. overnight) measurements. Due to these interactive features, the platform brings the concept of the Internet-of-Things (IoT) to the chemistry laboratory environment. PMID:26423626

  9. Fast low-pressurized microwave-assisted extraction of benzotriazole, benzothiazole and benezenesulfonamide compounds from soil samples.

    Science.gov (United States)

    Speltini, Andrea; Sturini, Michela; Maraschi, Federica; Porta, Alessio; Profumo, Antonella

    2016-01-15

    Benzotriazoles (BTRs), benzothiazoles (BTs) and benzenesulfonamides (BSAs), compounds largely used in industrial and household applications, are ubiquitous emerging contaminants. In this work a novel, straightforward procedure for the simultaneous determination of two BTRs (1H-benzotriazole, 5-methyl-1H-benzotriazole), three BTs (benzothiazole, 2-hydroxybenzothiazole, 2-methylthiobenzothiazole) and two BSAs (benzenesulfonamide, toluenesulfonamide) in soil has been developed. The target analytes were extracted from soil by a single low-pressurized microwave-assisted extraction (MAE) cycle (120°C, 10min) and quantified by high-performance liquid chromatography with UV detection. For all the seven analytes, quantitative extraction yields (72-119%, n=4) were observed from recovery tests on soil samples (1g) spiked with 5, 10 and 50mg kg(-1), using 4mL water-methanol (85:15) as extracting solution. For the lower concentrations levels (100, 250 and 500μg kg(-1)), the analytes were extracted from soil samples (2-3g) using 6mL methanol, and the extract was pre-concentrated by evaporation before analysis; recoveries in the range 70-117% were obtained (n=4). Suitable intra-day and inter-day precision were observed, with values of relative standard deviation generally below 6% and 11% (n=4), respectively. Linearity was evaluated in the concentration range 0.5-10mg L(-1) by matrix-matched standards, obtaining r(2)>0.9996. The experimental method quantification limit (MQL) was 100μg kg(-1). The entire procedure has been successfully applied to the analysis of real impacted soil samples. PMID:26592614

  10. Sequential extraction procedure for determination of uranium, thorium, radium, lead and polonium radionuclides by alpha spectrometry in environmental samples

    International Nuclear Information System (INIS)

    A sequential extraction technique was developed and tested for common naturally-occurring radionuclides. This technique allows the extraction and purification of uranium, thorium, radium, lead, and polonium radionuclides from the same sample. Environmental materials such as water, soil, and biological samples can be analyzed for those radionuclides without matrix interferences in the quality of radioelement purification and in the radiochemical yield. The use of isotopic tracers (232U, 229Th, 224Ra, 209Po, and stable lead carrier) added to the sample in the beginning of the chemical procedure, enables an accurate control of the radiochemical yield for each radioelement. The ion extraction procedure, applied after either complete dissolution of the solid sample with mineral acids or co-precipitation of dissolved radionuclide with MnO2 for aqueous samples, includes the use of commercially available pre-packed columns from Eichrom(r) and ion exchange columns packed with Bio-Rad resins, in altogether three chromatography columns. All radioactive elements but one are purified and electroplated on stainless steel discs. Polonium is spontaneously plated on a silver disc. The discs are measured using high resolution silicon surface barrier detectors. 210Pb, a beta emitter, can be measured either through the beta emission of 210Bi, or stored for a few months and determined by alpha spectrometry through the in-growth of 210Po. This sequential extraction chromatography technique was tested and validated with the analysis of certified reference materials from the IAEA. Reproducibility was tested through repeated analysis of the same homogeneous material (water sample). (author)

  11. Determination of the distribution and speciation of selenium in an argillaceous sample using chemical extractions and post-extractions analyses: application to the hydrogeological experimental site of Poitiers.

    Science.gov (United States)

    Bassil, Joseph; Naveau, Aude; Bueno, Maïté; Di Tullo, Pamela; Grasset, Laurent; Kazpard, Véronique; Razack, Moumtaz

    2016-05-01

    To better understand selenium's dynamics in environmental systems, the present study aims to investigate selenium speciation and distribution in black argillaceous sediments, partially fulfilling karstic cavities into the Hydrogeological Experimental Site of Poitiers. These sediments are suspected to be responsible for selenium concentrations exceeding the European Framework Directive's drinking water limit value (10 μg L(-1)) in some specific wells. A combination of a sequential extractions scheme and single parallel extractions was thus applied on a representative argillaceous sample. Impacts of the extractions on mineral dissolution and organic matter mobilization were followed by quantifying major cations and total organic carbon (TOC) in the aqueous extracts. The nature of the released organic matter was characterized using thermochemolysis coupled with gas chromatography-mass spectrometry (GC-MS). About 10 % of selenium from the black argillaceous studied matrix could be defined as 'easily mobilizable' when the majority (around 70 %) revealed associated with the aliphatic and alkaline-soluble organic matter's fraction (about 20 %). In these fractions, selenium speciation was moreover dominated by oxidized species including a mixture of Se(VI) (20-30 %) and Se(IV) (70-80 %) in the 'easily mobilizable' fraction, while only Se(IV) was detected in alkaline-soluble organic matter fraction. PMID:26846236

  12. Extraction of Aflatoxins from Liquid Foodstuff Samples with Polydopamine-Coated Superparamagnetic Nanoparticles for HPLC-MS/MS Analysis

    OpenAIRE

    McCullum, Cassandra; Tchounwou, Paul; Ding, Li-Sheng; Liao, Xun; Liu, Yi-Ming

    2014-01-01

    A facile magnetic solid phase extraction (MSPE) of aflatoxins (AFs) from liquid samples was developed using polydopamine-coated magnetic nanoparticles (PD-MNPs) as the adsorbent. PD-MNPs were prepared from amine-terminated MNPs and dopamine via an in situ oxidative self-polymerization approach. Under the selected MSPE conditions, extraction yields ranging from 59.3% for AF G2 to 89.0% for AF B1 were obtained with good repeatability. Coupled with HPLC-MS/MS quantification, the MSPE procedure s...

  13. A sensitive method based on HDEHP extraction and LSS for the determination of 90Sr in solid samples

    International Nuclear Information System (INIS)

    An improved and rapid method is described for the determination of 90Sr in environmental samples, through the separation of the daughter 90Y at equilibrium. The procedure is based on the HDEHP solvent extraction in combination with liquid scintillation spectrometry (LSS). A low background QuantulusTM has been optimized for low level counting of Cerenkov radiation emitted by the hard β-emitter 90Y. The counting efficiency was 60% and the background 0.53 cqm. The reliability and reproducibility of the method have been checked using IAEA reference materials. The chemical recovery for 90Y extraction ranges from 83 to 90%. (author)

  14. Molecular Threading: Mechanical Extraction, Stretching and Placement of DNA Molecules from a Liquid-Air Interface

    OpenAIRE

    Payne, Andrew C.; Andregg, Michael; Kemmish, Kent; Hamalainen, Mark; Bowell, Charlotte; Bleloch, Andrew; Klejwa, Nathan; Lehrach, Wolfgang; Schatz, Ken; Stark, Heather; Marblestone, Adam; Church, George; Own, Christopher S.; Andregg, William

    2013-01-01

    We present “molecular threading”, a surface independent tip-based method for stretching and depositing single and double-stranded DNA molecules. DNA is stretched into air at a liquid-air interface, and can be subsequently deposited onto a dry substrate isolated from solution. The design of an apparatus used for molecular threading is presented, and fluorescence and electron microscopies are used to characterize the angular distribution, straightness, and reproducibility of stretched DNA depos...

  15. Simultaneous Determination of TetracyclinesResidues in Bovine Milk Samples by Solid Phase Extraction and HPLC-FL Method

    Directory of Open Access Journals (Sweden)

    Mehra Mesgari Abbasi

    2011-06-01

    Full Text Available Introduction:Tetracyclines (TCs are widely used in animal husbandry and their residues in milk may resultinharmful effects on human. The aim of this study was to investigate the presence of TCs residues in various bovine milk samples from local markets of Ardabil, Iran. Methods:One hundred and fourteen pasteurized, sterilized and raw milk samples were collected from markets of Ardabil. Tetracycline, Oxytetracycline and Chlortetracycline (TCs residues extraction carried out by Solid Phase Extraction method. Determination of TCs residues were performed by high performance liquid chromatography (HPLC method using Fluorescence detector.Results: The mean of total TCs residues in all samples (114 samples was 97.6 ±16.9ng/g and that of pasteurized, sterilized and raw milk samples were 87.1 ± 17.7, 112.0 ± 57.3 and 154.0 ± 66.3ng/g respectively. Twenty five point four percent of the all samples, and24.4%, 30% and 28.6% of the pasteurized, sterilized and raw milk samples, respectively had higher TCs residues than the recommended maximum levels (100ng/g. Conclusion:This study indicates the presence of tetracycline residues more than allowed amount. Regulatory authorities should ensure proper withdrawal period before milking the animals and definite supervisions are necessary on application of these drugs.

  16. Combined in-situ and ex-situ bioremediation of petroleum hydrocarbon contaminated soils by closed-loop soil vapor extraction and air injection

    International Nuclear Information System (INIS)

    Treatment and restoration of petroleum hydrocarbon contaminated soils at a bulk petroleum above-ground storage tank (AST) site in Michigan is being conducted through in-situ and ex-situ closed-loop soil vapor extraction (SVE), soil vapor treatment, and treated air injection (AI) processes. The soil vapor extraction process applies a vacuum through the petroleum hydrocarbon affected soils in the ex-situ bio-remediation pile (bio-pile) and along the perimeter of excavated area (in-situ area) to remove the volatile or light petroleum hydrocarbons. This process also draws ambient air into the ex-situ bio-pile and in-situ vadose zone soil along the perimeter of excavated area to enhance biodegradation of light and heavy petroleum hydrocarbons in the soil. The extracted soil vapor is treated using a custom-designed air bio-remediation filter (bio-filter) to degrade the petroleum hydrocarbon compounds in the soil vapor extraction air streams. The treated air is then injected into a flush grade soil bed in the backfill area to perform final polishing of the air stream, and to form a closed-loop air flow with the soil vapor extraction perforated pipes along the perimeter of the excavated area

  17. Air

    Science.gov (United States)

    ... house) Industrial emissions (like smoke and chemicals from factories) Household cleaners (spray cleaners, air fresheners) Car emissions (like carbon monoxide) *All of these things make up “particle pollution.” They mostly come from cars, trucks, buses, and ...

  18. A validation of extraction methods for noninvasive sampling of glucocorticoids in free-living ground squirrels.

    Science.gov (United States)

    Mateo, Jill M; Cavigelli, Sonia A

    2005-01-01

    Fecal hormone assays provide a powerful tool for noninvasive monitoring of endocrine status in wild animals. In this study we validated a protocol for extracting and measuring glucocorticoids in free-living and captive Belding's ground squirrels (Spermophilus beldingi). We first compared two commonly used extraction protocols to determine which performed better with commercially available antibodies. We next verified the preferred extraction method by correlating circulating and fecal glucocorticoid measures from a group of individuals over time. For this comparison, we used both a cortisol and a corticosterone antibody to determine which had greater affinity to the fecal metabolites. Cortisol was the primary circulating glucocorticoid, but both hormones were present in well above detectable concentrations in the blood, which does not occur in other sciurids. In addition, the cortisol antibody showed greater binding with the fecal extracts than did the corticosterone antibody. Finally, we used adrenocorticotropic hormone and dexamethasone challenges to demonstrate that changes in adrenal functioning are reflected in changing fecal corticoid levels. These results suggest that our extraction protocol provides a fast, reliable assay of stress hormones in free-living ground squirrels without the confounding influence of short-term rises in glucocorticoid concentrations caused by handling and restraint stress and that it can facilitate ecological and evolutionary studies of stress in wild species. PMID:16228945

  19. Extraction, isolation, and purification of analytes from samples of marine origin--a multivariate task.

    Science.gov (United States)

    Liguori, Lucia; Bjørsvik, Hans-René

    2012-12-01

    The development of a multivariate study for a quantitative analysis of six different polybrominated diphenyl ethers (PBDEs) in tissue of Atlantic Salmo salar L. is reported. An extraction, isolation, and purification process based on an accelerated solvent extraction system was designed, investigated, and optimized by means of statistical experimental design and multivariate data analysis and regression. An accompanying gas chromatography-mass spectrometry analytical method was developed for the identification and quantification of the analytes, BDE 28, BDE 47, BDE 99, BDE 100, BDE 153, and BDE 154. These PBDEs have been used in commercial blends that were used as flame-retardants for a variety of materials, including electronic devices, synthetic polymers and textiles. The present study revealed that an extracting solvent mixture composed of hexane and CH₂Cl₂ (10:90) provided excellent recoveries of all of the six PBDEs studied herein. A somewhat lower polarity in the extracting solvent, hexane and CH₂Cl₂ (40:60) decreased the analyte %-recoveries, which still remain acceptable and satisfactory. The study demonstrates the necessity to perform an intimately investigation of the extraction and purification process in order to achieve quantitative isolation of the analytes from the specific matrix. PMID:22840418

  20. Microwave-assisted extraction of pyrethroid insecticides from semi permeable membrane devices (SPMDs) used to indoor air monitoring

    International Nuclear Information System (INIS)

    A rapid and environmentally friendly methodology was developed for the extraction of pyrethroid insecticides from semi permeable membrane devices (SPMDs), in which they were preconcentrated in gas phase. The method was based on gas chromatography mass-mass spectrometry determination after a microwave-assisted extraction, in front of the widely employed dialysis method. SPMDs were extracted twice with 30 mL hexane:acetone, irradiated with 250 W power output, until 90 deg. C in 10 min, this temperature being held for another 10 min. Clean-up of the extracts was performed by acetonitrile-hexane partitioning and solid-phase extraction (SPE) with a combined cartridge of 2 g basic-alumina, deactivated with 5% water, and 500 mg C18. Pyrethroids investigated were Allethrin, Prallethrin, Tetramethrin, Bifenthrin, Phenothrin, λ-Cyhalothrin, Permethrin, Cyfluthrin, Cypermethrin, Flucythrinate, Esfenvalerate, Fluvalinate and Deltamethrin. The main pyrethroid synergist compound, Pyperonyl Butoxide, was also studied. Limit of detection values ranging from 0.3 to 0.9 ng/SPMD and repeatability data, as relative standard deviation, from 2.9 to 9.4%, were achieved. Pyrethroid recoveries, for spiked SPMDs, with 100 ng of each one of the pyrethroids evaluated, were from 61 ± 8 to 103 ± 7% for microwave-assisted extraction, versus 54 ± 4 to 104 ± 3% for dialysis reference method. Substantial reduction of solvent consumed (from 400 to 60 mL) and analysis time (from 48 to 1 h) was achieved by using the developed procedure. High concentration levels of pyrethroid compounds, from 0.14 to 7.3 μg/SPMD, were found in indoor air after 2 h of a standard application

  1. Air sampling system for evaluating the thyroid dose commitment due to fission products released from reactor containment. Final report

    International Nuclear Information System (INIS)

    Accidental releases of radioactivity from fission reactors will consist of active vapors and aerosols. Composition of the released plume or cloud will depend on the energy of release and fission product volatility. In accidents at Windscale and SL-1, 131I was the predominant isotope present in both the initial cloud and later release. Thus an air sampling system was developed for efficient radioiodine collection. The air sampling, readout, and dose assessment system was developed to be used in the environment after loss of containment accidents. The system can detect less than 1 rem dose commitments to thyroids of 5 year old children for immersion times of 10 hours or less. The air mover can be operated on either 110V ac power or 12V dc power available from vehicles with cigar lighter sockets. An inorganic silver loaded silica gel adsorber was developed for high mehyl iodine, HOI, and elemental iodine efficiency and low noble gas efficiency. A peal away high efficiency particulate filter permits the gaseous and particulate sample fractions to be evaluated separately. Predicted particulate iodine is combined with the adsorbed component to account for the total radioiodine in a given sample

  2. The lung cancer breath signature: a comparative analysis of exhaled breath and air sampled from inside the lungs

    Science.gov (United States)

    Capuano, Rosamaria; Santonico, Marco; Pennazza, Giorgio; Ghezzi, Silvia; Martinelli, Eugenio; Roscioni, Claudio; Lucantoni, Gabriele; Galluccio, Giovanni; Paolesse, Roberto; di Natale, Corrado; D'Amico, Arnaldo

    2015-11-01

    Results collected in more than 20 years of studies suggest a relationship between the volatile organic compounds exhaled in breath and lung cancer. However, the origin of these compounds is still not completely elucidated. In spite of the simplistic vision that cancerous tissues in lungs directly emit the volatile metabolites into the airways, some papers point out that metabolites are collected by the blood and then exchanged at the air-blood interface in the lung. To shed light on this subject we performed an experiment collecting both the breath and the air inside both the lungs with a modified bronchoscopic probe. The samples were measured with a gas chromatography-mass spectrometer (GC-MS) and an electronic nose. We found that the diagnostic capability of the electronic nose does not depend on the presence of cancer in the sampled lung, reaching in both cases an above 90% correct classification rate between cancer and non-cancer samples. On the other hand, multivariate analysis of GC-MS achieved a correct classification rate between the two lungs of only 76%. GC-MS analysis of breath and air sampled from the lungs demonstrates a substantial preservation of the VOCs pattern from inside the lung to the exhaled breath.

  3. The Use of Features Extracted from Noisy Samples for Image Restoration Purposes

    Directory of Open Access Journals (Sweden)

    2007-01-01

    Full Text Available An important feature of neural networks is the ability they have to learn from their environment, and, through learning to improve performance in some sense. In the following we restrict the development to the problem of feature extracting unsupervised neural networks derived on the base of the biologically motivated Hebbian self-organizing principle which is conjectured to govern the natural neural assemblies and the classical principal component analysis (PCA method used by statisticians for almost a century for multivariate data analysis and feature extraction. The research work reported in the paper aims to propose a new image reconstruction method based on the features extracted from the noise given by the principal components of the noise covariance matrix.

  4. Speciation of Chromium in Water Samples with Homogeneous Liquid-Liquid Extraction and Determination by Flame Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    A novel method was developed for the speciation of chromium in natural water samples based on homogeneous liquid-liquid extraction and determination by flame atomic absorption spectrometry (FAAS). In this method, Cr(III) reacts with a new Schiff's base ligand to form the hydrophobic complex, which is subsequently entrapped in the sediment phase, whereas Cr(VI) remained in aqueous phase. The Cr(VI) assay is based on its reduction to Cr(III) by the addition of sodium sulfite to the sample solution. Thus, separation of Cr(III) and Cr(VI) could be realized. Homogeneous liquid-liquid extraction based on the pH-independent phase-separation process was investigated using a ternary solvent system (water-tetrabutylammonium ion (TBA+)-chloroform) for the preconcentration of chromium. The phase separation phenomenon occurred by an ion-pair formation of TBA and perchlorate ion. Then sedimented phase was separated using a 100 μL micro-syringe and diluted to 1.0 mL with ethanol. The sample was introduced into the flame by conventional aspiration. After the optimization of complexation and extraction conditions such as pH = 9.5, [ligand] = 1.0 x 10-4 M, [TBA+] = 2.0 x 10-2 M, [CHCl3] = 100.0 μL and [ClO4-] = 2.0 x 10-2 M, a preconcentration factor (Va/Vs) of 100 was obtained for only 10 mL of the sample. The relative standard deviation was 2.8% (n = 10). The limit of detection was sufficiently low and lie at ppb level. The proposed method was applied for the extraction and determination of chromium in natural water samples with satisfactory results

  5. Application of copolymer coated frits for solid-phase extraction of poly cyclic aromatic hydrocarbons in water samples

    Energy Technology Data Exchange (ETDEWEB)

    Rahimi, M., E-mail: m_rahimi543@yahoo.com [Department of Chemistry, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Young Researchers Society, Shahid Bahonar University of Kerman, P.O. Box 76169–133, Kerman (Iran, Islamic Republic of); Noroozian, E. [Department of Chemistry, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

    2014-07-11

    Graphical abstract: Electrodeposition and using of the copolymer of pyrrole and phenol for frit-SPE for the enrichment of organic pollutants from real samples and HPLC–UV analysis. - Highlights: • A copolymer of pyrrole and phenol was electrosynthesised on steel frit. • Coated frit was used for the first time as a SPE sorbent for PAHs in real samples. • Using the designed device was simple and it needs no vacuum or pressure system. - Abstract: A conducting copolymer of pyrrole and phenol was electrochemically synthesized on steel frits as a sorbent. The applicability of the frit was assessed for the solid-phase extraction of trace amounts of polycyclic aromatic hydrocarbons (PAHs) in aqueous samples followed by HPLC–UV. The coating produced was very adherent and the scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and FTIR spectrum for the coated frit were studied. The effects of various parameters on the efficiency of the solid-phase extraction process, such as the sample loading rate, elution solvent type, salt effect, volume and flow rate of sample and elution solvent were investigated. Under the optimal conditions, the calibration curves were obtained in the range of 0.1–500 ng mL{sup −1} (r{sup 2} > 0.98) and the LODs (S/N = 3) were obtained in the range of 0.01–0.08 ng mL{sup −1}. Relative standard deviations (RSDs) for intra- and inter-day precision were 2.7–10.2% and 3.6–11.4%, respectively. The recoveries (8 and 40 ng mL{sup −1}) ranged from 79% to 115%. The simplicity of experimental procedure, short sample analysis, high extraction efficiency, and the use of low-cost adsorbent show the potential of this method for routine analysis of PAHs in real samples.

  6. Development and practical application of accelerated solvent extraction for the isolation of cocaine/crack biomarkers in meconium samples.

    Science.gov (United States)

    Mantovani, Cínthia de Carvalho; Lima, Marcela Bittar; Oliveira, Carolina Dizioli Rodrigues de; Menck, Rafael de Almeida; Diniz, Edna Maria de Albuquerque; Yonamine, Mauricio

    2014-04-15

    A method using accelerated solvent extraction (ASE) for the isolation of cocaine/crack biomarkers in meconium samples, followed by solid phase extraction (SPE) and the simultaneous quantification by gas chromatography-mass spectrometry (GC-MS) was developed and validated. Initially, meconium samples were submitted to an ASE procedure, which was followed by SPE with Bond Elut Certify I cartridges. The analytes were derivatizated with PFP/PFPA and analyzed by GC-MS. The limits of detection (LOD) were between 11 and 17ng/g for all analytes. The limits of quantification (LOQ) were 30ng/g for anhydroecgonine methyl ester, and 20ng/g for cocaine, benzoylecgonine, ecgonine methyl ester and cocaethylene. Linearity ranged from the LOQ to 1500ng/g for all analytes, with a coefficients of determination greater than 0.991, except for m-hydroxybenzoylecgonine, which was only qualitatively detected. Precision and accuracy were evaluated at three concentration levels. For all analytes, inter-assay precision ranged from 3.2 to 18.1%, and intra-assay precision did not exceed 12.7%. The accuracy results were between 84.5 and 114.2% and the average recovery ranged from 17 to 84%. The method was applied to 342 meconium samples randomly collected in the University Hospital-University of São Paulo (HU-USP), Brazil. Cocaine biomarkers were detected in 19 samples, which represent 5.6% of exposure prevalence. Significantly lower birth weight, length and head circumference were found for the exposed newborns compared with the non-exposed group. This is the first report in which ASE was used as a sample preparation technique to extract cocaine biomarkers from a complex biological matrix such as meconium samples. The advantages of the developed method are the smaller demand for organic solvents and the minor sample handling, which allows a faster and accurate procedure, appropriate to confirm fetal exposure to cocaine/crack. PMID:24657406

  7. SAMPLE RESULTS FROM THE NEXT GENERATION SOLVENT PROGRAM REAL WASTE EXTRACTION-SCRUB-STRIP TESTING

    Energy Technology Data Exchange (ETDEWEB)

    Peters, T.; Washington, A.

    2013-06-03

    Savannah River National Laboratory (SRNL) performed multiple Extraction-Scrub-Strip (ESS) testing using real waste solutions, and three Next Generation Solvent (NGS) variations, which included radiologically clean pure NGS, a blend of radiologically clean NGS and radiologically clean BOBCalixC6 (NGS-MCU), and a blend of radiologically clean NGS and radiologically contaminated BOBCalixC6 from the MCU Solvent system. The results from the tests indicate that both the NGS and the NGS-MCU blend exhibit adequate extraction, scrub and strip behavior.

  8. Sample Results From The Next Generation Solvent Program Real Waste Extraction-Scrub-Strip Testing

    Energy Technology Data Exchange (ETDEWEB)

    Peters, T. B.; Washington, A. L. II

    2013-08-08

    Savannah River National Laboratory (SRNL) performed multiple Extraction-Scrub-Strip (ESS) testing using real waste solutions, and three Next Generation Solvent (NGS) variations, which included radiologically clean pure NGS, a blend of radiologically clean NGS and radiologically clean BOBCalixC6 (NGS-MCU), and a blend of radiologically clean NGS and radiologically contaminated BOBCalixC6 from the MCU Solvent system. The results from the tests indicate that both the NGS and the NGS-MCU blend exhibit adequate extraction, scrub and strip behavior.

  9. Selective solid-phase extraction of Ni(II) by an ion-imprinted polymer from water samples

    Energy Technology Data Exchange (ETDEWEB)

    Saraji, Mohammad, E-mail: saraji@cc.iut.ac.ir [Department of Chemistry, Isfahan University of Technology, Isfahan 84154-83111 (Iran, Islamic Republic of); Yousefi, Hamideh [Department of Chemistry, Isfahan University of Technology, Isfahan 84154-83111 (Iran, Islamic Republic of)

    2009-08-15

    A new ion-imprinted polymer (IIP) material was synthesized by copolymerization of 4-vinylpyridine as monomer, ethyleneglycoldimethacrylate as crosslinking agent and 2,2'-azobis-sobutyronitrile as initiator in the presence of Ni-dithizone complex. The IIP was used as sorbent in a solid-phase extraction column. The effects of sampling volume, elution conditions, sample pH and sample flow rate on the extraction of Ni ions form water samples were studied. The maximum adsorption capacity and the relative selectivity coefficients of imprinted polymer for Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were calculated. Compared with non-imprinted polymer particles, the IIP had higher selectivity for Ni(II). The relative selectivity factor ({alpha}{sub r}) values of Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were 21.6, 54.3, and 22.7, respectively, which are greater than 1. The relative standard deviation of the five replicate determinations of Ni(II) was 3.4%. The detection limit for 150 mL of sample was 1.6 {mu}g L{sup -1} using flame atomic absorption spectrometry. The developed method was successfully applied to the determination of trace nickel in water samples with satisfactory results.

  10. Inverse supercritical fluid extraction as a sample preparation method for the analysis of the nanoparticle content in sunscreen agents.

    Science.gov (United States)

    Müller, David; Cattaneo, Stefano; Meier, Florian; Welz, Roland; de Vries, Tjerk; Portugal-Cohen, Meital; Antonio, Diana C; Cascio, Claudia; Calzolai, Luigi; Gilliland, Douglas; de Mello, Andrew

    2016-04-01

    We demonstrate the use of inverse supercritical carbon dioxide (scCO2) extraction as a novel method of sample preparation for the analysis of complex nanoparticle-containing samples, in our case a model sunscreen agent with titanium dioxide nanoparticles. The sample was prepared for analysis in a simplified process using a lab scale supercritical fluid extraction system. The residual material was easily dispersed in an aqueous solution and analyzed by Asymmetrical Flow Field-Flow Fractionation (AF4) hyphenated with UV- and Multi-Angle Light Scattering detection. The obtained results allowed an unambiguous determination of the presence of nanoparticles within the sample, with almost no background from the matrix itself, and showed that the size distribution of the nanoparticles is essentially maintained. These results are especially relevant in view of recently introduced regulatory requirements concerning the labeling of nanoparticle-containing products. The novel sample preparation method is potentially applicable to commercial sunscreens or other emulsion-based cosmetic products and has important ecological advantages over currently used sample preparation techniques involving organic solvents. PMID:26931426

  11. Selective solid-phase extraction of Ni(II) by an ion-imprinted polymer from water samples

    International Nuclear Information System (INIS)

    A new ion-imprinted polymer (IIP) material was synthesized by copolymerization of 4-vinylpyridine as monomer, ethyleneglycoldimethacrylate as crosslinking agent and 2,2'-azobis-sobutyronitrile as initiator in the presence of Ni-dithizone complex. The IIP was used as sorbent in a solid-phase extraction column. The effects of sampling volume, elution conditions, sample pH and sample flow rate on the extraction of Ni ions form water samples were studied. The maximum adsorption capacity and the relative selectivity coefficients of imprinted polymer for Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were calculated. Compared with non-imprinted polymer particles, the IIP had higher selectivity for Ni(II). The relative selectivity factor (αr) values of Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were 21.6, 54.3, and 22.7, respectively, which are greater than 1. The relative standard deviation of the five replicate determinations of Ni(II) was 3.4%. The detection limit for 150 mL of sample was 1.6 μg L-1 using flame atomic absorption spectrometry. The developed method was successfully applied to the determination of trace nickel in water samples with satisfactory results.

  12. Air oxidation of samples from different clay formations of East Paris basin: quantitative and qualitative consequences on the dissolved organic matter

    International Nuclear Information System (INIS)

    Document available in extended abstract form only. During the excavation and the building of an underground research laboratory in clay geological formations, exposure to air is one of the most important parameters affecting the composition of fossil organic matter. Indeed the net effect of air oxidation of the organic matter is enrichment in oxygen and carbon combined with a loss of hydrogen. Effluents formed are CO2 and water as well as the liberation of hydrocarbons. This process may have an impact on water chemistry of the clay, especially on the quantity and composition of Dissolved Organic Matter (DOM). The clays studied were the following and may be distinguished on the basis of their organic matter content: - The Callovo-Oxfordian argillite, collected in the Bure Underground Research Laboratory (Meuse, France), which contains a mixture of type II and III kerogen; - The Toarcian shales of East Paris Basin collected from drilling EST 204 (Meuse, France) contains type II kerogen; - The Kimmeridgian shales of East Paris Basin collected from drilling HTM 102 (Meuse, France) also contains type II kerogen. The powdered clay samples were oxidized in a ventilated oven at 100 C under air flow during 2, 256, 512 and 1088 hours for Callovo-Oxfordian samples and during 512 and 2048 hours for Toarcian and Kimmeridgian samples. The DOM of each sample was extracted by soxhlet using pure water. Different analyses were carried out: - Quantitative evolution of DOM with the oxidation process; - Evolution of several chemical parameters of DOM with oxidation using molecular analyses (PyGC-MS) molecular weight distribution (GPC-HPLC) as well as spectroscopic measurements (3D-Fluorescence). Increasing oxidation induces an increase of DOC values for all samples. Also, Changes in the chemical composition of the DOM are observed: decrease in the molecular weight range; enrichment in acidic functional groups (alkane-dioic acids, alkanoic acids, aromatics poly acids). Moreover the

  13. Fabric phase sorptive extraction: An innovative sample preparation approach applied to the analysis of specific migration from food packaging.

    Science.gov (United States)

    Aznar, M; Alfaro, P; Nerin, C; Kabir, A; Furton, K G

    2016-09-14

    Additives added to food packaging materials can migrate to food in contact with them during storage and shelf life. A novel simple, fast and sensitive analyte extraction method based on fabric phase sorptive extraction (FPSE), followed by analysis using ultra-high performance liquid chromatography and mass spectrometry detection (UPLC-MS) was applied to the analysis of 18 common non-volatile plastic additives. Three FPSE media coated with different sol-gel sorbents characterized with different polarities including sol-gel poly(dimethylsiloxane), sol-gel poly(ethylene glycol) and sol-gel poly(tetrahydrofuran) were studied. All three FPSE media showed very satisfactory results. In general, compounds with low logP values seemed to have higher enrichment factors (EFs), especially with poly(tetrahydrofuran) and poly(ethylene glycol) media. For compounds with high logP values, the use of sol-gel poly(dimethylsiloxane) improved the enrichment capacity. Sample preparation time was optimized at 20 min for sample extraction and 10 min for solvent desorption. Acetonitrile was selected as desorption solvent since recoveries were over 70% for 13 out of 18 selected compounds in all FPSE media. The best extraction recovery values were obtained when compounds were dissolved in aqueous acetic acid solution (3%), where 17 out of 18 compounds showed improvement in their signal intensity after FPSE extraction and 10 obtained enrichment factors above 3 for all the tested FPSE media. When FPSE extracts were concentrated under nitrogen, 11 out of 18 compounds reached EFs values above 100. PMID:27566344

  14. Extraction Chromatographic Methods in the Sample Preparation Sequence for Thermal Ionization Mass Spectrometric Analysis of Plutonium Isotopes

    International Nuclear Information System (INIS)

    A sample preparation sequence for actinide isotopic analysis by TIMS is described that includes column-based extraction chromatography as the first separation step, followed by anion exchange column separations. The sequence is designed to include a wet ashing step after the extraction chromatography to prevent any leached extractant or oxalic acid eluent reagents from interfering with subsequent separations, source preparation, or TIMS ionization. TEVA-resin and DGA-resin materials, containing extractants that consist only of C, N, O, and H atoms, were investigated for isolation of plutonium. Radiotracer level studies confirmed expected high yields from column-based separation procedures. Femtogram-level studies were carried out with TIMS detection, using multiple isotopic spikes through the separation sequence. Pu recoveries were 87% and 86% for TEVA- and DGA-resins separations respectively. The Pu recoveries from 400 μL anion-exchange column separations were 89% and 93% for trial sequences incorporating TEVA and DGA-resin. Thus, a prior extraction chromatography step in the sequence did not interfere with the subsequent anion exchange separation when a simple wet ash step was carried out in between these column separations. The average measurement efficiency, for Pu, encompassing the chemical separation recoveries and the TIMS ionization efficiency, was 2.73 ± 0.77% (2-sigma) for the DGA-resin trials and 2.67 ± 0.54% for the TEVA-resin trials, compared to 3.41% and 2.37% (average 2.89%) for two spikes in the experimental set. These compare with an average measurement efficiency of 2.78 ± 1.70%, n = 33 from process benchmark analyses using Pu spikes processed through a sequence of oxalate precipitation, wet ash, iron hydroxide precipitation, and anion exchange column separations. We conclude that extraction chromatography can be a viable separation procedure as part of a multistep sequence for TIMS sample preparation.

  15. A sequential extraction procedure for determination of uranium, thorium, radium, lead and polonium radionuclides by alpha spectrometry in environmental samples

    International Nuclear Information System (INIS)

    A sequential extraction technique was developed allowing the extraction and purification of uranium, thorium, radium, lead and polonium radionuclides from the same sample. Environmental materials such as water, soil, biological materials, can be analyzed for those radionuclides without matrix interferences in the quality of radioelement purification and in the radiochemical yield. The use of isotopic tracers (232U, 229Th, 224Ra, 209Po and stable lead carrier) added to the sample at the beginning of the chemical procedure enables an accurate control of the radiochemical yield for each radioelement. The ion extraction procedure, applied after either complete dissolution of the solid sample with mineral acids or dissolution of MnO2 precipitate for aqueous samples, includes the use of commercially available columns from Eichrom and laboratory prepared anionic and cationic columns, in a total of three chromatography columns. All radioelements are purified and electroplated on stainless steel discs except for polonium which is spontaneously plated on a silver disc. The discs are measured using high resolution silicon surface barrier detectors. 210Pb, a beta emitter, can be measured either through the beta emission of 210Bi, or stored for a few months and determined by alpha spectrometry through the in-growth of 210Po. This sequential extraction chromatography technique was tested and validated by analysis of certified reference materials from IAEA (soil, marine sediment, and fish). Reproducibility was tested through repeated analysis of the same homogeneous material (water sample). Performance, when applied to samples with different matrix, was tested analyzing cabbage, potatoes, fish filet, meat, water, urine, soils and sediments with high yield of recovery and complete separation of radioelements. Precision was tested also through participation in analytical inter laboratory world wide comparisons analysing blind samples (round robin tests) organized by the IAEA and

  16. Nanostructured conducting molecularly imprinted polymer for selective extraction of salicylate from urine and serum samples by electrochemically controlled solid-phase micro-extraction

    Energy Technology Data Exchange (ETDEWEB)

    Ameli, Akram [Department of Chemistry, Faculty of Science, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Alizadeh, Naader, E-mail: alizaden@modares.ac.ir [Department of Chemistry, Faculty of Science, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of)

    2011-11-30

    Highlights: Black-Right-Pointing-Pointer Overoxidized polypyrrole templated with salicylate has been utilized as conducting molecular imprinted polymer for EC-SPME. Black-Right-Pointing-Pointer This first study reported on conducting molecular imprinted polymer was used to EC-SPME of salicylate. Black-Right-Pointing-Pointer Proposed method, is particularly effective in sample clean-up and selective monitoring of salicylate in physiological samples. - Abstract: Overoxidized polypyrrole (OPPy) films templated with salicylate (SA) have been utilized as conducting molecular imprinted polymers (CMIPs) for potential-induced selective solid-phase micro-extraction processes. Various important fabrication factors for controlling the performance of the OPPy films have been investigated using fluorescence spectrometry. Several key parameters such as applied potential for uptake, release, pH of uptake and release solution were varied to achieve the optimum micro-extraction procedure. The film template with SA exhibited excellent selectivity over some interference. The calibration graphs were linear in the ranges of 5 Multiplication-Sign 10{sup -8} to 5 Multiplication-Sign 10{sup -4} and 1.2 Multiplication-Sign 10{sup -6} to 5 Multiplication-Sign 10{sup -4} mol mL{sup -1} and the detection limit was 4 Multiplication-Sign 10{sup -8} mol L{sup -1}. The OPPy film as the solid-phase micro-extraction absorbent has been applied for the selective clean-up and quantification of trace amounts of SA from physiological samples. The results of scanning electron microscopy (SEM) have confirmed the nano-structure morphologies of the films.

  17. Potential of on-line coupling of extraction and chromatography in the analysis of complex samples

    Czech Academy of Sciences Publication Activity Database

    Hyötyläinen, T.; Lüthje, K.; Rautiainen-Rämä, M.; Pól, Jaroslav; Ranta-Aho, O.; Riekkola, M. L.

    Kortrijk: I.O.P.M.S. vzw, 2004 - (Sandra, T.; Sandra, P.), J12 [International Symposium on Capillary Chromatography /27./. Riva del Garda (IT), 31.05.2004-04.06.2004] R&D Projects: GA AV ČR KJB4031405 Institutional research plan: CEZ:AV0Z4031919 Keywords : on-line - extraction * chromatography Subject RIV: CB - Analytical Chemistry, Separation

  18. An Improved Method for High Quality Metagenomics DNA Extraction from Human and Environmental Samples

    DEFF Research Database (Denmark)

    Bag, Satyabrata; Saha, Bipasa; Mehta, Ojasvi;

    2016-01-01

    To explore the natural microbial community of any ecosystems by high-resolution molecular approaches including next generation sequencing, it is extremely important to develop a sensitive and reproducible DNA extraction method that facilitate isolation of microbial DNA of sufficient purity and qu...

  19. Air

    International Nuclear Information System (INIS)

    In recent years several regulations and standards for air quality and limits for air pollution were issued or are in preparation by the European Union, which have severe influence on the environmental monitoring and legislation in Austria. This chapter of the environmental control report of Austria gives an overview about the legal situation of air pollution control in the European Union and in specific the legal situation in Austria. It gives a comprehensive inventory of air pollution measurements for the whole area of Austria of total suspended particulates, ozone, volatile organic compounds, nitrogen oxides, sulfur dioxide, carbon monoxide, heavy metals, benzene, dioxin, polycyclic aromatic hydrocarbons and eutrophication. For each of these pollutants the measured emission values throughout Austria are given in tables and geographical charts, the environmental impact is discussed, statistical data and time series of the emission sources are given and legal regulations and measures for an effective environmental pollution control are discussed. In particular the impact of fossil-fuel power plants on the air pollution is analyzed. (a.n.)

  20. Determination of trace amount of lead in industrial and municipal effluent water samples based on dispersive liquid-liquid extraction

    International Nuclear Information System (INIS)

    In this study, a simple, sensitive and accurate method was developed for the determination of lead ion by combining ionic liquid dispersive liquid-liquid extraction (Il-DLL E) with flame atomic absorption spectrometry. Tetraethyl thiuram disulfide (Tetd), acetone and 1-octyl-3m ethylimidazolium hexafluorophosphate [(C8MIM) (PF6)] were used as the chelating agent, dispersive and extraction solvent, respectively. Under the optimal conditions, the calibration graph was linear in the range of 5-190 μg L-1 of lead and the detection limit was 0.8 μg L-1 with a sample volume of 200 ml. The proposed method was validated by the analysis of one certified reference material and applied successfully to the determination of lead in real water samples. (Author)

  1. Optimization of an analytical method using extraction chromatography for the determination of plutonium, americium and curium in soil samples

    International Nuclear Information System (INIS)

    An analytical method for determination of the actinides 238Pu, 239+240Pu, 241Am and 244Cm in soil samples was developed and optimized to allow specific immission measurements of radionuclides in the vicinity of the recently constructed radwaste facility at Wuerenlingen/Switzerland. Following a rapid extraction from the soil sample, as well as a preconcentration step via calcium oxalate precipitation, the actinides are separated using extraction chromatography. Separation of the actinides is carrie out applying the specific resins U/TEVA, TRU and TEVA (Eichrom Technologies IL/USA) and the anion exchange resin BioRAD 1-X2. Measurements are then performed using an α-spectrometer equipped with ion-implanted silicon charged particle detectors. For counting times of less than three days a detection limit of less than 0.05 Bq/kg is obtained for the actinides 238Pu, 239+240Pu, 241Am and 244Cm. (author)

  2. Determination of trace amount of lead in industrial and municipal effluent water samples based on dispersive liquid-liquid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Shirkhanloo, H. [Iranian Petroleum Industry Health Research Institute, Occupational and Environmental Health Research Center, Tehran (Iran, Islamic Republic of); Sedighi, K.; Mousavi, H. Z., E-mail: hzmousavi@semnan.ac.ir [Semnan University, College of Science, Department of Chemistry, Semnan (Iran, Islamic Republic of)

    2014-10-01

    In this study, a simple, sensitive and accurate method was developed for the determination of lead ion by combining ionic liquid dispersive liquid-liquid extraction (Il-DLL E) with flame atomic absorption spectrometry. Tetraethyl thiuram disulfide (Tetd), acetone and 1-octyl-3m ethylimidazolium hexafluorophosphate [(C{sub 8}MIM) (PF{sub 6})] were used as the chelating agent, dispersive and extraction solvent, respectively. Under the optimal conditions, the calibration graph was linear in the range of 5-190 μg L{sup -1} of lead and the detection limit was 0.8 μg L{sup -1} with a sample volume of 200 ml. The proposed method was validated by the analysis of one certified reference material and applied successfully to the determination of lead in real water samples. (Author)

  3. The sampling of hydrogen sulfide in air with impregnated filter paper

    NARCIS (Netherlands)

    Huygen, C.

    1964-01-01

    A method is proposed for the quantitative collection of hydrogen sulfide in air on impregnated filter paper. An aqueous solution of potassium hydroxide, potassium zincate and glycerol is used as impregnating fluid. The stability of the collected sulfide and the efficiency of collection at different

  4. Validation of Internal Controls for Extraction and Amplification of Nucleic Acids from Enteric Viruses in Water Samples ▿ †

    OpenAIRE

    Hata, Akihiko; Katayama, Hiroyuki; Kitajima, Masaaki; Visvanathan, Chettiyappan; Nol, Chea; Furumai, Hiroaki

    2011-01-01

    Inhibitors that reduce viral nucleic acid extraction efficiency and interfere with cDNA synthesis and/or polymerase activity affect the molecular detection of viruses in aquatic environments. To overcome these significant problems, we developed a methodology for assessing nucleic acid yields and DNA amplification efficiencies for environmental water samples. This involved adding particles of adenovirus type 5 and murine norovirus and newly developed primer-sharing controls, which are amplifie...

  5. Supercritical Fluid Extraction and Ultra Performance Liquid Chromatography of Respiratory Quinones for Microbial Community Analysis in Environmental and Biological Samples

    OpenAIRE

    Koichi Fujie; Hiroyuki Daimon; Yoichi Atsuta; Muhammad Hanif

    2012-01-01

    Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE) and ultra performance liquid chromatography (UPLC) method for the analysis of bacterial respiratory quinones (RQ) in environmental and biological samples. RQ profile analysi...

  6. A solid-phase extraction method using Transcarpathian clinoptilolite for preconcentration of trace amounts of terbium in water samples

    OpenAIRE

    Vasylechko, Volodymyr O.; Gryshchouk, Galyna V.; Zakordonskiy, Victor P.; Vyviurska, Olga; Pashuk, Andriy V.

    2015-01-01

    Background 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 aqu...

  7. Regional CO2 fluxes inferred from mixing ratio measurements: estimates from flask air samples in central Kansas, USA

    OpenAIRE

    Lai, Chun-Ta; Schauer, Andrew J.; Owensby, Clenton; Ham, Hay M.; Helliker, Brent; Tans, Pieter P.; Ehleringer, James R

    2011-01-01

    We estimated regional fluxes of carbon dioxide (CO2) using mixing ratios measured in a tallgrass prairie in central Kansas, USA over 3 yr (2002–2004). Glass flasks were used to collect whole air samples in the midafternoon for determining CO2 mixing ratios and their carbon isotopic composition. Regional CO2 fluxes were calculated assuming atmospheric boundary layer (ABL) approaches an equilibrium state on a monthly basis. CO2 mixing ratios derived from the marine boundary layer data were used...

  8. Field Air Sampling with SPME for Ranking and Prioritization of Downwind Livestock Odors with MDGC-MS-Olfactometry

    Science.gov (United States)

    Koziel, Jacek A.; Cai, Lingshuang; Wright, Donald W.; Hoff, Steven J.

    2009-05-01

    Air sampling and characterization of odorous livestock gases is one of the most challenging analytical tasks. This is due to low concentrations, physicochemical properties, and problems with sample recoveries for typical odorants. Livestock operations emit a very complex mixture of volatile organic compounds and other gases. Many of these gases are odorous. Relatively little is known about the link between specific VOCs/gases and specifically, about the impact of specific odorants downwind from sources. In this research, solid phase microextraction (SPME) was used for field air sampling of odors downwind from swine and beef cattle operations. Sampling time ranged from 20 min to 1 hr. Samples were analyzed using a commercial GC-MS-Olfactometry system. Odor profiling efforts were directed at odorant prioritization with respect to distance from the source. The results indicated the odor downwind was increasingly defined by a smaller number of high priority odorants. These `character defining' odorants appeared to be dominated by compounds of relatively low volatility, high molecular weight and high polarity. In particular, p-cresol alone appeared to carry much of the overall odor impact for swine and beef cattle operations. Of particular interest was the character-defining odor impact of p-cresol as far as 16 km downwind of the nearest beef cattle feedlot. The findings are very relevant to scientists and engineers working on improved air sampling and analysis protocols and on improved technologies for odor abatement. More research evaluating the use of p-cresol and a few other key odorants as a surrogate for the overall odor dispersion modeling is warranted.

  9. System and method for liquid extraction electrospray-assisted sample transfer to solution for chemical analysis

    Energy Technology Data Exchange (ETDEWEB)

    Kertesz, Vilmos; Van Berkel, Gary J.

    2016-07-12

    A system for sampling a surface includes a surface sampling probe comprising a solvent liquid supply conduit and a distal end, and a sample collector for suspending a sample collection liquid adjacent to the distal end of the probe. A first electrode provides a first voltage to solvent liquid at the distal end of the probe. The first voltage produces a field sufficient to generate electrospray plume at the distal end of the probe. A second electrode provides a second voltage and is positioned to produce a plume-directing field sufficient to direct the electrospray droplets and ions to the suspended sample collection liquid. The second voltage is less than the first voltage in absolute value. A voltage supply system supplies the voltages to the first electrode and the second electrode. The first electrode can apply the first voltage directly to the solvent liquid. A method for sampling for a surface is also disclosed.

  10. Influence of EDTA and magnesium on DNA extraction from blood samples and specificity of polymerase chain reaction

    OpenAIRE

    H. Khosravinia; Ramesha, KP

    2007-01-01

    This study consisting of two trails conducted to examine the impact of initial EDTA level added to blood samples on quantity and quality of genomic DNA isolated from avian fresh blood and the influence of initial EDTA level with various levels of $MgCl_2$ added to polymerase chain reaction (PCR) final volume on amplification pattern. EDTA level added to collected blood samples had no significant impact on quantity as well as quality of extracted genomic DNA. However, higher levels of EDTA inc...

  11. A magnetic sorbent for the efficient and rapid extraction of organic micropollutants from large-volume environmental water samples.

    Science.gov (United States)

    Zhang, Mancheng; Zhou, Qing; Li, Aimin; Shuang, Chendong; Wang, Wei; Wang, Mengqiao

    2013-11-01

    A magnetic solid-phase extraction (MSPE) method based on a novel magnetic sorbent was proposed for the extraction of target compounds from large-volume water samples. First, magnetic hypercrosslinked microspheres (NAND-1) were prepared via membrane emulsification-suspension polymerization and post crosslinking reaction. To ensure that the Fe3O4 nanoparticles could completely pass through the membrane without blocking the pores, oleic acid was used to modify the Fe3O4 nanoparticles, which enhanced lipophilicity and monodispersity of the magnetite nanoparticles. The obtained NAND-1 microspheres exhibited super paramagnetic characteristics and excellent magnetic responsiveness with a saturation magnetization of 2.53 emu/g. In addition, a uniform particle size (~8 μm) and a large average surface area (1303.59 m(2)/g) were also observed, which were both beneficial for the extraction of the target compounds. Thus, NAND-1 has the potential to simultaneously exhibit good extraction efficiencies toward different types of organic micropollutants (OMPs), including triazines, carbamazepine and diethyl phthalate. The conditions of the MSPE based on NAND-1 were optimized by single factor and orthogonal design experiments. This MSPE method needed only a small amount of sorbent (50mg/L) for the extraction of OMPs from a large-volume aquatic sample (5L) and reached equilibrium in a short amount of time (30 min). Moreover, the solution volume, the pH, and the salinity had insignificant influences on the extraction of the eight target OMPs. Under the optimum conditions, the recoveries of the eight OMPs calculated by analyzing the spiked samples were from 91.7% to 99.4%. The NAND-1 could be recycled ten times and still achieve recoveries of the eight OMPs higher than 86%. The limits of detection of the eight OMPs ranged from 1.76 to 27.56 ng/L, and the limits of quantification were from 5.71 to 92.05 ng/L. These results indicated that the proposed method, based on the use of NAND-1

  12. Analysis of Mars Analogue Soil Samples Using Solid-Phase Microextraction, Organic Solvent Extraction and Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Orzechowska, G. E.; Kidd, R. D.; Foing, B. H.; Kanik, I.; Stoker, C.; Ehrenfreund, P.

    2011-01-01

    Polycyclic aromatic hydrocarbons (PAHs) are robust and abundant molecules in extraterrestrial environments. They are found ubiquitously in the interstellar medium and have been identified in extracts of meteorites collected on Earth. PAHs are important target molecules for planetary exploration missions that investigate the organic inventory of planets, moons and small bodies. This study is part of an interdisciplinary preparation phase to search for organic molecules and life on Mars. We have investigated PAH compounds in desert soils to determine their composition, distribution and stability. Soil samples (Mars analogue soils) were collected at desert areas of Utah in the vicinity of the Mars Desert Research Station (MDRS), in the Arequipa region in Peru and from the Jutland region of Denmark. The aim of this study was to optimize the solid-phase microextraction (SPME) method for fast screening and determination of PAHs in soil samples. This method minimizes sample handling and preserves the chemical integrity of the sample. Complementary liquid extraction was used to obtain information on five- and six-ring PAH compounds. The measured concentrations of PAHs are, in general, very low, ranging from 1 to 60 ng g(sup -1). The texture of soils is mostly sandy loam with few samples being 100% silt. Collected soils are moderately basic with pH values of 8-9 except for the Salten Skov soil, which is slightly acidic. Although the diverse and variable microbial populations of the samples at the sample sites might have affected the levels and variety of PAHs detected, SPME appears to be a rapid, viable field sampling technique with implications for use on planetary missions.

  13. Complete extraction of arsenic species from biological samples - a worthwhile goal? (W2)

    International Nuclear Information System (INIS)

    Full text: A major reason cited for carrying out arsenic speciation work is that the various species have different toxicities. In accordance with this is the fact, that they also have very different chemical and physical properties including solubility. The polarity of naturally-occurring arsenic species range from highly polar arsenate to arseno-lipids of low polarity. It thus seems an impossible task to find extraction conditions suitable for all such arsenic species. And yet researchers are prepared to try. This lecture reports a brief history of the reported extraction procedures for speciation analysis, and the methods commonly used today. The rationale behind the methods and their applicability to quantitative analysis are also discussed. (author)

  14. Single sample extraction protocol for the quantification of NAD and NADH redox states in Saccharomyces cerevisiae

    OpenAIRE

    Sporty, Jennifer L.; Kabir, Md. Mohiuddin; Turteltaub, Kenneth W.; Ognibene, Ted; Lin, Su-Ju; Bench, Graham

    2008-01-01

    A robust redox extraction protocol for quantitative and reproducible metabolite isolation and recovery has been developed for simultaneous measurement of nicotin-amide adenine dinucleotide (NAD) and its reduced form, NADH, from Saccharomyces cerevisiae. Following culture in liquid media, yeast cells were harvested by centrifugation and then lysed under nonoxidizing conditions by bead blasting in ice-cold, nitrogen-saturated 50 mM ammonium acetate. To enable protein denaturation, ice cold nitr...

  15. A Comparative Analysis of Extraction Methods for the Recovery of Anguina sp. from Grass Seed Samples

    OpenAIRE

    Griesbach, J.A.; Chitambar, J. J.; Hamerlynck, M. J.; Duarte, E. O.

    1999-01-01

    Four procedures were compared in their efficacy to extract juveniles of Anguina agrostis from commercial grass seed. The procedures included those currently used by the state regulatory laboratories of Oregon and California, as well as new tests developed to determine juvenile viability for the phytosanitary certification of fumigated grass seed. Eleven seed lots of Agrostis tenuis (bentgrass) and Dactylis glomerata (orchardgrass) naturally infested with varying levels of juveniles of Anguina...

  16. Solid-phase extraction approach in comprehensive analysis of wort and beer samples

    Czech Academy of Sciences Publication Activity Database

    Čmelík, Richard; Žídková, Jitka; Bobálová, Janette

    Praha : Institute of Chemical Technology, 2011 - (Pulkrabová, J.; Tomaniová, M.). s. 237 ISBN 978-80-7080-795-8. [International Symposium on Recent Advances in Food Analysis /5./. 01.11.2011-04.11.2011, Praha] R&D Projects: GA MŠk 1M06030; GA MŠk 1M0570 Institutional research plan: CEZ:AV0Z40310501 Keywords : solid phase extraction * carbohydrates * beer Subject RIV: CB - Analytical Chemistry, Separation

  17. Determination of cadmium and lead in urine samples after dispersive solid–liquid extraction on multiwalled carbon nanotubes by slurry sampling electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Álvarez Méndez, J.; Barciela García, J.; García Martín, S.; Peña Crecente, R.M.; Herrero Latorre, C., E-mail: carlos.herrero@usc.es

    2015-04-01

    A new method for the determination of Cd and Pb in urine samples has been developed. The method involves dispersive solid-phase extraction (DSPE), slurry sampling (SS), and subsequent electrothermal atomic absorption spectrometry (ETAAS). Oxidized multiwalled carbon nanotubes (MWCNTs) were used as the sorbent material. The isolated MWCNT/analyte aggregates were treated with nitric acid to form a slurry and both metals were determined directly by injecting the slurry into the ETAAS-atomizer. The parameters that influence the adsorption of the metals on MWCNTs in the DSPE process, the formation and extraction of the slurry, and the ETAAS conditions were studied by different factorial design strategies. The detection and quantification limits obtained for Cd under optimized conditions were 9.7 and 32.3 ng L{sup −1}, respectively, and for Pb these limits were 0.13 and 0.43 μg L{sup −1}. The preconcentration factors achieved were 3.9 and 5.4. The RSD values (n = 10) were less than 4.1% and 5.9% for Cd and Pb, respectively. The accuracy of the method was assessed in recovery studies, with values in the range 96–102% obtained for Cd and 97–101% for Pb. In addition, the analysis of certified reference materials gave consistent results. The DSPE–SS–ETAAS method is a novel and useful strategy for the determination of Pb and Cd at low levels in human urine samples. The method is sensitive, fast, and free of matrix interferences, and it avoids the tedious and time-consuming on-column adsorption and elution steps associated with commonly used SPE procedures. The proposed method was used to determine Cd and Pb in urine samples of unexposed healthy people and satisfactory results were obtained. - Highlights: • Cd and Pb determination based on the combination of DSP, SS and ETAAS • Urine matrix was eliminated using DSPE based on multiwalled carbon nanotubes. • Slurry sampling technique permitted the direct injection of sample into the ETAAS atomizer.

  18. Determination of cadmium and lead in urine samples after dispersive solid–liquid extraction on multiwalled carbon nanotubes by slurry sampling electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    A new method for the determination of Cd and Pb in urine samples has been developed. The method involves dispersive solid-phase extraction (DSPE), slurry sampling (SS), and subsequent electrothermal atomic absorption spectrometry (ETAAS). Oxidized multiwalled carbon nanotubes (MWCNTs) were used as the sorbent material. The isolated MWCNT/analyte aggregates were treated with nitric acid to form a slurry and both metals were determined directly by injecting the slurry into the ETAAS-atomizer. The parameters that influence the adsorption of the metals on MWCNTs in the DSPE process, the formation and extraction of the slurry, and the ETAAS conditions were studied by different factorial design strategies. The detection and quantification limits obtained for Cd under optimized conditions were 9.7 and 32.3 ng L−1, respectively, and for Pb these limits were 0.13 and 0.43 μg L−1. The preconcentration factors achieved were 3.9 and 5.4. The RSD values (n = 10) were less than 4.1% and 5.9% for Cd and Pb, respectively. The accuracy of the method was assessed in recovery studies, with values in the range 96–102% obtained for Cd and 97–101% for Pb. In addition, the analysis of certified reference materials gave consistent results. The DSPE–SS–ETAAS method is a novel and useful strategy for the determination of Pb and Cd at low levels in human urine samples. The method is sensitive, fast, and free of matrix interferences, and it avoids the tedious and time-consuming on-column adsorption and elution steps associated with commonly used SPE procedures. The proposed method was used to determine Cd and Pb in urine samples of unexposed healthy people and satisfactory results were obtained. - Highlights: • Cd and Pb determination based on the combination of DSP, SS and ETAAS • Urine matrix was eliminated using DSPE based on multiwalled carbon nanotubes. • Slurry sampling technique permitted the direct injection of sample into the ETAAS atomizer. • Appropriate

  19. Mezcla génica en una muestra poblacional de la ciudad de Buenos Aires Gene mixture in a population sample from Buenos Aires City

    Directory of Open Access Journals (Sweden)

    Sergio A. Avena

    2006-04-01

    Full Text Available Este estudio tiene como objetivo estimar la mezcla génica en la población de la Ciudad de Buenos Aires, a partir de muestras de dadores de sangre provenientes de un centro público de salud (Hospital de Clínicas. Los estudios se realizaron sobre 218 personas no emparentadas que donaron su sangre durante el año 2002. Se analizaron 8 sistemas genéticos eritrocitarios y los alotipos GM/KM. Se realizó una encuesta con la finalidad de obtener información sobre lugar de nacimiento, residencia actual y datos genealógicos de los dadores. Las frecuencias génicas se determinaron empleando métodos de máxima verosimilitud. Para calcular la mezcla génica se aplicó el programa ADMIX (trihíbrido. Se registró un 15.8% de aporte indígena (AI y 4.3% de africano (AA. Estos datos se compararon con un estudio previo realizado en un centro privado (Hospital Italiano de Buenos Aires, no observándose diferencias significativas salvo en el sistema Km. Los resultados obtenidos se corresponden con la información histórica y demográfica de la ciudad de Buenos Aires.The aim of this study is to estimate the gene admixture in the population of Buenos Aires City from samples of blood donors, which come from a public health centre (Hospital de Clínicas. These studies were performed on 218 unrelated people, who donated blood during the year 2002. Eight erythrocyte genetic systems and GM/KM allotypes were analysed. A survey to obtain information about place of birth, present residence and genealogical data of the donors was performed. The gene frequencies were determined using a method of maximum likelihood. The genetic admixture was calculated through the ADMIX program (trihibride. The Amerindian and African contributions were 15.8% and 4.3% respectively. These data were compared with those obtained in a previous study performed in a private centre (Hospital Italiano de Buenos Aires and significant differences were observed, except in the KM system. The

  20. Development of natural sorbent based micro-solid-phase extraction for determination of phthalate esters in milk samples.

    Science.gov (United States)

    Sajid, Muhammad; Basheer, Chanbasha; Alsharaa, Abdulnaser; Narasimhan, Kothandaraman; Buhmeida, Abdelbaset; Al Qahtani, Mohammed; Al-Ahwal, Mahmoud Shaheen

    2016-06-14

    In the present study, a natural sorbent based micro-solid phase extraction (μ-SPE) was developed for determination of phthalate esters in milk samples. For the first time, an efficient and cost effective natural material (seed powder of Moringa oleifera) was employed as sorbent in μ-SPE. The sorbent was found to be naturally enriched with variety of functional groups and having a network of interconnected fibers. This method of extraction integrates different steps such as removal of proteins and fatty stuff, extraction and pre-concentration of target analytes into a single step. Thirteen phthalate esters were selected as target compounds for the development and evaluation of method. Some key parameters affecting the extraction efficiency were optimized, including selection of membrane, selection and amount of sorbent, extraction time, desorption solvent, volume of desorption solvent, desorption time and effect of salt addition. Under the optimum conditions, very good linearity was achieved for all the analytes with coefficient of determinations (R(2)) ranging between 0.9768 and 0.9977. The limits of detection ranged from 0.01 to 1.2 μg L(-1). Proposed method showed satisfactory reproducibility with relative standard deviations ranging from 3.6% to 10.2% (n = 7). Finally, the developed method was applied to tetra pack and bottled milk samples for the determination of phthalate esters. The performance of natural sorbent based μ-SPE was better or comparable to the methods reported in the literature. PMID:27181642