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Sample records for air sample extract

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

    International Nuclear Information System (INIS)

    Hebel, S.; Hands, J.; Goering, F.; Kirchner, G.; Purtschert, R.

    2015-01-01

    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)

  2. Quantitative analysis of semivolatile organic compounds in selected fractions of air sample extracts by GC/MI-IR spectrometry

    International Nuclear Information System (INIS)

    Childers, J.W.; Wilson, N.K.; Barbour, R.K.

    1990-01-01

    The authors are currently investigating the capabilities of gas chromatography/matrix isolation infrared (GC/MI-IR) spectrometry for the determination of semivolatile organic compounds (SVOCs) in environmental air sample extracts. Their efforts are focused on the determination of SVOCs such as alkylbenzene positional isomers, which are difficult to separate chromatographically and to distinguish by conventional electron-impact ionization GC/mass spectrometry. They have performed a series of systematic experiments to identify sources of error in quantitative GC/MI-IR analyses. These experiments were designed to distinguish between errors due to instrument design or performance and errors that arise from some characteristic inherent to the GC/MI-IR technique, such as matrix effects. They have investigated repeatability as a function of several aspects of GC/MI IR spectrometry, including sample injection, spectral acquisition, cryogenic disk movement, and matrix deposition. The precision, linearity, dynamic range, and detection limits of a commercial GC/MI-IR system for target SVOCs were determined and compared to those obtained with the system's flame ionization detector. The use of deuterated internal standards in the quantitative GC/MI-IR analysis of selected fractions of ambient air sample extracts will be demonstrated. They will also discuss the current limitations of the technique in quantitative analyses and suggest improvements for future consideration

  3. Operational air sampling report

    International Nuclear Information System (INIS)

    Lyons, C.L.

    1994-03-01

    Nevada Test Site vertical shaft and tunnel events generate beta/gamma fission products. The REECo air sampling program is designed to measure these radionuclides at various facilities supporting these events. The current testing moratorium and closure of the Decontamination Facility has decreased the scope of the program significantly. Of the 118 air samples collected in the only active tunnel complex, only one showed any airborne fission products. Tritiated water vapor concentrations were very similar to previously reported levels. The 206 air samples collected at the Area-6 decontamination bays and laundry were again well below any Derived Air Concentration calculation standard. Laboratory analyses of these samples were negative for any airborne fission products

  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. Determination of fragrance allergens in indoor air by active sampling followed by ultrasound-assisted solvent extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lamas, J Pablo; Sanchez-Prado, Lucia; Garcia-Jares, Carmen; Llompart, Maria

    2010-03-19

    Fragrances are ubiquitous pollutants in the environment, present in the most of household products, air fresheners, insecticides and cosmetics. Commercial perfumes may contain hundreds of individual fragrance chemicals. In addition to the widespread use and exposure to fragranced products, many of the raw fragrance materials have limited available health and safety data. Because of their nature as artificial fragrances, inhalation should be considered as an important exposure pathway, especially in indoor environments. In this work, a very simple, fast, and sensitive methodology for the analysis of 24 fragrance allergens in indoor air is presented. Considered compounds include those regulated by the EU Directive, excluding limonene; methyl eugenol was also included due to its toxicity. The proposed methodology is based on the use of a very low amount of adsorbent to retain the target compounds, and the rapid ultrasound-assisted solvent extraction (UAE) using a very low volume of solvent which avoids further extract concentration. Quantification was performed by gas chromatography coupled to mass spectrometry (GC-MS). The influence of main factors involved in the UAE step (type of adsorbent and solvent, solvent volume and extraction time) was studied using an experimental design approach to account for possible factor interactions. Using the optimized procedure, 0.2 m(-3) air are sampled, analytes are retained on 25 mg Florisil, from which they are extracted by UAE (5 min) with 2 mL ethyl acetate. Linearity was demonstrated in a wide concentration range. Efficiency of the total sampling-extraction process was studied at several concentration levels (1, 5 and 125 microg m(-3)), obtaining quantitative recoveries, and good precision (RSD<10%). Method detection limits were < or =0.6 microg m(-3). Finally, the proposed method was applied to real samples collected in indoor environments in which several of the target compounds were determined. Copyright 2010 Elsevier B

  7. Integrated sampling and analysis unit for the determination of sexual pheromones in environmental air using fabric phase sorptive extraction and headspace-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Alcudia-León, M Carmen; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel; Kabir, Abuzar; Furton, Kenneth G

    2017-03-10

    This article presents a novel unit that integrates for the first time air sampling and preconcentration based on the use of fabric phase sorptive extraction principles. The determination of Tuta absoluta sexual pheromone traces in environmental air has been selected as analytical problem. For this aim, a novel laboratory-built unit made up of commercial brass elements as holder of the sol-gel coated fabric extracting phase has been designed and optimized. The performance of the integrated unit was evaluated analyzing environmental air sampled in tomato crops. The unit can work under sampling and analysis mode which eliminates any need for sorptive phase manipulation prior to instrumental analysis. In the sampling mode, the unit can be connected to a sampling pump to pass the air through the sorptive phase at a controlled flow-rate. In the analysis mode, it is placed in the gas chromatograph autosampler without any instrumental modification. It also diminishes the risk of cross contamination between sampling and analysis. The performance of the new unit has been evaluated using the main components of the sexual pheromone of Tuta absoluta [(3E,8Z,11Z)-tetradecatrien-1-yl acetate and (3E,8Z)-tetradecadien-1-yl acetate] as model analytes. The limits of detection for both compounds resulted to be 1.6μg and 0.8μg, respectively, while the precision (expressed as relative standard deviation) was better than 3.7%. Finally, the unit has been deployed in the field to analyze a number of real life samples, some of them were found positive. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Air sampling in the workplace

    International Nuclear Information System (INIS)

    Hickey, E.E.; Stoetzel, G.A.; Strom, D.J.; Cicotte, G.R.; Wiblin, C.M.; McGuire, S.A.

    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

  9. Air-assisted liquid-liquid microextraction using floating organic droplet solidification for simultaneous extraction and spectrophotometric determination of some drugs in biological samples through chemometrics methods

    Science.gov (United States)

    Farahmand, Farnaz; Ghasemzadeh, Bahar; Naseri, Abdolhossein

    2018-01-01

    An air assisted liquid-liquid microextraction by applying the solidification of a floating organic droplet method (AALLME-SFOD) coupled with a multivariate calibration method, namely partial least squares (PLS), was introduced for the fast and easy determination of Atenolol (ATE), Propanolol (PRO) and Carvedilol (CAR) in biological samples via a spectrophotometric approach. The analytes would be extracted from neutral aqueous solution into 1-dodecanol as an organic solvent, using AALLME. In this approach a low-density solvent with a melting point close to room temperature was applied as the extraction solvent. The emulsion was immediately formed by repeatedly pulling in and pushing out the aqueous sample solution and extraction solvent mixture via a 10-mL glass syringe for ten times. After centrifugation, the extractant droplet could be simply collected from the aqueous samples by solidifying the emulsion at a lower than the melting point temperature. In the next step, analytes were back extracted simultaneously into the acidic aqueous solution. Derringer and Suich multi-response optimization were utilized for simultaneous optimizing the parameters of three analytes. This method incorporates the benefits of AALLME and dispersive liquid-liquid microextraction considering the solidification of floating organic droplets (DLLME-SFOD). Calibration graphs under optimized conditions were linear in the range of 0.30-6.00, 0.32-2.00 and 0.30-1.40 μg mL- 1 for ATE, CAR and PRO, respectively. Other analytical parameters were obtained as follows: enrichment factors (EFs) were found to be 11.24, 16.55 and 14.90, and limits of detection (LODs) were determined to be 0.09, 0.10 and 0.08 μg mL- 1 for ATE, CAR and PRO, respectively. The proposed method will require neither a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly.

  10. Dissolvable layered double hydroxide as an efficient nanosorbent for centrifugeless air-agitated dispersive solid-phase extraction of potentially toxic metal ions from bio-fluid samples

    Energy Technology Data Exchange (ETDEWEB)

    Rajabi, Maryam, E-mail: mrajabi@semnan.ac.ir; Arghavani-Beydokhti, Somayeh; Barfi, Behruz; Asghari, Alireza

    2017-03-08

    In the present work, a novel nanosorbent namely layered double hydroxides with 4-amino-5-hydroxyl-2,7-naphthalendisulfonic acid monosodium salt interlayer anion (Mg-Al-AHNDA-LDH) was synthesized and applied as a dissolvable nanosorbent in a centrifugeless ultrasound-enhanced air-agitated dispersive solid-phase extraction (USE-AA-D-SPE) method. This method was used for the separation and preconcentration of some metal ions including Cd{sup 2+}, Cr{sup 6+}, Pb{sup 2+}, Co{sup 2+}, and Ni{sup 2+} prior to their determination using the micro-sampling flame atomic absorption spectrometry (MS-FAAS) technique. The most interesting aspect of this nanosorbent is its immediate dissolvability at pH values lower than 4. This capability drastically eliminates the elution step, leading to a great improvement in the extraction efficiency and a decrease in the extraction time. Also in this method, the use of a syringe nanofilter eliminates the need for the centrifugation step, which is time-consuming and essentially causes the analysis to be off-line. Several effective parameters governing the extraction efficiency including the sample solution pH, amount of nanosorbent, eluent condition, number of air-agitation cycles, and sonication time were investigated and optimized. Under the optimized conditions, the good linear dynamic ranges of 2–70, 6–360, 7–725, 7–370, and 8–450 ng mL{sup −1} for the Cd{sup 2+}, Cr{sup 6+}, Pb{sup 2+}, Co{sup 2+}and Ni{sup 2+} ions, respectively, with the correlation of determinations (R{sup 2}s) higher than 0.997 were obtained. The limits of detection (LODs) were found to be 0.6, 1.7, 2.0, 2.1, and 2.4 for the Cd{sup 2+}, Cr{sup 6+}, Pb{sup 2+}, Co{sup 2+}, and Ni{sup 2+} ions, respectively. The intra-day and inter-day precisions (percent relative standard deviations (%RSDs) (n = 5)) were below 7.8%. The proposed method was also successfully applied for the extraction and determination of the target ions in different biological fluid

  11. Dissolvable layered double hydroxide as an efficient nanosorbent for centrifugeless air-agitated dispersive solid-phase extraction of potentially toxic metal ions from bio-fluid samples

    International Nuclear Information System (INIS)

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

    2017-01-01

    In the present work, a novel nanosorbent namely layered double hydroxides with 4-amino-5-hydroxyl-2,7-naphthalendisulfonic acid monosodium salt interlayer anion (Mg-Al-AHNDA-LDH) was synthesized and applied as a dissolvable nanosorbent in a centrifugeless ultrasound-enhanced air-agitated dispersive solid-phase extraction (USE-AA-D-SPE) method. This method was used for the separation and preconcentration of some metal ions including Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ , and Ni 2+ prior to their determination using the micro-sampling flame atomic absorption spectrometry (MS-FAAS) technique. The most interesting aspect of this nanosorbent is its immediate dissolvability at pH values lower than 4. This capability drastically eliminates the elution step, leading to a great improvement in the extraction efficiency and a decrease in the extraction time. Also in this method, the use of a syringe nanofilter eliminates the need for the centrifugation step, which is time-consuming and essentially causes the analysis to be off-line. Several effective parameters governing the extraction efficiency including the sample solution pH, amount of nanosorbent, eluent condition, number of air-agitation cycles, and sonication time were investigated and optimized. Under the optimized conditions, the good linear dynamic ranges of 2–70, 6–360, 7–725, 7–370, and 8–450 ng mL −1 for the Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ and Ni 2+ ions, respectively, with the correlation of determinations (R 2 s) higher than 0.997 were obtained. The limits of detection (LODs) were found to be 0.6, 1.7, 2.0, 2.1, and 2.4 for the Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ , and Ni 2+ ions, respectively. The intra-day and inter-day precisions (percent relative standard deviations (%RSDs) (n = 5)) were below 7.8%. The proposed method was also successfully applied for the extraction and determination of the target ions in different biological fluid and tap water samples. - Highlights: • A novel centrifugeless dispersive

  12. Dissolvable layered double hydroxide as an efficient nanosorbent for centrifugeless air-agitated dispersive solid-phase extraction of potentially toxic metal ions from bio-fluid samples.

    Science.gov (United States)

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

    2017-03-08

    In the present work, a novel nanosorbent namely layered double hydroxides with 4-amino-5-hydroxyl-2,7-naphthalendisulfonic acid monosodium salt interlayer anion (Mg-Al-AHNDA-LDH) was synthesized and applied as a dissolvable nanosorbent in a centrifugeless ultrasound-enhanced air-agitated dispersive solid-phase extraction (USE-AA-D-SPE) method. This method was used for the separation and preconcentration of some metal ions including Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ , and Ni 2+ prior to their determination using the micro-sampling flame atomic absorption spectrometry (MS-FAAS) technique. The most interesting aspect of this nanosorbent is its immediate dissolvability at pH values lower than 4. This capability drastically eliminates the elution step, leading to a great improvement in the extraction efficiency and a decrease in the extraction time. Also in this method, the use of a syringe nanofilter eliminates the need for the centrifugation step, which is time-consuming and essentially causes the analysis to be off-line. Several effective parameters governing the extraction efficiency including the sample solution pH, amount of nanosorbent, eluent condition, number of air-agitation cycles, and sonication time were investigated and optimized. Under the optimized conditions, the good linear dynamic ranges of 2-70, 6-360, 7-725, 7-370, and 8-450 ng mL -1 for the Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ and Ni 2+ ions, respectively, with the correlation of determinations (R 2 s) higher than 0.997 were obtained. The limits of detection (LODs) were found to be 0.6, 1.7, 2.0, 2.1, and 2.4 for the Cd 2+ , Cr 6+ , Pb 2+ , Co 2+ , and Ni 2+ ions, respectively. The intra-day and inter-day precisions (percent relative standard deviations (%RSDs) (n = 5)) were below 7.8%. The proposed method was also successfully applied for the extraction and determination of the target ions in different biological fluid and tap water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. 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.

  14. Directional dependency of air sampling

    International Nuclear Information System (INIS)

    1994-01-01

    A field study was performed by Idaho State University-Environmental Monitoring Laboratory (EML) to examine the directional dependency of low-volume air samplers. A typical continuous low volume air sampler contains a sample head that is mounted on the sampler housing either horizontally through one of four walls or vertically on an exterior wall 'looking down or up.' In 1992, a field study was undertaken to estimate sampling error and to detect the directional effect of sampler head orientation. Approximately 1/2 mile downwind from a phosphate plant (continuous source of alpha activity), four samplers were positioned in identical orientation alongside one sampler configured with the sample head 'looking down'. At least five consecutive weekly samples were collected. The alpha activity, beta activity, and the Be-7 activity collected on the particulate filter were analyzed to determine sampling error. Four sample heads were than oriented to the four different horizontal directions. Samples were collected for at least five weeks. Analysis of the alpha data can show the effect of sampler orientation to a know near source term. Analysis of the beta and Be-7 activity shows the effect of sampler orientation to a ubiquitous source term

  15. Guidance for air sampling at nuclear facilities

    International Nuclear Information System (INIS)

    Breslin, A.J.

    1976-11-01

    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

  16. 40 CFR 61.34 - Air sampling.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 8 2010-07-01 2010-07-01 false Air sampling. 61.34 Section 61.34... sampling. (a) Stationary sources subject to § 61.32(b) shall locate air sampling sites in accordance with a... concentrations calculated within 30 days after filters are collected. Records of concentrations at all sampling...

  17. Organic solvent-free air-assisted liquid-liquid microextraction for optimized extraction of illegal azo-based dyes and their main metabolite from spices, cosmetics and human bio-fluid samples in one step.

    Science.gov (United States)

    Barfi, Behruz; Asghari, Alireza; Rajabi, Maryam; Sabzalian, Sedigheh

    2015-08-15

    Air-assisted liquid-liquid microextraction (AALLME) has unique capabilities to develop as an organic solvent-free and one-step microextraction method, applying ionic-liquids as extraction solvent and avoiding centrifugation step. Herein, a novel and simple eco-friendly method, termed one-step air-assisted liquid-liquid microextraction (OS-AALLME), was developed to extract some illegal azo-based dyes (including Sudan I to IV, and Orange G) from food and cosmetic products. A series of experiments were investigated to achieve the most favorable conditions (including extraction solvent: 77μL of 1-Hexyl-3-methylimidazolium hexafluorophosphate; sample pH 6.3, without salt addition; and extraction cycles: 25 during 100s of sonication) using a central composite design strategy. Under these conditions, limits of detection, linear dynamic ranges, enrichment factors and consumptive indices were in the range of 3.9-84.8ngmL(-1), 0.013-3.1μgmL(-1), 33-39, and 0.13-0.15, respectively. The results showed that -as well as its simplicity, fastness, and use of no hazardous disperser and extraction solvents- OS-AALLME is an enough sensitive and efficient method for the extraction of these dyes from complex matrices. After optimization and validation, OS-AALLME was applied to estimate the concentration of 1-amino-2-naphthol in human bio-fluids as a main reductive metabolite of selected dyes. Levels of 1-amino-2-naphthol in plasma and urinary excretion suggested that this compound may be used as a new potential biomarker of these dyes in human body. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Evaluation of personal air sampling pumps

    International Nuclear Information System (INIS)

    Ritter, P.D.; Novick, V.J.; Alvarez, J.L.; Huntsman, B.L.

    1987-01-01

    Personal air samplers are used to more conveniently obtain breathing zone samples from individuals over periods of several hours. Personal air sampling pumps must meet minimum performance levels under all working conditions to be suitable for use in radiation protection programs. In addition, the pumps should be simple to operate and as comfortable to wear as possible. Ten models of personal air sampling pumps were tested to evaluate their mechanical performance and physical characteristics. The pumps varied over a wide range in basic performance and operating features. Some of the pumps were found to have adequate performance for use in health physics air sampling applications. 3 references, 2 figures, 5 tables

  19. Determination of plutonium in air and smear samples

    International Nuclear Information System (INIS)

    Hinton, E.R. Jr.; Tucker, W.O.

    1981-01-01

    A method has been developed for the determination of plutonium in air samples and smear samples that were collected on filter papers. The sample papers are digested in nitric acid, extracted into 2-thenoyltrifluoroacetone (TTA)-xylene, and evaporated onto stainless steel disks. Alpha spectrometry is employed to determine the activity of each plutonium isotope. Each sample is spiked with plutonium-236. All glassware used in the procedure is disposable. The detection limits are 3 and 5 dpm (disintegrations per minute) for air and smear samples, respectively, with an average recovery of 87%

  20. Evaluation of vacuum microwave-assisted extraction technique for the extraction of antioxidants from plant samples.

    Science.gov (United States)

    Xiao, Xiao-Hua; Wang, Jun-Xia; Wang, Gang; Wang, Jia-Yue; Li, Gong-Ke

    2009-12-18

    In the present work, vacuum microwave-assisted extraction (VMAE) was to perform microwave-assisted extraction in vacuum. Two well-known antioxidants, vitamin C from guava and green pepper, and vitamin E (alpha-tocopherol and gamma-tocopherol) from soybean and tea leaves, which were easy to be oxidized, were chosen as representative target compounds for the evaluation of VMAE. The extraction yields of vitamin C, alpha-tocopherol and gamma-tocopherol in VMAE and those in MAE performed in atmosphere (air-MAE) were compared and the effects of extraction time, extraction temperature and sample matrix were studied. Moreover, the effects of the oxygen and subpressure invacuo were also discussed via performed MAE in N(2) atmosphere (N(2)-MAE). The extraction yields of vitamin C, alpha-tocopherol and gamma-tocopherol in VMAE were higher than that in air-MAE, 35% increments of vitamin C from green pepper, 22% increments of alpha-tocopherol and 47% increments of gamma-tocopherol from tea leaves were obtained, respectively. The comparable increased extraction yields of vitamin C, alpha-tocopherol and gamma-tocopherol in N(2)-MAE to that in air-MAE confirmed that oxygen in system was the crucial factor for the oxidation of vitamin C and vitamin E, VMAE was beneficial for the extraction of these oxygen-sensitive compounds. In addition, the subpressure invacuo in the VMAE system also showed positive affect on the extraction yields. On the basis of preventing oxidation and improving extraction efficiency of target compounds because of less oxygen and subpressure invacuo in the extraction system, VMAE has good potential for the extraction of oxygen-sensitive and thermosensitive compounds from plant samples.

  1. Simultaneous derivatization and lighter-than-water air-assisted liquid-liquid microextraction using a homemade device for the extraction and preconcentration of some parabens in different samples.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Aghdam, Mehri Bakhshizadeh; Mogaddam, Mohammad Reza Afshar; Nabil, Ali Akbar Alizadeh

    2018-06-06

    Simultaneous derivatization and air-assisted liquid-liquid microextraction using an organic solvent lighter than water has been developed for the extraction of some parabens in different samples with the aid of a newly designed device for collecting the extractant. For this purpose, the sample solution is transferred into a glass test tube and a few microliters of acetic anhydride (as a derivatization agent) and p-xylene (as an extraction solvent) are added to the solution. After performing the procedure, the homemade device consists of an inverse funnel with a capillary tube placed into the tube. In this step, the collected extraction solvent and a part of the aqueous solution are transferred into the device and the organic phase indwells in the capillary tube of the device. Under the optimal conditions, limits of detection and quantification for the analytes were obtained in the ranges of 0.90-2.7 and 3.0-6.1 ng mL -1 , respectively. The enrichment and enhancement factors were in the ranges of 370-430 and 489-660, respectively. The method precision, expressed as the relative standard deviation, was within the ranges of 4-6% (n = 6) and 4-9% (n = 4) for intra- and inter-day precisions, respectively. The proposed method was successfully used for the determination of methyl-, ethyl-, and propyl parabens in cosmetic, hygiene, and food samples, and personal care products. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  2. Air sampling with solid phase microextraction

    Science.gov (United States)

    Martos, Perry Anthony

    There is an increasing need for simple yet accurate air sampling methods. The acceptance of new air sampling methods requires compatibility with conventional chromatographic equipment, and the new methods have to be environmentally friendly, simple to use, yet with equal, or better, detection limits, accuracy and precision than standard methods. Solid phase microextraction (SPME) satisfies the conditions for new air sampling methods. Analyte detection limits, accuracy and precision of analysis with SPME are typically better than with any conventional air sampling methods. Yet, air sampling with SPME requires no pumps, solvents, is re-usable, extremely simple to use, is completely compatible with current chromatographic equipment, and requires a small capital investment. The first SPME fiber coating used in this study was poly(dimethylsiloxane) (PDMS), a hydrophobic liquid film, to sample a large range of airborne hydrocarbons such as benzene and octane. Quantification without an external calibration procedure is possible with this coating. Well understood are the physical and chemical properties of this coating, which are quite similar to those of the siloxane stationary phase used in capillary columns. The log of analyte distribution coefficients for PDMS are linearly related to chromatographic retention indices and to the inverse of temperature. Therefore, the actual chromatogram from the analysis of the PDMS air sampler will yield the calibration parameters which are used to quantify unknown airborne analyte concentrations (ppb v to ppm v range). The second fiber coating used in this study was PDMS/divinyl benzene (PDMS/DVB) onto which o-(2,3,4,5,6- pentafluorobenzyl) hydroxylamine (PFBHA) was adsorbed for the on-fiber derivatization of gaseous formaldehyde (ppb v range), with and without external calibration. The oxime formed from the reaction can be detected with conventional gas chromatographic detectors. Typical grab sampling times were as small as 5 seconds

  3. Air sampling system for airborne surveys

    International Nuclear Information System (INIS)

    Jupiter, C.; Tipton, W.J.

    1975-01-01

    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

  4. Combination syringe provides air-free blood samples

    Science.gov (United States)

    Pool, S. L.

    1970-01-01

    Standard syringe and spinal needle are combined in unique manner to secure air-free blood samples. Combination syringe obtains air free samples because air bubbles become insignificant when samples greater than 1 cc are drawn.

  5. Sampling and analytical procedures for the determination of VOCs released into air from natural and anthropogenic sources: A comparison between SPME (Solid Phase Micro Extraction) and ST (Solid Trap) methods

    International Nuclear Information System (INIS)

    Tassi, F.; Capecchiacci, F.; Buccianti, A.; Vaselli, O.

    2012-01-01

    In the present study, two sampling and analytical methods for VOC determination in fumarolic exhalations related to hydrothermal-magmatic reservoirs in volcanic and geothermal areas and biogas released from waste landfills were compared: (a) Solid Traps (STs), consisting of three phase (Carboxen B, Carboxen C and Carbosieve S111) absorbent stainless steel tubes and (b) Solid Phase Micro Extraction (SPME) fibers, composed of DiVinylBenzene (DVB), Carboxen and PolyDimethylSiloxane. These techniques were applied to pre-concentrate VOCs discharged from: (i) low-to-high temperature fumaroles collected at Vulcano Island, Phlegrean Fields (Italy), and Nisyros Island (Greece), (ii) recovery wells in a solid waste disposal site located near Florence (Italy). A glass condensing system cooled with water was used to collect the dry fraction of the fumarolic gases, in order to allow more efficient VOC absorption avoiding any interference by water vapor and acidic gases, such as SO 2 , H 2 S, HF and HCl, typically present at relatively high concentrations in these fluids. Up to 37 organic species, in the range of 40–400 m/z, were determined by coupling gas chromatography to mass spectrometry (GC–MS). This study shows that the VOC compositions of fumaroles and biogas determined via SPME and ST are largely consistent and can be applied to the analysis of VOCs in gases released from different natural and anthropogenic environments. The SPME method is rapid and simple and more appropriate for volcanic and geothermal emissions, where VOCs are present at relatively high concentrations and prolonged gas sampling may be hazardous for the operator. The ST method, allowing the collection of large quantities of sample, is to be preferred to analyze the VOC composition of fluids from diffuse emissions and air, where these compounds are present at relatively low concentrations.

  6. Ambient krypton-85 air sampling at Hanford

    International Nuclear Information System (INIS)

    Trevathan, M.S.; Price, K.R.

    1985-01-01

    In the fall of 1982, the Environmental Evaluations Section of Pacific Northwest Laboratory (PNL) initiated a network of continuous 85 Kr air samplers located on and around the Hanford Site. This effort was in response to the resumption of operations at a nuclear fuel reprocessing plant located onsite where 85 Kr was to be released during fuel dissolution. Preoperational data were collected using noble gas samplers designed by the Environmental Protection Agency-Las Vegas (EPA-LV). The samplers functioned erratically resulting in excessive maintenance costs and prompted a search for a new sampling system. State-of-the-art 85 Dr sampling methods were reviewed and found to be too costly, too complex and inappropriate for field application, so a simple bag collection system was designed and field tested. The system is composed of a reinforced, heavy plastic bag, connected to a variable flow pump and housed in a weatherproof enclosure. At the end of the four week sampling period the air in the bag is transferred by a compressor into a pressure tank for easy transport to the laboratory for analysis. After several months of operation, the air sampling system has proven its reliability and sensitivity to ambient levels of 85 Kr

  7. Ambient krypton-85 air sampling at Hanford

    International Nuclear Information System (INIS)

    Trevathan, M.S.; Price, K.R.

    1984-10-01

    In the fall of 1982, the Environmental Evaluations Section of Pacific Northwest Laboratory (PNL) initiated a network of continuous krypton-85 air samplers located on and around the Hanford Site. This effort was in response to the resumption of operations at a nuclear fuel reprocessing plant located onsite where krypton-85 was to be released during fuel dissolution. Preoperational data were collected using noble gas samplers designed by the Environmental Protection Agency-Las Vegas (EPA-LV). The samplers functioned erratically resulting in excessive maintenance costs and prompted a search for a new sampling system. State of the art krypton-85 sampling methods were reviewed and found to be too costly, too complex and inappropriate for field application, so a simple bag collection system was designed and field tested. The system is composed of a reinforced, heavy plastic bag, connected to a variable flow pump and housed in a weatherproof enclosure. At the end of the four week sampling period the air in the bag is transferred by a compressor into a pressure tank for easy transport to the laboratory for analysis. After several months of operation, the air sampling system has proven its reliability and sensitivity to ambient levels of krypton-85. 3 references, 3 figures, 1 table

  8. Radon discrimination for work place air samples

    International Nuclear Information System (INIS)

    Bratvold, T.

    1994-01-01

    Gross alpha/beta measurement systems are designed solely to identify an incident particle as either an alpha or a beta and register a count accordingly. The tool of choice for radon identification, via decay daughters, is an instrument capable of identifying the energy of incident alpha particles and storing that information separately from detected alpha emissions of different energy. In simpler terms, the desired instrument is an alpha spectroscopy system. K Basins Radiological Control (KBRC) procured an EG ampersand G ORTEC OCTETE PC alpha spectroscopy system to facilitate radon identification on work place air samples. The alpha spectrometer allows for the identification of any alpha emitting isotope based on characteristic alpha emission energies. With this new capability, KBRC will explicitly know whether or not there exists a true airborne concern. Based on historical air quality data, this new information venue will reduce the use of respirators substantially. Situations where an area remains ''on mask'' due solely to the presence of radon daughters on the grab air filter will finally be eliminated. This document serves to introduce a new method for radon daughter detection at the 183KE Health Physics Analytical Laboratory (HPAL). A new work place air sampling analysis program will be described throughout this paper. There is no new technology being introduced, nor any unproven analytical process. The program defined over the expanse of this document simply explains how K Basins Radiological Control will employ their alpha spectrometer

  9. Permeability of gypsum samples dehydrated in air

    Science.gov (United States)

    Milsch, Harald; Priegnitz, Mike; Blöcher, Guido

    2011-09-01

    We report on changes in rock permeability induced by devolatilization reactions using gypsum as a reference analog material. Cylindrical samples of natural alabaster were dehydrated in air (dry) for up to 800 h at ambient pressure and temperatures between 378 and 423 K. Subsequently, the reaction kinetics, so induced changes in porosity, and the concurrent evolution of sample permeability were constrained. Weighing the heated samples in predefined time intervals yielded the reaction progress where the stoichiometric mass balance indicated an ultimate and complete dehydration to anhydrite regardless of temperature. Porosity showed to continuously increase with reaction progress from approximately 2% to 30%, whilst the initial bulk volume remained unchanged. Within these limits permeability significantly increased with porosity by almost three orders of magnitude from approximately 7 × 10-19 m2 to 3 × 10-16 m2. We show that - when mechanical and hydraulic feedbacks can be excluded - permeability, reaction progress, and porosity are related unequivocally.

  10. 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...

  11. Sampling and identification of gaseous and particle bounded air pollutants

    International Nuclear Information System (INIS)

    Kettrup, A.

    1993-01-01

    Air pollutants are gaseous, components of aerosols or particle bounded. Sampling, sample preparation, identification and quantification of compounds depend from kind and chemical composition of the air pollutants. Quality assurance of analytical data must be guaranted. (orig.) [de

  12. Air extraction in gas turbines burning coal-derived gas

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Tah-teh; Agrawal, A.K.; Kapat, J.S.

    1993-11-01

    In the first phase of this contracted research, a comprehensive investigation was performed. Principally, the effort was directed to identify the technical barriers which might exist in integrating the air-blown coal gasification process with a hot gas cleanup scheme and the state-of-the-art, US made, heavy-frame gas turbine. The guiding rule of the integration is to keep the compressor and the expander unchanged if possible. Because of the low-heat content of coal gas and of the need to accommodate air extraction, the combustor and perhaps, the flow region between the compressor exit and the expander inlet might need to be modified. In selecting a compressed air extraction scheme, one must consider how the scheme affects the air supply to the hot section of the turbine and the total pressure loss in the flow region. Air extraction must preserve effective cooling of the hot components, such as the transition pieces. It must also ensure proper air/fuel mixing in the combustor, hence the combustor exit pattern factor. The overall thermal efficiency of the power plant can be increased by minimizing the total pressure loss in the diffusers associated with the air extraction. Therefore, a study of airflow in the pre- and dump-diffusers with and without air extraction would provide information crucial to attaining high-thermal efficiency and to preventing hot spots. The research group at Clemson University suggested using a Griffith diffuser for the prediffuser and extracting air from the diffuser inlet. The present research establishes that the analytically identified problems in the impingement cooling flow are factual. This phase of the contracted research substantiates experimentally the advantage of using the Griffith diffuser with air extraction at the diffuser inlet.

  13. 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.

  14. Systematic Evaluation of Aggressive Air Sampling for Bacillus ...

    Science.gov (United States)

    Report The primary objectives of this project were to evaluate the Aggressive Air Sampling (AAS) method compared to currently used surface sampling methods and to determine if AAS is a viable option for sampling Bacillus anthracis spores.

  15. Accelerated Solvent Extraction: An Innovative Sample Extraction Technique for Natural Products

    International Nuclear Information System (INIS)

    Hazlina Ahmad Hassali; Azfar Hanif Abd Aziz; Rosniza Razali

    2015-01-01

    Accelerated solvent extraction (ASE) is one of the novel techniques that have been developed for the extraction of phytochemicals from plants in order to shorten the extraction time, decrease the solvent consumption, increase the extraction yield and enhance the quality of extracts. This technique combines elevated temperatures and pressure with liquid solvents. This paper gives a brief overview of accelerated solvent extraction technique for sample preparation and its application to the extraction of natural products. Through practical examples, the effects of operational parameters such as temperature, volume of solvent used, extraction time and extraction yields on the performance of ASE are discussed. It is demonstrated that ASE technique allows reduced solvent consumption and shorter extraction time, while the extraction yields are even higher than those obtained with conventional methods. (author)

  16. Crossett Hydrogen Sulfide Air Sampling Report

    Science.gov (United States)

    This report summarizes the results of the EPA’s hydrogen sulfide air monitoring conducted along Georgia Pacific’s wastewater treatment system and in surrounding Crossett, AR, neighborhoods in 2017.

  17. 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......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...... by easyMag® from the same fecal samples. Furthermore, DNA extracts obtained using easyMag® seemed to contain inhibitory compounds, since in order to perform a successful PCR-analysis, the sample should be diluted at least 10 times. DGGE performed on PCR from DNA extracted by QIAamp DNA Stool Mini Kit DNA...

  18. Compressed air-assisted solvent extraction (CASX) for metal removal.

    Science.gov (United States)

    Li, Chi-Wang; Chen, Yi-Ming; Hsiao, Shin-Tien

    2008-03-01

    A novel process, compressed air-assisted solvent extraction (CASX), was developed to generate micro-sized solvent-coated air bubbles (MSAB) for metal extraction. Through pressurization of solvent with compressed air followed by releasing air-oversaturated solvent into metal-containing wastewater, MSAB were generated instantaneously. The enormous surface area of MSAB makes extraction process extremely fast and achieves very high aqueous/solvent weight ratio (A/S ratio). CASX process completely removed Cr(VI) from acidic electroplating wastewater under A/S ratio of 115 and extraction time of less than 10s. When synthetic wastewater containing Cd(II) of 50mgl(-1) was treated, A/S ratios of higher than 714 and 1190 could be achieved using solvent with extractant/diluent weight ratio of 1:1 and 5:1, respectively. Also, MSAB have very different physical properties, such as size and density, compared to the emulsified solvent droplets, making separation and recovery of solvent from treated effluent very easy.

  19. Phytochemical Screening of Aqueous Extract of Luffa aegyptiaca (Sponge gourd) Leave Sample from Northern Nigeria: A Short Communication

    OpenAIRE

    Mhya DH; Mankilik, M

    2014-01-01

    Aqueous extract of the leaves of Luffa aegyptiaca was preliminary screened with the aim of assessing the availability of some biologically active compounds. Pulverized leaves sample of Luffa aegyptiaca was extracted with water; the filtrate was concentrated on water bath and then air-dried at 25oC. The prepared aqueous-extract was used for the phytochemical screening study which was carried out using standard methods. The phytochemicals screened from the aqueous extract of Luffa aegyptiaca sh...

  20. A simple air sampling technique for monitoring nitrous oxide pollution

    Energy Technology Data Exchange (ETDEWEB)

    Austin, J C; Shaw, R; Moyes, D; Cleaton-Jones, P E

    1981-01-01

    A simple, inexpensive device for the continuous low-flow sampling of air was devised to permit monitoring of pollution by gaseous anaesthetics. The device consisted of a water-filled Perspex cylinder in which a double-walled flexible-film gas sample collection bag was suspended. Air samples could be aspirated into the collection bag at flow rates of as low as 1 ml min-1 by allowing the water to drain from the cylinder at a controlled rate. The maintenance of sample integrity with aspiration and storage of samples of nitrous oxide in air at concentrations of 1000, 100 and 30 p.p.m. v/v was examined using gas chromatography. The sample bags retained a mean 94% of the nitrous oxide in air samples containing nitrous oxide 25 p.p.m. over a 72-h storage period.

  1. Venturi Air-Jet Vacuum Ejector For Sampling Air

    Science.gov (United States)

    Hill, Gerald F.; Sachse, Glen W.; Burney, L. Garland; Wade, Larry O.

    1990-01-01

    Venturi air-jet vacuum ejector pump light in weight, requires no electrical power, does not contribute heat to aircraft, and provides high pumping speeds at moderate suctions. High-pressure motive gas required for this type of pump bled from compressor of aircraft engine with negligible effect on performance of engine. Used as source of vacuum for differential-absorption CO-measurement (DACOM), modified to achieve in situ measurements of CO at frequency response of 10 Hz. Provides improvement in spatial resolution and potentially leads to capability to measure turbulent flux of CO by use of eddy-correlation technique.

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

    International Nuclear Information System (INIS)

    Metzger, R.L.; Jessop, B.H.; McDowell, B.L.

    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 3 O 8 . Profiles developed for U 3 O 8 samples show good agreement with in vitro and in vivo tests performed by other investigators on samples from the same uranium mills

  3. Workplace air monitoring and sampling practices at DOE facilities

    International Nuclear Information System (INIS)

    Swinth, K.L.; Kenoyer, J.L.; Selby, J.M.

    1987-01-01

    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

  4. Automated bar coding of air samples at Hanford (ABCASH)

    International Nuclear Information System (INIS)

    Troyer, G.L.; Brayton, D.D.; McNeece, S.G.

    1992-10-01

    This article describes the basis, main features and benefits of an automated system for tracking and reporting radioactive air particulate samples. The system was developed due to recognized need for improving the quality and integrity of air sample data related to personnel and environmental protection. The data capture, storage, and retrieval of air sample data are described. The automation aspect of the associated and data input eliminates a large potential for human error. The system utilizes personal computers, handheld computers, a commercial personal computer database package, commercial programming languages, and complete documentation to satisfy the system's automation objective

  5. Microfabricated Devices for Sample Extraction, Concentrations, and Related Sample Processing Technologies

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Gang; Lin, Yuehe

    2006-12-01

    This is an invited book chapter. As with other analytical techniques, sample pretreatments, sample extraction, sample introduction, and related techniques are of extreme importance for micro-electro-mechanical systems (MEMS). Bio-MEMS devices and systems start with a sampling step. The biological sample then usually undergoes some kinds of sample preparation steps before the actual analysis. These steps may involve extracting the target sample from its matrix, removing interferences from the sample, derivatizing the sample to detectable species, or performing a sample preconcentration step. The integration of the components for sample pretreatment into microfluidic devices represents one of the remaining the bottle-neck towards achieving true miniaturized total analysis systems (?TAS). This chapter provides a thorough state-of-art of the developments in this field to date.

  6. 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.

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

    International Nuclear Information System (INIS)

    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 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, 7 Be and 210 Pb, continue to be detected in most air filter samples. Variations in the annual mean concentrations of 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 7 Be and 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 7 Be, 95 Zr, 137 Cs, 144 Ce, and 210 Pb measured at sampling sites in SASP during 1990--1993 are presented. The weekly mean surface air concentrations of 7 Be, 95 Zr, 137 Cs, 144 Ce, and 210 Pb for samples collected during 1990--1993 are given for 17 sites

  8. Operational air sampling report, January--June 30, 1992

    International Nuclear Information System (INIS)

    Lyons, C.L.

    1992-09-01

    Nevada Test Site postshot and tunnel events generate beta/gamma fission products. The Reynolds Electrical ampersand Engineering Co., Inc. air sampling program is designed for measurement of these radionuclides at various facilities supporting these events. Monthly radon sampling is done for documentation of working levels in the tunnel complexes, which would be expected to hove the highest radon levels for on-site facilities. Out of a total of 281 air samples taken in the tunnel complexes, 25 showed airborne fission products with concentrations well below their respective Derived Air Concentrations (DAC). All of these were related to event reentry or mineback operations. Tritiated water vapor and radon levels were very similar to previously reported levels. The 975 air samples taken at the Area-6 decontamination bays and laundry were again well below any DAC calculation standard and negative for any airborne fission products from laboratory analyses

  9. Operational air sampling report, July 1--December 31, 1992

    International Nuclear Information System (INIS)

    Lyons, C.L.

    1993-04-01

    Nevada Test Site postshot and tunnel events generate beta/gamma fission products. The REECo air sampling program is designed for measurement of these radionuclides at various facilities supporting these events. Monthly radon sampling is done for documentation of working levels in the tunnel complexes, which would be expected to have the highest radon levels for on-site facilities. Out of a total of 628 air samples taken in the tunnel complexes, 24 showed airborne fission products with concentrations well below their respective Derived Air Concentrations (DAC). All of these were related to event reentry or mineback operations. Tritiated water vapor concentrations were very similar to previously reported levels. The 838 air samples taken at the Area-6 decontamination bays and laundry were again well below any DAC calculation standard and negative for any airborne fission products from laboratory analyses

  10. Rapid extraction and assay of uranium from environmental surface samples

    Energy Technology Data Exchange (ETDEWEB)

    Barrett, Christopher A.; Chouyyok, Wilaiwan; Speakman, Robert J.; Olsen, Khris B.; Addleman, Raymond Shane

    2017-10-01

    Extraction methods enabling faster removal and concentration of uranium compounds for improved trace and low-level assay are demonstrated for standard surface sampling material in support of nuclear safeguards efforts, health monitoring, and other nuclear analysis applications. A key problem with the existing surface sampling swipes is the requirement for complete digestion of sample and sampling matrix. This is a time-consuming and labour-intensive process that limits laboratory throughput, elevates costs, and increases background levels. Various extraction methods are explored for their potential to quickly and efficiently remove different chemical forms of uranium from standard surface sampling material. A combination of carbonate and peroxide solutions is shown to give the most rapid and complete form of uranyl compound extraction and dissolution. This rapid extraction process is demonstrated to be compatible with standard inductive coupled plasma mass spectrometry methods for uranium isotopic assay as well as screening techniques such as x-ray fluorescence. The general approach described has application beyond uranium to other analytes of nuclear forensic interest (e.g., rare earth elements and plutonium) as well as heavy metals for environmental and industrial hygiene monitoring.

  11. 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...

  12. Ultrasonic assisted extraction - an alternative for sample preparation (M4)

    International Nuclear Information System (INIS)

    Santos Junior, P.; Barbosa Junior, F.; Krug, F.J.; Trevizan, L.C.; Nobrega, J.A.

    2002-01-01

    Full text: In the last years the ultrasound assisted metal extraction has been frequency proposed as a simple and inexpensive alternative for sample preparation of biological and inorganic samples. The extraction effect is considered as being caused by acoustic cavitation, that is, bubble formation and subsequent disruptive action. The collapse of bubbles created by sonication of solutions results in the generation of extremely high local temperature and pressure gradients, which may be regarded as localized 'hot spots'. On a timescale of about 10 -10 s, effective local pressures and temperature of about 10 5 atm and about 5000 K, respectively, are generated under sonochemical conditions. Usually, this method uses a diluted acid medium decreasing blank values and reducing both reagents and time consumption compared to traditional wet digestion systems using conductive or microwave-assisted heating. Furthermore, sonication can also allow the preparation of samples directly within the sample container, thereby preventing sample losses and minimizing sample contamination. Although some controversial results concerning metals extraction behavior have been reported, they could be explained by analyte-matrix interaction and the ability of the ultrasonic processor to generate ultrasound (i.e. the use of an ultrasonic bath or an ultrasonic probe at different power, frequency, and amplitude). This contribution presents a review of ultrasound assisted metal extraction and recent performance data obtained in our laboratory for determination of elements in biological materials, soils and sediments by ICP-OES and ETAAS. The effect of extraction parameters, such as type and concentration of the leaching solution, sonication time and performance of ultrasonic processor (bath or probe) will be presented. (author)

  13. Measurements of acetylene in air extracted from polar ice cores

    Science.gov (United States)

    Nicewonger, M. R.; Aydin, M.; Montzka, S. A.; Saltzman, E. S.

    2016-12-01

    Acetylene (ethyne) is a non-methane hydrocarbon emitted during combustion of fossil fuels, biofuels, and biomass. The major atmospheric loss pathway of acetylene is oxidation by hydroxyl radical with a lifetime estimated at roughly two weeks. The mean annual acetylene levels over Greenland and Antarctica are 250 ppt and 20 ppt, respectively. Firn air measurements suggest atmospheric acetylene is preserved unaltered in polar snow and firn. Atmospheric reconstructions based on firn air measurements indicate acetylene levels rose significantly during the twentieth century, peaked near 1980, then declined to modern day levels. This historical trend is similar to that of other fossil fuel-derived non-methane hydrocarbons. In the preindustrial atmosphere, acetylene levels should primarily reflect emissions from biomass burning. In this study, we present the first measurements of acetylene in preindustrial air extracted from polar ice cores. Air from fluid and dry-drilled ice cores from Summit, Greenland and WAIS-Divide Antarctica is extracted using a wet-extraction technique. The ice core air is analyzed using gas chromatography and high-resolution mass spectrometry. Between 1400 to 1800 C.E., acetylene levels over Greenland and Antarctica varied between roughly 70-120 ppt and 10-30 ppt, respectively. The preindustrial Greenland acetylene levels are significantly lower than modern levels, reflecting the importance of northern hemisphere fossil fuel sources today. The preindustrial Antarctic acetylene levels are comparable to modern day levels, indicating similar emissions in the preindustrial atmosphere, likely from biomass burning. The implications of the preindustrial atmospheric acetylene records from both hemispheres will be discussed.

  14. Occurrence and distribution of extractable and non-extractable GDGTs in podzols: implications for the reconstruction of mean air temperature

    Science.gov (United States)

    Huguet, Arnaud; Fosse, Céline; Metzger, Pierre; Derenne, Sylvie

    2010-05-01

    Glycerol dialkyl glycerol tetraethers (GDGTs) are complex lipids of high molecular weight, present in cell membranes of archaea and some bacteria. Archaeal membranes are formed predominantly by isoprenoid GDGTs with acyclic or ring-containing biphytanyl chains. Another type of GDGTs with branched instead of isoprenoid alkyl chains was recently discovered in soils. Branched tetraethers were suggested to be produced by anaerobic bacteria and can be used to reconstruct past air temperature and soil pH. Lipids preserved in soils can take two broad chemical forms: extractable lipids, recoverable upon solvent extraction, and non-extractable lipids, linked to the organic or mineral matrix of soils. Moreover, within the extractable pool, core (i.e. "free") lipids and intact polar (i.e. "bound") lipids can be distinguished. These three lipid fractions may respond to environmental changes in different ways and the information derived from these three pools may differ. The aim of the present work was therefore to compare the abundance and distribution of the three GDGT pools in two contrasted podzols: a temperate podzol located 40 km north of Paris and a tropical podzol from the upper Amazon Basin. Five samples were collected from the whole profile of the temperate podzol including the litter layer. Five additional samples were obtained from three profiles of the tropical soil sequence, representative of the transition between a latosol and a well-developed podzol. Vertical and/or lateral variations in GDGT content and composition were highlighted. In particular, in the tropical sequence, GDGTs were present at relatively low concentrations in the early stages of podzolisation and were more abundant in the well-developed podzolic horizons, where higher acidity and increased bacterial activity may favour their stabilization. Concerning the temperate podzol, GDGT distribution was shown to vary greatly with depth in the soil profile, the methylation degree of bacterial GDGTs

  15. Neutron activation analysis for the optimal sampling and extraction of extractable organohalogens in human hari

    International Nuclear Information System (INIS)

    Zhang, H.; Chai, Z.F.; Sun, H.B.; Xu, H.F.

    2005-01-01

    Many persistent organohalogen compounds such as DDTs and polychlorinated biphenyls have caused seriously environmental pollution problem that now involves all life. It is know that neutron activation analysis (NAA) is a very convenient method for halogen analysis and is also the only method currently available for simultaneously determining organic chlorine, bromine and iodine in one extract. Human hair is a convenient material to evaluate the burden of such compounds in human body and dan be easily collected from people over wide ranges of age, sex, residential areas, eating habits and working environments. To effectively extract organohalogen compounds from human hair, in present work the optimal Soxhelt-extraction time of extractable organohalogen (EOX) and extractable persistent organohalogen (EPOX) from hair of different lengths were studied by NAA. The results indicated that the optimal Soxhelt-extraction time of EOX and EPOX from human hair was 8-11 h, and the highest EOX and EPOX contents were observed in hair powder extract. The concentrations of both EOX and EPOX in different hair sections were in the order of hair powder ≥ 2 mm > 5 mm, which stated that hair samples milled into hair powder or cut into very short sections were not only for homogeneous. hair sample but for the best hair extraction efficiency.

  16. Extraction of DNA from Forensic Biological Samples for Genotyping.

    Science.gov (United States)

    Stray, J E; Liu, J Y; Brevnov, M G; Shewale, J G

    2010-07-01

    Biological forensic samples constitute evidence with probative organic matter. Evidence believed to contain DNA is typically processed for extraction and purification of its nucleic acid content. Forensic DNA samples are composed of two things, a tissue and the substrate it resides on. Compositionally, a sample may contain almost anything and for each, the type, integrity, and content of both tissue and substrate will vary, as will the contaminant levels. This fact makes the success of extraction one of the most unpredictable steps in genotypic analysis. The development of robust genotyping systems and analysis platforms for short tandem repeat (STR) and mitochondrial DNA sequencing and the acceptance of results generated by these methods in the court system, resulted in a high demand for DNA testing. The increasing variety of sample submissions created a need to isolate DNA from forensic samples that may be compromised or contain low levels of biological material. In the past decade, several robust chemistries and isolation methods have been developed to safely and reliably recover DNA from a wide array of sample types in high yield and free of PCR inhibitors. In addition, high-throughput automated workflows have been developed to meet the demand for processing increasing numbers of samples. This review summarizes a number of the most widely adopted methods and the best practices for DNA isolation from forensic biological samples, including manual, semiautomated, and fully automated platforms. Copyright © 2010 Central Police University.

  17. Printed Self-Powered Miniature Air Sampling Sensors

    Directory of Open Access Journals (Sweden)

    Joseph Birmingham

    2017-07-01

    Full Text Available The recent geo-political climate has increased the necessity for autonomous, chip-sized, lightweight, air sampling systems which can quickly detect and characterize chemical, biological, radiological, nuclear, and high explosive (CBRNE hazardous materials and relay the results. To address these issues, we have developed a self-powered 3-D chip architecture that processes air to produce concentrated size- sorted particle (and vapor samples that could be integrated with on-chip nanoelectronic detectors for the discovery of weapons of mass destruction (WMD. The unique air movement approach is composed of a nanoscale energy harvester that provides electricity to a printed ion-drag pump to push air through coated-microstructured arrays. The self-powered microstructured array air sampler was designed using computational fluid dynamics (CFD modeling to collect particles from 1-10 microns at greater than 99.9999 % efficiency with less than 100 Pascal [Pa] pressure drop at a specified air flow rate. Surprisingly, even at minimum air flow rates below specifications, these CFD predictions were matched by experimental results gathered in a Government aerosol chamber. The microstructured array engineered filter equaled the collection capability of a membrane or a high efficiency particle air (HEPA filter at a fraction of the filter pressure drop.

  18. Experimental verification of air flow rate measurement for representative isokinetic air sampling in ventilation stacks

    International Nuclear Information System (INIS)

    Okruhlica, P.; Mrtvy, M.; Kopecky, Z.

    2009-01-01

    Nuclear facilities are obliged to monitor their discharge's influence on environment. Main monitored factions in NPP's ventilation stacks are usually noble gasses, particulates and iodine. These factions are monitored in air sampled from ventilation stack by means of sampling rosette and bypass followed with on-line measuring monitors and balance sampling devices with laboratory evaluations. Correct air flow rate measurement and representative iso-kinetic air sampling system is essential for physical correct and metrological accurate evaluation of discharge influence on environment. Pairs of measuring sensors (Anemometer, pressure gauge, thermometer and humidity meter) are symmetrically placed in horizontal projection of stack on positions based on measured air flow velocity distribution characteristic, Analogically diameter of sampling rosette nozzles and their placement in the middle of 6 - 7 annuluses are calculated for assurance of representative iso-kinetic sampling. (authors)

  19. Experimental verification of air flow rate measurement for representative isokinetic air sampling in ventilation stacks

    International Nuclear Information System (INIS)

    Okruhlica, P.; Mrtvy, M.; Kopecky, Z.

    2008-01-01

    Nuclear facilities are obliged to monitor their discharge's influence on environment. Main monitored factions in NPP's ventilation stacks are usually noble gasses, particulates and iodine. These factions are monitored in air sampled from ventilation stack by means of sampling rosette and bypass followed with on-line measuring monitors and balance sampling devices with laboratory evaluations. Correct air flow rate measurement and representative iso-kinetic air sampling system is essential for physical correct and metrological accurate evaluation of discharge influence on environment. Pairs of measuring sensors (Anemometer, pressure gauge, thermometer and humidity meter) are symmetrically placed in horizontal projection of stack on positions based on measured air flow velocity distribution characteristic, Analogically diameter of sampling rosette nozzles and their placement in the middle of 6- 7 annuluses are calculated for assurance of representative iso-kinetic sampling. (authors)

  20. Operational air sampling report, July--December 1991

    International Nuclear Information System (INIS)

    Lyons, C.L.

    1992-11-01

    Air sampling is one of the more useful ways of assessing the effectiveness of operational radiation safety programs at the Nevada Test Site (NTS). Air sampling programs document NTS airborne radionuclide concentrations in various work locations and environments. These concentrations generally remain well below the Derived Air Concentration (DAC) values prescribed by the Department of Energy (DOE 5480.11, Attachment 1) or the Derived Concentration Guide (DCG) values prescribed by the Department of Energy DOE 5400.5, Chapter Ill. The Defense Nuclear Agency (DNA) tunnel complexes, Area 12 Test Support Compound and the Area 6 Decontamination Pad and Laundry air sampling programs are summarized in this report. Evaluations are based on Analytical Services Department (ASD) Counting Laboratory analyses and Health Protection Department (HPD)/Radiological Field Operations Section (RFOS) radiation protection technician's (RPT) or health physicists' calculations for air samples collected July 1 through December 31, 1991. Of the NTS operational air sampling programs in the tunnel complexes, the initial mining and event reentry and recovery operations represent the only real airborne radioactive inhalation potentials to personnel. Monthly filter and scintillation cell samples were taken and counted in RDA-200 Radon Detectors to document working levels of radon/thoron daughters and picocurie/liter (PCVL) concentrations of radon gas. Weekly Drierite samples for tritium analysis were taken in the active tunnel complexes to document any changes in normal background levels or reentry drifts as they are advanced toward ground zero (GZ) areas. Underground water sources are considered primary transporters of tritium from old event areas

  1. 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).

  2. Hypercrosslinked particles for the extraction of sweeteners using dispersive solid-phase extraction from environmental samples.

    Science.gov (United States)

    Lakade, Sameer S; Zhou, Qing; Li, Aimin; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa M

    2018-04-01

    This work presents a new extraction material, namely, Q-100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid-phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q-100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior toward sweeteners. Different dispersive solid-phase extraction parameters such as amount of magnetic particles or extraction time were optimized. Under optimum conditions, Q-100 showed suitable apparent recovery, ranging in the case of river water sample from 21 to 88% for all the sweeteners, except for alitame (12%). The validated method based on dispersive solid-phase extraction using Q-100 followed by liquid chromatography with tandem mass spectrometry provided good linearity and limits of quantification between 0.01 and 0.1 μg/L. The method was applied to analyze samples from river water and effluent wastewater, and four sweeteners (acesulfame, saccharin, cyclamate, and sucralose) were found in both types of sample. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. 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.

  4. 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.

  5. Enhanced spot preparation for liquid extractive sampling and analysis

    Science.gov (United States)

    Van Berkel, Gary J.; King, Richard C.

    2015-09-22

    A method for performing surface sampling of an analyte, includes the step of placing the analyte on a stage with a material in molar excess to the analyte, such that analyte-analyte interactions are prevented and the analyte can be solubilized for further analysis. The material can be a matrix material that is mixed with the analyte. The material can be provided on a sample support. The analyte can then be contacted with a solvent to extract the analyte for further processing, such as by electrospray mass spectrometry.

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

    Science.gov (United States)

    Punín Crespo, M O; Lage Yusty, M A

    2005-06-01

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

  7. Sample design considerations of indoor air exposure surveys

    International Nuclear Information System (INIS)

    Cox, B.G.; Mage, D.T.; Immerman, F.W.

    1988-01-01

    Concern about the potential for indoor air pollution has prompted recent surveys of radon and NO 2 concentrations in homes and personal exposure studies of volatile organics, carbon monoxide and pesticides, to name a few. The statistical problems in designing sample surveys that measure the physical environment are diverse and more complicated than those encountered in traditional surveys of human attitudes and attributes. This paper addresses issues encountered when designing indoor air quality (IAQ) studies. General statistical concepts related to target population definition, frame creation, and sample selection for area household surveys and telephone surveys are presented. The implications of different measurement approaches are discussed, and response rate considerations are described

  8. Polycyclic aromatic hydrocarbons in air samples of meat smokehouses

    DEFF Research Database (Denmark)

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

    1992-01-01

    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 approx......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...

  9. 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/. © The Author(s) 2016. Published by Oxford University Press.

  10. Air sampling program at the Portsmouth Gaseous Diffusion Plant

    International Nuclear Information System (INIS)

    Hulett, S.H.

    1975-01-01

    An extensive air sampling program has been developed at the Portsmouth Gaseous Diffusion Plant for monitoring the concentrations of radioactive aerosols present in the atmosphere on plantsite as well as in the environs. The program is designed to minimize exposures of employees and the environment to airborne radioactive particulates. Five different air sampling systems, utilizing either filtration or impaction, are employed for measuring airborne alpha and beta-gamma activity produced from 235 U and 234 Th, respectively. Two of the systems have particle selection capabilities: a personal sampler with a 10-mm nylon cyclone eliminates most particles larger than about 10 microns in diameter; and an Annular Kinetic Impactor collects particulates greater than 0.4 microns in diameter which have a density greater than 12-15 gm/cm 3 . A Hi-Volume Air Sampler and an Eberline Model AIM-3 Scintillation Air Monitor are used in collecting short-term samples for assessing compliance with ''ceiling'' standards or peak concentration limits. A film-sort aperture IBM card system is utilized for continuous 8-hour samples. This sampling program has proven to be both practical and effective for assuring accurate monitoring of the airborne activity associated with plant operations

  11. Sampling density for the quantitative evaluation of air trapping

    International Nuclear Information System (INIS)

    Goris, Michael L.; Robinson, Terry E.

    2009-01-01

    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.)

  12. Stir Bar Sorptive Extraction (SBSE), a novel extraction technique for aqueous samples: theory and principles

    NARCIS (Netherlands)

    Baltussen, H.A.; Sandra, P.J.F.; David, F.; Cramers, C.A.M.G.

    1999-01-01

    The theory and practice of a novel approach for sample enrichment, namely the application of stir bars coated with the sorbent polydimethylsiloxane (PDMS) and referred to as stir bar sorptive extraction (SBSE) are presented. Stir bars with a length of 10 and 40 mm coated with 55 and 219 L of PDMS

  13. Micro-electromembrane extraction across free liquid membranes. Extractions of basic drugs from undiluted biological samples

    Czech Academy of Sciences Publication Activity Database

    Kubáň, Pavel; Boček, Petr

    2014-01-01

    Roč. 1337, Apr (2014), s. 32-39 ISSN 0021-9673 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : micro-electromembrane extraction * free liquid membranes * biological samples Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.169, year: 2014

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

    Science.gov (United States)

    Ledesma-Escobar, Carlos A.; 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 extraction method on the profile of flavonoids isolated from lemon. Results 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. Conclusions The present study shows clear discrimination caused by both sample pretreatments and extraction methods. Under the studied

  15. 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

    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....... 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....

  16. Methods for Sampling and Measurement of Compressed Air Contaminants

    International Nuclear Information System (INIS)

    Stroem, L.

    1976-10-01

    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

  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)

    Tanaka, A.; Ishii, K.; Komori, Y.

    2002-01-01

    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. Efficient sample preparation from complex biological samples using a sliding lid for immobilized droplet extractions.

    Science.gov (United States)

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

    2014-07-01

    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 (with immobilized analyte-bound PMPs). In this paper, we explore the third and least studied method for PMP-based sample preparation using a platform termed Sliding Lid for Immobilized Droplet Extractions (SLIDE). SLIDE leverages principles of surface tension and patterned hydrophobicity to create a simple-to-operate platform for sample isolation (cells, DNA, RNA, protein) and preparation (cell staining) without the need for time-intensive wash steps, use of immiscible fluids, or precise pinning geometries. Compared to other standard isolation protocols using PMPs, SLIDE is able to perform rapid sample preparation with low (0.6%) carryover of contaminants from the original sample. The natural recirculation occurring within the pinned droplets of SLIDE make possible the performance of multistep cell staining protocols within the SLIDE by simply resting the lid over the various sample droplets. SLIDE demonstrates a simple easy to use platform for sample preparation on a range of complex biological samples.

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

    International Nuclear Information System (INIS)

    Fox, R.V.; Mincher, B.J.; Holmes, R.G.G.

    1999-01-01

    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

  1. Programmable automatic alpha--beta air sample counter

    International Nuclear Information System (INIS)

    Howell, W.P.

    1978-01-01

    A programmable automatic alpha-beta air sample counter was developed for routine sample counting by operational health physics personnel. The system is composed of an automatic sample changer utilizing a large silicon diode detector, an electronic counting system with energy analysis capability, an automatic data acquisition controller, an interface module, and a teletypewriter with paper tape punch and paper tape reader. The system is operated through the teletypewriter keyboard and the paper tape reader, which are used to instruct the automatic data acquisition controller. Paper tape programs are provided for background counting, Chi 2 test, and sample counting. Output data are printed by the teletypewriter on standard continuous roll or multifold paper. Data are automatically corrected for background and counter efficiency

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

    International Nuclear Information System (INIS)

    Kanekar, A.S.; Pathak, P.N.; Acharya, R.; Mohapatra, P.K.; Manchanda, V.K.

    2011-01-01

    Direct extraction of uranium from different samples viz. sintered UO 2 , soil and ores was carried out by modifier free supercritical fluid using tri-n-butyl phosphate-nitric acid (TBP-HNO 3 ) adduct as extractant. These studies showed that pre-equilibration with more concentrated nitric acid helps in better dissolution and extraction of uranium from sintered UO 2 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)

  3. 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.

  4. Study on sampling conditions for the monitoring of waste air

    International Nuclear Information System (INIS)

    Moeller, T.J.; Buetefisch, K.A.

    1998-01-01

    The technical codes for radiological monitoring of the waste air released from a radwaste repository demand that sampling for determination of aerosol-borne radioactivity is to be made with a screener equipped with a suitable number of measuring probes extending over the entire cross-sectional surface of the vent. Another requirement is to ensure that the waste air stream passing through the measuring channel is representative, containing the typical, operation-induced distribution of aerosols across the surface to be scanned. The study reported was intended to determine in a scaled-down model (1:10) of a repository ventilating duct the typical spatial distribution of aerosols (3D particulate density) in order to establish information on the type of typical distributions of aerosols, to be used for optimisation of the measuring site and monitoring instruments. (orig./CB) [de

  5. Using silver nano particles for sampling of toxic mercury vapors from industrial air sample

    Directory of Open Access Journals (Sweden)

    M. Osanloo

    2014-05-01

    .Conclusion: The presented adsorbent is very useful for sampling of the trace amounts of mercury vapors from air. Moreover, it can be regenerated easily is suitable or sampling at 25 to 70 °C. Due to oxidation of silver and reduction in uptake of nanoparticles, oven temperature of 245 °C is used for the recovery of metallic silver. Low amount of adsorbent, high absorbency, high repeatability for sampling, low cost and high accuracy are of the advantages of the presented method.

  6. 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.

  7. The air quality in inhabited areas located near from a petroleum perforation and extraction company

    International Nuclear Information System (INIS)

    Colas, J.; Diaz, M.; Fuentes, E.; Teutelo, R.

    2003-01-01

    The quality of the air is studied in inhabited areas located near from a petroleum perforation and extraction company. Three halfway points of the areas of more racking and of treatment of product were selected and it was determined the day variation of the levels of concentration of SO2 and SH2 with a frequency of sampling of every 6 hours. By means of the statistical analysis it concludes that the ambient air in the valued points receives a severe contamination with directions of East component wind and variable speed, and the potential sources of emissions that influence on each point settle down. It is recommended to improve the hermetic in the storage and pumping of crude oil systems in the central battery of the company to minimize the fugitive emissions of SH2

  8. 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.

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

    Science.gov (United States)

    Andrew, Andrea; Del Vecchio, Rossana; Zhang, Yi; Subramaniam, Ajit; Blough, Neil

    2016-02-01

    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.

  10. Are Extracted Materials Truly Representative of Original Samples? Impact of C18 Extraction on CDOM Optical and Chemical Properties.

    Science.gov (United States)

    Andrew, Andrea A; Del Vecchio, Rossana; Zhang, Yi; Subramaniam, Ajit; Blough, Neil V

    2016-01-01

    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 (SPE) 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.

  11. Extractive sampling and optical remote sensing of F100 aircraft engine emissions.

    Science.gov (United States)

    Cowen, Kenneth; Goodwin, Bradley; Joseph, Darrell; Tefend, Matthew; Satola, Jan; Kagann, Robert; Hashmonay, Ram; Spicer, Chester; Holdren, Michael; Mayfield, Howard

    2009-05-01

    The Strategic Environmental Research and Development Program (SERDP) has initiated several programs to develop and evaluate techniques to characterize emissions from military aircraft to meet increasingly stringent regulatory requirements. This paper describes the results of a recent field study using extractive and optical remote sensing (ORS) techniques to measure emissions from six F-15 fighter aircraft. Testing was performed between November 14 and 16, 2006 on the trim-pad facility at Tyndall Air Force Base in Panama City, FL. Measurements were made on eight different F100 engines, and the engines were tested on-wing of in-use aircraft. A total of 39 test runs were performed at engine power levels that ranged from idle to military power. The approach adopted for these tests involved extractive sampling with collocated ORS measurements at a distance of approximately 20-25 nozzle diameters downstream of the engine exit plane. The emission indices calculated for carbon dioxide, carbon monoxide, nitric oxide, and several volatile organic compounds showed very good agreement when comparing the extractive and ORS sampling methods.

  12. Speciation of 210Po and 210Pb in air particulates determined by sequential extraction

    International Nuclear Information System (INIS)

    Al-Masri, M.S.; Al-Karfan, K.; Khalili, H.; Hassan, M.

    2006-01-01

    Speciation of 210 Po and 210 Pb in air particulates of two Syrian phosphate sites with different climate conditions has been studied. The sites are the mines and Tartous port at the Mediterranean Sea. Air filters were collected during September 2000 until February 2002 and extracted chemically using different selective fluids in an attempt to identify the different forms of these two radionuclides. The results have shown that the inorganic and insoluble 21 Po and 21 Pb (attached to silica and soluble in mineral acids) portion was found to be high in both sites and reached a maximum value of 94% and 77% in the mine site and Tartous port site, respectively. In addition, only 24% of 21 Pb in air particulates was found to be associated with organic materials probably produced from the incomplete burning of fuel vehicle and similar activities. Moreover, the 210 Po/ 21- Pb activity ratio in air particulates was higher than that in all samples at both sites and varied between 3.85 in November 2000 at Tartous port site and 20 in April 2001 at the mine area. These activity ratios were also higher than the natural levels. The 210 Po/ 210 Pb activity ratio was also determined in each portion resulting from the selective extraction and found to be higher than that in most samples. The sources of 210 Po excess in these portions are discussed. Soil suspension, which is common in the dry climate dominant in the area, sea water spray and heating of phosphate ores were considered; polonium is more volatile than the lead compounds at even moderate temperature. Furthermore, variations in the chemical forms of 210 Po and 210 Pb during the year were also investigated. However, the results of this study can also be utilized for dose assessment to phosphate industry workers

  13. Speciation of 210Po and 210Pb in air particulates determined by sequential extraction.

    Science.gov (United States)

    Al-Masri, M S; Al-Karfan, K; Khalili, H; Hassan, M

    2006-01-01

    Speciation of (210)Po and (210)Pb in air particulates of two Syrian phosphate sites with different climate conditions has been studied. The sites are the mines and Tartous port at the Mediterranean Sea. Air filters were collected during September 2000 until February 2002 and extracted chemically using different selective fluids in an attempt to identify the different forms of these two radionuclides. The results have shown that the inorganic and insoluble (210)Po and (210)Pb (attached to silica and soluble in mineral acids) portion was found to be high in both sites and reached a maximum value of 94% and 77% in the mine site and Tartous port site, respectively. In addition, only 24% of (210)Pb in air particulates was found to be associated with organic materials probably produced from the incomplete burning of fuel vehicle and similar activities. Moreover, the (210)Po/(210)Pb activity ratio in air particulates was higher than that in all samples at both sites and varied between 3.85 in November 2000 at Tartous port site and 20 in April 2001 at the mine area. These activity ratios were also higher than the natural levels. The (210)Po/(210)Pb activity ratio was also determined in each portion resulting from the selective extraction and found to be higher than that in most samples. The sources of (210)Po excess in these portions are discussed. Soil suspension, which is common in the dry climate dominant in the area, sea water spray and heating of phosphate ores were considered; polonium is more volatile than the lead compounds at even moderate temperature. Furthermore, variations in the chemical forms of (210)Po and (210)Pb during the year were also investigated. However, the results of this study can also be utilized for dose assessment to phosphate industry workers.

  14. Sample-based XPath Ranking for Web Information Extraction

    NARCIS (Netherlands)

    Jundt, Oliver; van Keulen, Maurice

    Web information extraction typically relies on a wrapper, i.e., program code or a configuration that specifies how to extract some information from web pages at a specific website. Manually creating and maintaining wrappers is a cumbersome and error-prone task. It may even be prohibitive as some

  15. Uncertainties in monitoring of SVOCs in air caused by within-sampler degradation during active and passive air sampling

    Science.gov (United States)

    Melymuk, Lisa; Bohlin-Nizzetto, Pernilla; Prokeš, Roman; Kukučka, Petr; Přibylová, Petra; Vojta, Šimon; Kohoutek, Jiří; Lammel, Gerhard; Klánová, Jana

    2017-10-01

    Degradation of semivolatile organic compounds (SVOCs) occurs naturally in ambient air due to reactions with reactive trace gases (e.g., ozone, NOx). During air sampling there is also the possibility for degradation of SVOCs within the air sampler, leading to underestimates of ambient air concentrations. We investigated the possibility of this sampling artifact in commonly used active and passive air samplers for seven classes of SVOCs, including persistent organic pollutants (POPs) typically covered by air monitoring programs, as well as SVOCs of emerging concern. Two active air samplers were used, one equipped with an ozone denuder and one without, to compare relative differences in mass of collected compounds. Two sets of passive samplers were also deployed to determine the influence of degradation during longer deployment times in passive sampling. In active air samplers, comparison of the two sampling configurations suggested degradation of particle-bound polycyclic aromatic hydrocarbons (PAHs), with concentrations up to 2× higher in the denuder-equipped sampler, while halogenated POPs did not have clear evidence of degradation. In contrast, more polar, reactive compounds (e.g., organophosphate esters and current use pesticides) had evidence of losses in the sampler with denuder. This may be caused by the denuder itself, suggesting sampling bias for these compounds can be created when typical air sampling apparatuses are adapted to limit degradation. Passive air samplers recorded up to 4× higher concentrations when deployed for shorter consecutive sampling periods, suggesting that within-sampler degradation may also be relevant in passive air monitoring programs.

  16. 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)

    Wang Pu; Zhang Qinghua; Wang Yawei; Wang Thanh; Li Xiaomin; Ding Lei; Jiang Guibin

    2010-01-01

    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 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.

  17. 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.

  18. STORAGE STABILITY OF PESTICIDES IN EXTRACT SOLVENTS AND SAMPLING MEDIA

    Science.gov (United States)

    Demonstrating that pesticides are stable in field media and their extracts over extended storage periods allows operational flexibility and cost efficiency. Stability of the 31 neutral pesticides and 2 acid herbicides of the Agricultural Health Study exposure pilot was evaluate...

  19. Air sparging/high vacuum extraction to remove chlorinated solvents in groundwater and soil

    International Nuclear Information System (INIS)

    Phelan, J.M.; Gilliat, M.D.

    1998-01-01

    An air sparging and high vacuum extraction was installed as an alternative to a containment pump and treat system to reduce the long-term remediation schedule. The site is located at the DOE Mound facility in Miamisburg, Ohio, just south of Dayton. The air sparging system consists of 23 wells interspersed between 17 soil vapor extraction wells. The SVE system has extracted about 1,500 lbs of VOCs in five months. The air sparging system operated for about 6 weeks before shutdown due to suspected biochemical fouling. Technical data are presented on the operating characteristics of the system

  20. 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 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 extraction......) and on a laboratory scale (grams; mild oxalic acid extraction). Pectin composition (acidic and neutral sugars) and physicochemical properties (molar mass and intrinsic viscosity) were determined. Key Results Oxalic acid extraction allowed the recovery of pectin samples of high molecular weight. Mild oxalic acid......-extracted pectins were rich in long homogalacturonan stretches and contained rhamnogalacturonan I stretches with conserved side chains. Nitric acid-extracted pectins exhibited lower molecular weights and contained rhamnogalacturonan I stretches encompassing few and/or short side chains. Grapefruit pectin was found...

  1. 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

  2. An analytical method for trifluoroacetic Acid in water and air samples using headspace gas chromatographic determination of the methyl ester.

    Science.gov (United States)

    Zehavi, D; Seiber, J N

    1996-10-01

    An analytical method has been developed for the determination of trace levels of trifluoroacetic acid (TFA), an atmospheric breakdown product of several of the hydrofluorocarbon (HFC) and hydrochlorofluorocarbon (HCFC) replacements for the chlorofluorocarbon (CFC) refrigerants, in water and air. TFA is derivatized to the volatile methyl trifluoroacetate (MTFA) and determined by automated headspace gas chromatography (HSGC) with electron-capture detection or manual HSGC using GC/MS in the selected ion monitoring (SIM) mode. The method is based on the reaction of an aqueous sample containing TFA with dimethyl sulfate (DMS) in concentrated sulfuric acid in a sealed headspace vial under conditions favoring distribution of MTFA to the vapor phase. Water samples are prepared by evaporative concentration, during which TFA is retained as the anion, followed by extraction with diethyl ether of the acidified sample and then back-extraction of TFA (as the anion) in aqueous bicarbonate solution. The extraction step is required for samples with a relatively high background of other salts and organic materials. Air samples are collected in sodium bicarbonate-glycerin-coated glass denuder tubes and prepared by rinsing the denuder contents with water to form an aqueous sample for derivatization and analysis. Recoveries of TFA from spiked water, with and without evaporative concentration, and from spiked air were quantitative, with estimated detection limits of 10 ng/mL (unconcentrated) and 25 pg/mL (concentrated 250 mL:1 mL) for water and 1 ng/m(3) (72 h at 5 L/min) for air. Several environmental air, fogwater, rainwater, and surface water samples were successfully analyzed; many showed the presence of TFA.

  3. 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...

  4. Air and Surface Sampling Method for Assessing Exposures to Quaternary Ammonium Compounds Using Liquid Chromatography Tandem Mass Spectrometry.

    Science.gov (United States)

    LeBouf, Ryan F; Virji, Mohammed Abbas; Ranpara, Anand; Stefaniak, Aleksandr B

    2017-07-01

    This method was designed for sampling select quaternary ammonium (quat) compounds in air or on surfaces followed by analysis using ultraperformance liquid chromatography tandem mass spectrometry. Target quats were benzethonium chloride, didecyldimethylammonium bromide, benzyldimethyldodecylammonium chloride, benzyldimethyltetradecylammonium chloride, and benzyldimethylhexadecylammonium chloride. For air sampling, polytetrafluoroethylene (PTFE) filters are recommended for 15-min to 24-hour sampling. For surface sampling, Pro-wipe® 880 (PW) media was chosen. Samples were extracted in 60:40 acetonitrile:0.1% formic acid for 1 hour on an orbital shaker. Method detection limits range from 0.3 to 2 ng/ml depending on media and analyte. Matrix effects of media are minimized through the use of multiple reaction monitoring versus selected ion recording. Upper confidence limits on accuracy meet the National Institute for Occupational Safety and Health 25% criterion for PTFE and PW media for all analytes. Using PTFE and PW analyzed with multiple reaction monitoring, the method quantifies levels among the different quats compounds with high precision (detection limits to capture quats on air sampling filters with only a 15-min sample duration with a maximum assessed storage time of 103 days before sample extraction. This method will support future exposure assessment and quantitative epidemiologic studies to explore exposure-response relationships and establish levels of quats exposures associated with adverse health effects. © The Author 2017. Published by Oxford University Press on behalf of the British Occupational Hygiene Society.

  5. Composite Sampling Approaches for Bacillus anthracis Surrogate Extracted from Soil.

    Directory of Open Access Journals (Sweden)

    Brian France

    Full Text Available Any release of anthrax spores in the U.S. would require action to decontaminate the site and restore its use and operations as rapidly as possible. The remediation activity would require environmental sampling, both initially to determine the extent of contamination (hazard mapping and post-decon to determine that the site is free of contamination (clearance sampling. Whether the spore contamination is within a building or outdoors, collecting and analyzing what could be thousands of samples can become the factor that limits the pace of restoring operations. To address this sampling and analysis bottleneck and decrease the time needed to recover from an anthrax contamination event, this study investigates the use of composite sampling. Pooling or compositing of samples is an established technique to reduce the number of analyses required, and its use for anthrax spore sampling has recently been investigated. However, use of composite sampling in an anthrax spore remediation event will require well-documented and accepted methods. In particular, previous composite sampling studies have focused on sampling from hard surfaces; data on soil sampling are required to extend the procedure to outdoor use. Further, we must consider whether combining liquid samples, thus increasing the volume, lowers the sensitivity of detection and produces false negatives. In this study, methods to composite bacterial spore samples from soil are demonstrated. B. subtilis spore suspensions were used as a surrogate for anthrax spores. Two soils (Arizona Test Dust and sterilized potting soil were contaminated and spore recovery with composites was shown to match individual sample performance. Results show that dilution can be overcome by concentrating bacterial spores using standard filtration methods. This study shows that composite sampling can be a viable method of pooling samples to reduce the number of analysis that must be performed during anthrax spore remediation.

  6. Amines as extracting agents for the quantitative determinations of actinides in biological samples

    International Nuclear Information System (INIS)

    Singh, N.P.

    1987-01-01

    The use of amines (primary, secondary and tertiary chains and quaternary ammonium salts) as extracting agents for the quantitative determination of actinides in biological samples is reviewed. Among the primary amines, only Primene JM-T is used to determine Pu in urine and bone. No one has investigated the possibility of using secondary amines to quantitatively extract actinides from biological samples. Among the tertiary amines, tri-n-octylamine, tri-iso-octylamine, tyricaprylamine (Alamine) and trilaurylamine (tridodecylamine) are used extensively to extract and separate the actinides from biological samples. Only one quaternary ammonium salt, methyltricapryl ammonium chloride (Aliquat-336), is used to extract Pu from biological samples. (author) 28 refs

  7. Continuous air monitor correlation to fixed air sample data at Los Alamos National Laboratory

    International Nuclear Information System (INIS)

    Whicker, J.J.

    1993-01-01

    Continuous air monitoring instruments (CAMS) deployed in laboratories in the TA-55 plutonium facility at Los Alamos National Laboratory (LANL) alarmed less than 33 percent of the time when fixed air sample measurements in the same laboratory showed integrated concentrations exceeding 500 DAC-hrs. The purpose of this study was to explore effects of non-instrument variables on alarm sensitivities for properly working CAMS. Non-instrument variables include air flow patterns, particle size of released material, and the energy of the release. Dilution Factors (DFs) for 21 airborne releases in various rooms and of different magnitudes were calculated and compared. The median DF for releases where the CAM alarmed was 13.1 while the median DF for releases where the CAM did not alarm was 179. Particle sizes ranged considerably with many particles larger than 10 μm. The cause of the release was found to be important in predicting if a CAM would alarm with releases from bagouts resulting in the greatest percentage of CAM alarms. The results of this study suggest that a two-component strategy for CAM placement at LANL be utilized. The first component would require CAMs at exhaust points in the rooms to provide for reliable detection for random release locations. The second component would require placing CAMs at locations where releases have historically been seen. Finally, improvements in CAM instrumentation is needed

  8. Strontium-90 determination in air dust filter using solid phase extraction after the accident of FD-NPS

    International Nuclear Information System (INIS)

    Zhang, Zijian; Kakitani, Shunsuke; Ninomiya, Kazuhiko

    2013-01-01

    Radioactivities of Sr-90 in air-dust filters collected in Hitachi, Kawasaki and Toyonaka were determined using solid state extraction method and low background beta-ray counting system. In Hitachi, though the Sr-90 activity concentration was decreased with time, the activity rates of Sr-90/Cs-137 kept about 10"-"3 order. This fact suggests that Sr-90 transportation behavior in the atmosphere is similar to that of Cs-137 during the time of sample collection. (author)

  9. 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.

  10. Green Remediation Best Management Practices: Soil Vapor Extraction & Air Sparging

    Science.gov (United States)

    Historically, approximately one-quarter of Superfund source control projects have involved soil vapor extraction (SVE) to remove volatile organic compounds (VOCs) sorbed to soil in the unsaturated (vadose) zone.

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

    Directory of Open Access Journals (Sweden)

    Z. Wang

    2010-10-01

    Full Text Available We present a new analysis technique for stable isotope ratios (δ13C and δ18O of atmospheric carbon monoxide (CO from ice core samples. The technique is an online cryogenic vacuum extraction followed by continuous-flow isotope ratio mass spectrometry (CF-IRMS; it can also be used with small air samples. 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, gas chromatography purification, and subsequent injection into a Finnigan Delta Plus IRMS. Analytical precision of 0.2‰ (±1δ for δ13C and 0.6‰ (±1δ for δ18O can be obtained for 100 mL (STP air samples with CO mixing ratios ranging from 60 ppbv to 140 ppbv (~268–625 pmol CO. Six South Pole ice core samples from depths ranging from 133 m to 177 m were processed for CO isotope analysis after wet extraction. To our knowledge, this is the first measurement of stable isotopes of CO in ice core air.

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

    International Nuclear Information System (INIS)

    Gfrerer, M.; Lankmayr, E.

    2002-01-01

    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)

  13. Glyphosate–rich air samples induce IL–33, TSLP and generate IL–13 dependent airway inflammation

    Science.gov (United States)

    Kumar, Sudhir; Khodoun, Marat; Kettleson, Eric M.; McKnight, Christopher; Reponen, Tiina; Grinshpun, Sergey A.; Adhikari, Atin

    2014-01-01

    Several low weight molecules have often been implicated in the induction of occupational asthma. Glyphosate, a small molecule herbicide, is widely used in the world. There is a controversy regarding a role of glyphosate in developing asthma and rhinitis among farmers, the mechanism of which is unexplored. The aim of this study was to explore the mechanisms of glyphosate induced pulmonary pathology by utilizing murine models and real environmental samples. C57BL/6, TLR4−/−, and IL-13−/− mice inhaled extracts of glyphosate-rich air samples collected on farms during spraying of herbicides or inhaled different doses of glyphosate and ovalbumin. The cellular response, humoral response, and lung function of exposed mice were evaluated. Exposure to glyphosate-rich air samples as well as glyphosate alone to the lungs increased: eosinophil and neutrophil counts, mast cell degranulation, and production of IL-33, TSLP, IL-13, and IL-5. In contrast, in vivo systemic IL-4 production was not increased. Co-administration of ovalbumin with glyphosate did not substantially change the inflammatory immune response. However, IL-13-deficiency resulted in diminished inflammatory response but did not have a significant effect on airway resistance upon methacholine challenge after 7 or 21 days of glyphosate exposure. Glyphosate-rich farm air samples as well as glyphosate alone were found to induce pulmonary IL-13-dependent inflammation and promote Th2 type cytokines, but not IL-4 for glyphosate alone. This study, for the first time, provides evidence for the mechanism of glyphosate-induced occupational lung disease. PMID:25172162

  14. Air pollution impacts due to petroleum extraction in the Norwegian Sea during the ACCESS aircraft campaign

    NARCIS (Netherlands)

    Tuccella, P.; Thomas, J.L.; Law, K.S.; Raut, J.C.; Marelle, L.; Roiger, A.; Weinzierl, B.; Denier Van Der Gon, H.A.C.; Schlager, H.; Onishi, T.

    2017-01-01

    Emissions from oil/gas extraction activities in the Arctic are already important in certain regions and may increase as global warming opens up new opportunities for industrial development. Emissions from oil/gas extraction are sources of air pollutants, but large uncertainties exist with regard to

  15. Minimizing the water and air impacts of unconventional energy extraction

    Science.gov (United States)

    Jackson, R. B.

    2014-12-01

    Unconventional energy generates income and, done well, can reduce air pollution compared to other fossil fuels and even water use compared to fossil fuels and nuclear energy. Alternatively, it could slow the adoption of renewables and, done poorly, release toxic chemicals into water and air. Based on research to date, some primary threats to water resources come from surface spills, wastewater disposal, and drinking-water contamination through poor well integrity. For air resources, an increase in volatile organic compounds and air toxics locally is a potential health threat, but the switch from coal to natural gas for electricity generation will reduce sulfur, nitrogen, mercury, and particulate pollution regionally. Critical needs for future research include data for 1) estimated ultimate recovery (EUR) of unconventional hydrocarbons; 2) the potential for further reductions of water requirements and chemical toxicity; 3) whether unconventional resource development alters the frequency of well-integrity failures; 4) potential contamination of surface and ground waters from drilling and spills; and 5) the consequences of greenhouse gases and air pollution on ecosystems and human health.

  16. Fabrication and characterization of buckypapers for use in air sampling

    Science.gov (United States)

    Oh, Jonghwa

    Occupational exposure to volatile organic compounds (VOCs) is a concern from a public health perspective. In many industrial activities, workers' exposure to VOCs can be sufficiently high to induce adverse health effects, so their monitoring is necessary. In exposure assessment, post sampling extraction and quantification are the typical analytical procedures. Recently, our group developed the photothermal desorption (PTD) technique in which a pulse of light thermally desorbs an analyte directly from a sorbent. Advantages of this technique are; it is solvent free, repeated analysis is possible, sorbents are reusable, and no high cost of equipment is required. PTD overcomes almost all drawbacks of current extraction methods. This study was aimed to develop and test a new sorbent which will efficiently work with PTD. Single-walled carbon nanotubes (SWNTs) were examined as potential sorbents because of their high surface area, great thermal conductivity, and efficient light absorption. SWNTs were fabricated into a self-supporting form (i.e., buckypaper (BP)) which will preserve its physical integrity under normal working conditions. Largely two types of SWNTs were used, arc discharge (AD) and high-pressure carbon monoxide (HiPco), and different fabrication methods were examined. Upon fabrication, their adsorption properties were characterized in terms of Brunauer, Emmett, and Teller (BET) surface area, pore size, and toluene adsorption capacity. HiPco BP and methanol-cleaned AD BP (suspended/rinsed with methanol) were the top two materials, showing the highest surface area (649 and 387 m²/g, respectively) and adsorption capacity (106 and 46 mg/g, respectively) with relatively small mean pore diameter (7.7 and 8.8 nm, respectively). To further improve the adsorption properties, specific heat treatment conditions for each type of BPs were employed. After initial treatments only HiPco BP and acetone-cleaned AD BP (suspended/rinsed with acetone) were selected for further

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

    International Nuclear Information System (INIS)

    Acena, M.L.; Crespo, M.T.

    1989-01-01

    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)

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

    NARCIS (Netherlands)

    Henneken, H.

    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

  19. 46 CFR 161.002-15 - Sample extraction smoke detection systems.

    Science.gov (United States)

    2010-10-01

    ... 46 Shipping 6 2010-10-01 2010-10-01 false Sample extraction smoke detection systems. 161.002-15..., CONSTRUCTION, AND MATERIALS: SPECIFICATIONS AND APPROVAL ELECTRICAL EQUIPMENT Fire-Protective Systems § 161.002-15 Sample extraction smoke detection systems. The smoke detecting system must consist of a means for...

  20. Stratospheric Air Sub-sampler (SAS) and its application to analysis of Delta O-17(CO2) from small air samples collected with an AirCore

    NARCIS (Netherlands)

    Mrozek, Dorota Janina; van der Veen, Carina; Hofmann, Magdalena E. G.; Chen, Huilin; Kivi, Rigel; Heikkinen, Pauli; Rockmann, Thomas

    2016-01-01

    We present the set-up and a scientific application of the Stratospheric Air Sub-sampler (SAS), a device to collect and to store the vertical profile of air collected with an AirCore (Karion et al., 2010) in numerous sub-samples for later analysis in the laboratory. The SAS described here is a 20m

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

    Science.gov (United States)

    Kaya, Merve; Sousa, António G.; Crépeau, Marie-Jeanne; Sørensen, 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 plant source (orange, lemon, lime, grapefruit) and considers the influence of extraction conditions on 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 extraction) and on a laboratory scale (grams; mild oxalic acid extraction). Pectin composition (acidic and neutral sugars) and physicochemical properties (molar mass and intrinsic viscosity) were determined. Key Results Oxalic acid extraction allowed the recovery of pectin samples of high molecular weight. Mild oxalic acid-extracted pectins were rich in long homogalacturonan stretches and contained rhamnogalacturonan I stretches with conserved side chains. Nitric acid-extracted pectins exhibited lower molecular weights and contained rhamnogalacturonan I stretches encompassing few and/or short side chains. Grapefruit pectin was found to have short side chains compared with orange, lime and lemon. Orange and grapefruit pectin samples were both particularly rich in rhamnogalacturonan I backbones. Conclusions Structural, and hence macromolecular, variations within the different citrus pectin samples were mainly related to their rhamnogalacturonan I contents and integrity, and, to a lesser extent, to the length of their homogalacturonan domains. PMID:25081519

  2. 30 CFR 90.205 - Approved sampling devices; operation; air flowrate.

    Science.gov (United States)

    2010-07-01

    ... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Approved sampling devices; operation; air... LABOR COAL MINE SAFETY AND HEALTH MANDATORY HEALTH STANDARDS-COAL MINERS WHO HAVE EVIDENCE OF THE DEVELOPMENT OF PNEUMOCONIOSIS Sampling Procedures § 90.205 Approved sampling devices; operation; air flowrate...

  3. 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

    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...

  4. The application of extraction chromatography to the determination of radionuclides in biological and environmental samples

    International Nuclear Information System (INIS)

    Testa, C.; Delle Site, A.

    1976-01-01

    The paper describe the application of extraction chromatography to the determination of several alpha and beta emitters in biological and environmental samples. Both column extraction chromatography and batch extraction process have been used to isolate the radionuclides from the samples. The effect of several parameters (extractant concentration, support granulometry, stirring time, temperature, presence of a complexing agent) on the extraction and elution has been examined. The application of redox extraction chromatography is also described. A very simple and rapid determination of the activity retained on the column can be obtained by transferring the slurry to a counting vial and by adding the scintillation liquid for a direct detection of the α or β emission. The counting efficiencies obtained with this technique are compared with those obtained with ion exchange resins. The organic polymers used for the extraction chromatography give about 100% counting efficiency. The conventional ion exchange resin cannot be used to this purpose because of their strong light absorption. (T.G.)

  5. Determination of biomass burning tracers in air samples by GC/MS

    Directory of Open Access Journals (Sweden)

    Janoszka Katarzyna

    2018-01-01

    Full Text Available Levoglucosan (LG as a main cellulose burning product at 300°C is a biomass burning tracer. LG characterize by relatively high molar mass and it is sorbed by particulate matter. In the study of air pollution monitoring LG is mainly analyzed in particulate matter, PM1 and PM2,5. The tracer create relatively high O-H…O bond and weaker C-H…O bond. Due to the hydrogen bond, LG dissolves very well in water. Analytical procedure of LG determination include: extraction, derivatization and analysis by gas chromatography coupled with mass spectrometry detector. In water samples levoglucosan is determined by liquid chromatography. The paper presents a methodology for particulate matter samples determination their analysis by gas chromatography coupled with a mass spectrometry detector. Determination of LG content in particulate matter was performed according to an analytical method based on simultaneous pyridine extraction and derivatization using N,O-bis (trimethylsilyl trifluoroacetamide and trimethylchlorosilane mixture (BSTFA: TMCS, 99: 1.

  6. Determination of biomass burning tracers in air samples by GC/MS

    Science.gov (United States)

    Janoszka, Katarzyna

    2018-01-01

    Levoglucosan (LG) as a main cellulose burning product at 300°C is a biomass burning tracer. LG characterize by relatively high molar mass and it is sorbed by particulate matter. In the study of air pollution monitoring LG is mainly analyzed in particulate matter, PM1 and PM2,5. The tracer create relatively high O-H…O bond and weaker C-H…O bond. Due to the hydrogen bond, LG dissolves very well in water. Analytical procedure of LG determination include: extraction, derivatization and analysis by gas chromatography coupled with mass spectrometry detector. In water samples levoglucosan is determined by liquid chromatography. The paper presents a methodology for particulate matter samples determination their analysis by gas chromatography coupled with a mass spectrometry detector. Determination of LG content in particulate matter was performed according to an analytical method based on simultaneous pyridine extraction and derivatization using N,O-bis (trimethylsilyl) trifluoroacetamide and trimethylchlorosilane mixture (BSTFA: TMCS, 99: 1).

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

    Science.gov (United States)

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

    2002-10-01

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

  8. Evaluation of Legionella Air Contamination in Healthcare Facilities by Different Sampling Methods: An Italian Multicenter Study

    Science.gov (United States)

    Montagna, Maria Teresa; De Giglio, Osvalda; Cristina, Maria Luisa; Napoli, Christian; Pacifico, Claudia; Agodi, Antonella; Baldovin, Tatjana; Casini, Beatrice; Coniglio, Maria Anna; D’Errico, Marcello Mario; Delia, Santi Antonino; Deriu, Maria Grazia; Guida, Marco; Laganà, Pasqualina; Liguori, Giorgio; Moro, Matteo; Mura, Ida; Pennino, Francesca; Privitera, Gaetano; Romano Spica, Vincenzo; Sembeni, Silvia; Spagnolo, Anna Maria; Tardivo, Stefano; Torre, Ida; Valeriani, Federica; Albertini, Roberto; Pasquarella, Cesira

    2017-01-01

    Healthcare facilities (HF) represent an at-risk environment for legionellosis transmission occurring after inhalation of contaminated aerosols. In general, the control of water is preferred to that of air because, to date, there are no standardized sampling protocols. Legionella air contamination was investigated in the bathrooms of 11 HF by active sampling (Surface Air System and Coriolis®μ) and passive sampling using settling plates. During the 8-hour sampling, hot tap water was sampled three times. All air samples were evaluated using culture-based methods, whereas liquid samples collected using the Coriolis®μ were also analyzed by real-time PCR. Legionella presence in the air and water was then compared by sequence-based typing (SBT) methods. Air contamination was found in four HF (36.4%) by at least one of the culturable methods. The culturable investigation by Coriolis®μ did not yield Legionella in any enrolled HF. However, molecular investigation using Coriolis®μ resulted in eight HF testing positive for Legionella in the air. Comparison of Legionella air and water contamination indicated that Legionella water concentration could be predictive of its presence in the air. Furthermore, a molecular study of 12 L. pneumophila strains confirmed a match between the Legionella strains from air and water samples by SBT for three out of four HF that tested positive for Legionella by at least one of the culturable methods. Overall, our study shows that Legionella air detection cannot replace water sampling because the absence of microorganisms from the air does not necessarily represent their absence from water; nevertheless, air sampling may provide useful information for risk assessment. The liquid impingement technique appears to have the greatest capacity for collecting airborne Legionella if combined with molecular investigations. PMID:28640202

  9. Evaluation of Legionella Air Contamination in Healthcare Facilities by Different Sampling Methods: An Italian Multicenter Study.

    Science.gov (United States)

    Montagna, Maria Teresa; De Giglio, Osvalda; Cristina, Maria Luisa; Napoli, Christian; Pacifico, Claudia; Agodi, Antonella; Baldovin, Tatjana; Casini, Beatrice; Coniglio, Maria Anna; D'Errico, Marcello Mario; Delia, Santi Antonino; Deriu, Maria Grazia; Guida, Marco; Laganà, Pasqualina; Liguori, Giorgio; Moro, Matteo; Mura, Ida; Pennino, Francesca; Privitera, Gaetano; Romano Spica, Vincenzo; Sembeni, Silvia; Spagnolo, Anna Maria; Tardivo, Stefano; Torre, Ida; Valeriani, Federica; Albertini, Roberto; Pasquarella, Cesira

    2017-06-22

    Healthcare facilities (HF) represent an at-risk environment for legionellosis transmission occurring after inhalation of contaminated aerosols. In general, the control of water is preferred to that of air because, to date, there are no standardized sampling protocols. Legionella air contamination was investigated in the bathrooms of 11 HF by active sampling (Surface Air System and Coriolis ® μ) and passive sampling using settling plates. During the 8-hour sampling, hot tap water was sampled three times. All air samples were evaluated using culture-based methods, whereas liquid samples collected using the Coriolis ® μ were also analyzed by real-time PCR. Legionella presence in the air and water was then compared by sequence-based typing (SBT) methods. Air contamination was found in four HF (36.4%) by at least one of the culturable methods. The culturable investigation by Coriolis ® μ did not yield Legionella in any enrolled HF. However, molecular investigation using Coriolis ® μ resulted in eight HF testing positive for Legionella in the air. Comparison of Legionella air and water contamination indicated that Legionella water concentration could be predictive of its presence in the air. Furthermore, a molecular study of 12 L. pneumophila strains confirmed a match between the Legionella strains from air and water samples by SBT for three out of four HF that tested positive for Legionella by at least one of the culturable methods. Overall, our study shows that Legionella air detection cannot replace water sampling because the absence of microorganisms from the air does not necessarily represent their absence from water; nevertheless, air sampling may provide useful information for risk assessment. The liquid impingement technique appears to have the greatest capacity for collecting airborne Legionella if combined with molecular investigations.

  10. Aluminium, extractable from soil samples by the acid ammonium acetate soil-testing method

    Directory of Open Access Journals (Sweden)

    Osmo Mäkitie

    1968-05-01

    Full Text Available The extractant, 0.5 M acetic acid –0.5 M ammonium acetate at pH 4.65, which is used in soil-testing, extracts relatively high amounts of aluminium from acid soils. The mean values of acetate-extractable aluminium at pH 4.65, 1.75 meq Al/100 g of soil, and of exchangeable aluminium (M KCI extraction, 0.41 meq Al were obtained from a material of 30 samples of acid soils (Table 2. Several other acetic acid ammonium acetate extractants, from M acetic acid to M ammonium acetate solution were also used for studying the extractability of soil aluminium. The soil-testing extractant can be used for the estimation of the soluble amounts of aluminium in acid soils, however, further studies are needed for a better interpretation of the ammonium acetate extractable (at pH 4.65 aluminium in our soils.

  11. Molecular Biological Characterization of Air Samples: A Survey of Four Strategically Important Regions

    National Research Council Canada - National Science Library

    Francesconi, Stephen

    2003-01-01

    .... In support of this requirement, the Joint Program Office for Biological Defense initiated an aggressive program incorporating the development of air-sampling and agent detecting devices, coined...

  12. Studies on plant extracts as corrosion inhibitors for mild steel in air saturated water

    International Nuclear Information System (INIS)

    Mohamad Daud; Abdul Razak Daud; Zainal Abidin Sidi

    1988-01-01

    The effectiveness in inhibiting corrosion by garlic, soya bean, and tobacco extracts and their combinations in air saturated water at ambient temperature were studied by using electrochemical corrosion test. The range of inhibitor concentration studied was from 0.1 to 1.0 g/l. The variations of corrosion potential and corrosion current density was recorded and the results showed that the extracts have inhibitive properties in the corrosion of mild stee. The effectiveness of the inhibitors is in the following order: extract mixture > tobacco > garlic > soya bean extracts. (author)

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

    Science.gov (United States)

    2010-07-01

    ... ADMINISTRATION AIR FORCE FREEDOM OF INFORMATION ACT PROGRAM § 806.27 Samples of Air Force FOIA processing... determination within 20 workdays, we have instituted multitrack processing of requests. Based on the information... source; responsive records were part of the Air Force's decision-making process, and the prerelease...

  14. Extraction, Scrub, and Strip Test Results for the Salt Waste Processing Facility Caustic Side Solvent Extraction Solvent Sample

    Energy Technology Data Exchange (ETDEWEB)

    Peters, T. B. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2017-10-06

    An Extraction, Scrub, and Strip (ESS) test was performed on a sample of Salt Waste Processing Facility (SWPF) Caustic-Side Solvent Extraction (CSSX) solvent and salt simulant to determine cesium distribution ratios (D(Cs)), and cesium concentration in the strip effluent (SE) and decontaminated salt solution (DSS) streams; this data will be used by Parsons to help determine if the solvent is qualified for use at the SWPF. The ESS test showed acceptable performance of the solvent for extraction, scrub, and strip operations. The extraction D(Cs) measured 12.5, exceeding the required value of 8. This value is consistent with results from previous ESS tests using similar solvent formulations. Similarly, scrub and strip cesium distribution ratios fell within acceptable ranges. This revision was created to correct an error. The previous revision used an incorrect set of temperature correction coefficients which resulted in slight deviations from the correct D(Cs) results.

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

    Science.gov (United States)

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

    2017-01-15

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

  16. Development of activated charcoal impregnated air sampling filter media : their characteristics and use

    International Nuclear Information System (INIS)

    Khan, A.A.; Ramarathinam, K.; Gupta, S.K.; Deshingkar, D.S.; Kishore, A.G.

    1975-01-01

    Because of its low maximum permissible concentration in air, air-borne radioiodine must be accurately monitored in contaminated air streams, in the working environment and handling facilities, before release to the environment from the nuclear facilities. Activated charcoal impregnated air sampling filter media are found to be most suitable for monitoring airborne iodine-131. Because of its simplicity and reproducible nature in assessment of air-borne radioactive iodine, the work on the development of such media was undertaken in order to find a suitable substitute for imported activated charcoal impregnated air sampling filter media. Eight different media of such type were developed, evaluated and compared with two imported media. Best suitable medium is recommended for its use in air-borne iodine sampling which was found to be even better suited than imported media of such type. (author)

  17. Early detection of sugar beet pathogen Ramularia beticola in leaf and air samples using qPCR

    DEFF Research Database (Denmark)

    Wieczorek, Thies Marten; Jørgensen, Lise Nistrup; Hansen, Anne Lisbet

    2014-01-01

    A quantitative PCR method (qPCR) was developed for the detection and quantification of Ramularia beticola causing Ramularia leaf spot in sugar beet. R. beticola specific primers were designed based on the internal transcribed spacer region 2 (ITS2). The assay was applied on DNA extracted from...... spores trapped on tape from Burkard spore traps placed in an artificially inoculated sugar beet field trial and in two sugar beet fields with natural infections. R. beticola DNA was detected at variable amounts in the air samples 14 to 16 days prior to first visible symptoms. R. beticola DNA was detected...... in air samples from fields with natural infection at significant and increasing levels from development of the first symptoms, indicating that spore production within the crop plays a major role in the epidemic development of the disease. Sugar beet leaves sampled from the inoculated field trial were...

  18. Soil sampling and extraction methods with possible application to pear thrips (Thysanoptera: Thripidae)

    Science.gov (United States)

    John E. Bater

    1991-01-01

    Techniques are described for the sampling and extraction of microarthropods from soil and the potential of these methods to extract the larval stages of the pear thrips, Taeniothrips inconsequens (Uzel), from soil cores taken in sugar maple stands. Also described is a design for an emergence trap that could be used to estimate adult thrips...

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

    International Nuclear Information System (INIS)

    Hackworth, M.F.

    1995-01-01

    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

  20. Air bubbles and hemolysis of blood samples during transport by pneumatic tube systems.

    Science.gov (United States)

    Mullins, Garrett R; Bruns, David E

    2017-10-01

    Transport of blood samples through pneumatic tube systems (PTSs) generates air bubbles in transported blood samples and, with increasing duration of transport, the appearance of hemolysis. We investigated the role of air-bubble formation in PTS-induced hemolysis. Air was introduced into blood samples for 0, 1, 3 or 5min to form air bubbles. Hemolysis in the blood was assessed by (H)-index, lactate dehydrogenase (LD) and potassium in plasma. In an effort to prevent PTS-induced hemolysis, blood sample tubes were completely filled, to prevent air bubble formation, and compared with partially filled samples after PTS transport. We also compared hemolysis in anticoagulated vs clotted blood subjected to PTS transport. As with transport through PTSs, the duration of air bubble formation in blood by a gentle stream of air predicted the extent of hemolysis as measured by H-index (pair space in a blood sample prevented bubble formation and fully protected the blood from PTS-induced hemolysis (ptransport and was partially protected from hemolysis vs anticoagulated blood as indicated by lower LD (ptransport. Prevention of air bubble formation in blood samples during PTS transport protects samples from hemolysis. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

    Iswantoro; Sutanto, W.W

    2013-01-01

    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)

  2. 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. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Efficient discrimination and removal of phospholipids during electromembrane extraction from human plasma samples

    DEFF Research Database (Denmark)

    Vårdal, Linda; Gjelstad, Astrid; Huang, Chuixiu

    2017-01-01

    to be highly efficient for providing phospholipid-free extracts. CONCLUSION: Ultra-HPLC-MS/MS analysis of the donor solutions revealed that the phospholipids principally remained in the plasma samples. This proved that the phospholipids did not migrate in the electrical field and they were prevented from......AIM: For the first time, extracts obtained from human plasma samples by electromembrane extraction (EME) were investigated comprehensively with particular respect to phospholipids using ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). Thhe purpose...

  4. 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

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

    Science.gov (United States)

    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%; RSD: 24%). Comparable results were obtained with an established analysis method for PCBs, OH-PCBs and MeSO2-PCBs. PMID:19019378

  6. Comparison of indoor air sampling and dust collection methods for fungal exposure assessment using quantitative PCR

    Science.gov (United States)

    Evaluating fungal contamination indoors is complicated because of the many different sampling methods utilized. In this study, fungal contamination was evaluated using five sampling methods and four matrices for results. The five sampling methods were a 48 hour indoor air sample ...

  7. Improvement of Aluminum-Air Battery Performances by the Application of Flax Straw Extract.

    Science.gov (United States)

    Grishina, Ekaterina; Gelman, Danny; Belopukhov, Sergey; Starosvetsky, David; Groysman, Alec; Ein-Eli, Yair

    2016-08-23

    The effect of a flax straw extract on Al corrosion inhibition in a strong alkaline solution was studied by using electrochemical measurements, weight-loss analysis, SEM, and FTIR spectroscopy. Flax straw extract added (3 vol %) to the 5 m KOH solution to act as a mixed-type Al corrosion inhibitor. The electrochemistry of Al in the presence of a flax straw extract in the alkaline solution, the effect of the extract on the Al morphology and surface films formed, and the corrosion inhibition mechanism are discussed. Finally, the Al-air battery discharge capacity recorded from a cell that used the flax straw extract in the alkaline electrolyte is substantially higher than that with only a pure alkaline electrolyte. This improved sustainability of the Al anode is attributed to Al corrosion inhibition and, consequently, to hydrogen evolution suppression. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Energy Technology Data Exchange (ETDEWEB)

    Khajeh, Mostafa; Nemch, Tabandeh Karimi [Zabol Univ. (Iran, Islamic Republic of). Dept. of Chemistry

    2014-07-01

    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{sup -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.

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

    International Nuclear Information System (INIS)

    Khajeh, Mostafa; Nemch, Tabandeh Karimi

    2014-01-01

    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.

  10. Extraction of ochratoxin A in bread samples by the QuEChERS methodology.

    Science.gov (United States)

    Paíga, Paula; Morais, Simone; Oliva-Teles, Teresa; Correia, Manuela; Delerue-Matos, Cristina; Duarte, Sofia C; Pena, Angelina; Lino, Celeste Matos

    2012-12-15

    A QuEChERS method for the extraction of ochratoxin A (OTA) from bread samples was evaluated. A factorial design (2(3)) was used to find the optimal QuEChERS parameters (extraction time, extraction solvent volume and sample mass). Extracts were analysed by LC with fluorescence detection. The optimal extraction conditions were: 5 g of sample, 15 mL of acetonitrile and 3 min of agitation. The extraction procedure was validated by systematic recovery experiments at three levels. The recoveries obtained ranged from 94.8% (at 1.0 μg kg(-1)) to 96.6% (at 3.0 μg kg(-1)). The limit of quantification of the method was 0.05 μg kg(-1). The optimised procedure was applied to 20 samples of different bread types ("Carcaça", "Broa de Milho", and "Broa de Avintes") highly consumed in Portugal. None of the samples exceeded the established European legal limit of 3 μg kg(-1). Copyright © 2012 Elsevier Ltd. All rights reserved.

  11. 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°...

  12. 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

  13. 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)

    Hoefler, F.

    2002-01-01

    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)

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

    International Nuclear Information System (INIS)

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

    2013-01-01

    (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 chromium and technetium (i

  15. Permanganate-assisted removal of PCR inhibitors during the DNA Chelex extraction from stained denim samples.

    Science.gov (United States)

    Pîrlea, Sorina; Puiu, Mihaela; Răducan, Adina; Oancea, Dumitru

    2017-03-01

    In this study, it was demonstrated that the DNA Chelex extraction combined with the permanganate assisted-oxidation is highly efficient in removing the PCR inhibitors often found in clothing materials, such as phthalocyanine. The extraction assays were conducted in saliva, blood and epithelial cells samples mixed with three oxidation-resistant dye copper(II) α-phthalocyanine, copper(II) β-phthalocyanine and tetrasulfonated copper(II) β-phthalocyanine. After DNA amplification, all samples were able to provide full DNA profiles. The permanganate/Chelex system was tested further on denim-stained samples and displayed the same ability to remove the PCR inhibitors from the commercial textile materials.

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

    International Nuclear Information System (INIS)

    Qiu Dangui; Li Xinzhi; Hou Jianrong; Qiao Taifei; Wu Tao; Zhang Jirong; Han Lihong

    2012-01-01

    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. Determination of volatile organic hydrocarbons in water samples by solid-phase dynamic extraction.

    Science.gov (United States)

    Jochmann, Maik A; Yuan, Xue; Schmidt, Torsten C

    2007-03-01

    In the present study a headspace solid-phase dynamic extraction method coupled to gas chromatography-mass spectrometry (HS-SPDE-GC/MS) for the trace determination of volatile halogenated hydrocarbons and benzene from groundwater samples was developed and evaluated. As target compounds, benzene as well as 11 chlorinated and brominated hydrocarbons (vinyl chloride, dichloromethane, cis-1,2-dichloroethylene, trans-1,2-dichloroethylene, carbon tetrachloride, chloroform, trichloroethylene, tetrachloroethylene, bromoform) of environmental and toxicological concern were included in this study. The analytes were extracted using a SPDE needle device, coated with a poly(dimethylsiloxane) with 10% embedded activated carbon phase (50-microm film thickness and 56-mm film length) and were analyzed by GC/MS in full-scan mode. Parameters that affect the extraction yield such as extraction and desorption temperature, salting-out, extraction and desorption flow rate, extraction volume and desorption volume, the number of extraction cycles, and the pre-desorption time have been evaluated and optimized. The linearity of the HS-SPDE-GC/MS method was established over several orders of magnitude. Method detection limits (MDLs) for the compounds investigated ranged between 12 ng/L for cis-dichloroethylene and trans-dichloroethylene and 870 ng/L for vinyl chloride. The method was thoroughly validated, and the precision at two concentration levels (0.1 mg/L and a concentration 5 times above the MDL) was between 3.1 and 16% for the analytes investigated. SPDE provides high sensitivity, short sample preparation and extraction times and a high sample throughput because of full automation. Finally, the applicability to real environmental samples is shown exemplarily for various groundwater samples from a former waste-oil recycling facility. Groundwater from the site showed a complex contamination with chlorinated volatile organic compounds and aromatic hydrocarbons.

  18. Determination of volatile organic hydrocarbons in water samples by solid-phase dynamic extraction

    Energy Technology Data Exchange (ETDEWEB)

    Jochmann, Maik A.; Schmidt, Torsten C. [Eberhard-Karls-Universitaet Tuebingen, Center for Applied Geoscience (ZAG), Tuebingen (Germany); Chair of Instrumental Analysis, University Duisburg-Essen, Duisburg (Germany); Yuan, Xue [Eberhard-Karls-Universitaet Tuebingen, Center for Applied Geoscience (ZAG), Tuebingen (Germany)

    2007-03-15

    In the present study a headspace solid-phase dynamic extraction method coupled to gas chromatography-mass spectrometry (HS-SPDE-GC/MS) for the trace determination of volatile halogenated hydrocarbons and benzene from groundwater samples was developed and evaluated. As target compounds, benzene as well as 11 chlorinated and brominated hydrocarbons (vinyl chloride, dichloromethane, cis-1,2-dichloroethylene, trans-1,2-dichloroethylene, carbon tetrachloride, chloroform, trichloroethylene, tetrachloroethylene, bromoform) of environmental and toxicological concern were included in this study. The analytes were extracted using a SPDE needle device, coated with a poly(dimethylsiloxane) with 10% embedded activated carbon phase (50-{mu}m film thickness and 56-mm film length) and were analyzed by GC/MS in full-scan mode. Parameters that affect the extraction yield such as extraction and desorption temperature, salting-out, extraction and desorption flow rate, extraction volume and desorption volume, the number of extraction cycles, and the pre-desorption time have been evaluated and optimized. The linearity of the HS-SPDE-GC/MS method was established over several orders of magnitude. Method detection limits (MDLs) for the compounds investigated ranged between 12 ng/L for cis-dichloroethylene and trans-dichloroethylene and 870 ng/L for vinyl chloride. The method was thoroughly validated, and the precision at two concentration levels (0.1 mg/L and a concentration 5 times above the MDL) was between 3.1 and 16% for the analytes investigated. SPDE provides high sensitivity, short sample preparation and extraction times and a high sample throughput because of full automation. Finally, the applicability to real environmental samples is shown exemplarily for various groundwater samples from a former waste-oil recycling facility. Groundwater from the site showed a complex contamination with chlorinated volatile organic compounds and aromatic hydrocarbons. (orig.)

  19. Air sampling by pumping through a filter: effects of air flow rate, concentration, and decay of airborne substances

    OpenAIRE

    Šoštarić, Marko; Petrinec, Branko; Babić, Dinko

    2016-01-01

    This paper tackles the issue of interpreting the number of airborne particles adsorbed on a filter through which a certain volume of sampled air has been pumped. This number is equal to the product of the pumped volume and particle concentration in air, but only if the concentration is constant over time and if there is no substance decomposition on the filter during sampling. If this is not the case, one must take into account the inconstancy of the concentration and the decay law for a give...

  20. MEASUREMENT OF PYRETHROID RESIDUES IN ENVIRONMENTAL AND FOOD SAMPLES BY ENHANCED SOLVENT EXTRACTION/SUPERCRITICAL FLUID EXTRACTION COUPLED WITH GAS CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

    Science.gov (United States)

    The abstract summarizes pyrethorid methods development research. It provides a summary of sample preparation and analytical techniques such as supercritical fluid extraction, enhance solvent extraction, gas chromatography and tandem mass spectrometry.

  1. 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...

  2. 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.

  3. Comparison of three mycobacterial DNA extraction methods from extrapulmonary samples for PCR assay

    Directory of Open Access Journals (Sweden)

    Khandaker Shadia

    2012-01-01

    Full Text Available Sensitivity of the molecular diagnostic tests of extrapulmonary tuberculosis largely depends upon the efficiency of DNA extraction methods. The objective of our study was to compare three methods of extracting DNA of Mycobacterium tuberculosis for testing by polymerase chain reaction. All three methods; heating, heating with sonication and addition of lysis buffer with heating and sonication were implicated on 20 extrapulmonary samples. PCR positivity was 2 (10%, 4 (20% and 7 (35% in the samples extracted by heating, heat+sonication and heat+sonication+lysis buffer method respectively. Of the extraction methods evaluated, maximum PCR positive results were achieved by combined heat, sonication and lysis buffer method which can be applied in routine clinical practice. Ibrahim Med. Coll. J. 2012; 6(1: 9-11

  4. 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

  5. Gas-chromatographic quantitative determination of argon in air samples, by elimination of oxigen

    International Nuclear Information System (INIS)

    Sofronie, E.

    1982-08-01

    A method of gas-chromatographic quantitative determination of argon in air samples, by elimination of oxygen, is presented. Experiments were carried out in a static system. Conditions for the application of the method in dynamic systems are specified. Sensibility of the method: 5 10 -4 cm 3 Ar per cm 3 of air. (author)

  6. Mixed species radioiodine air sampling readout and dose assessment system

    International Nuclear Information System (INIS)

    Distenfeld, C.H.; Klemish, J.R. Jr.

    1978-01-01

    This invention provides a simple, reliable, inexpensive and portable means and method for determining the thyroid dose rate of mixed airborne species of solid and gaseous radioiodine without requiring highly skilled personnel, such as health physicists or electronics technicians. To this end, this invention provides a means and method for sampling a gas from a source of a mixed species of solid and gaseous radioiodine for collection of the mixed species and readout and assessment of the emissions therefrom by cylindrically, concentrically and annularly molding the respective species around a cylindrical passage for receiving a conventional probe-type Geiger-Mueller radiation detector

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

    International Nuclear Information System (INIS)

    Garcia-Ayuso, L.E.; Luque de Castro, M.D.; Velasco, J.; Dobarganes, M.C.

    1999-01-01

    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

  8. 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...

  9. Application of a 2D air flow model to soil vapor extraction and bioventing case studies

    International Nuclear Information System (INIS)

    Mohr, D.H.; Merz, P.H.

    1995-01-01

    Soil vapor extraction (SVE) is frequently the technology of choice to clean up hydrocarbon contamination in unsaturated soil. A two-dimensional air flow model provides a practical tool to evaluate pilot test data and estimate remediation rates for soil vapor extraction systems. The model predictions of soil vacuum versus distance are statistically compared to pilot test data for 65 SVE wells at 44 sites. For 17 of 21 sites where there was asphalt paving, the best agreement was obtained for boundary conditions with no barrier to air flow at the surface. The model predictions of air flow rates and stream lines around the well allow an estimate of the gasoline removal rates by both evaporation and bioremediation. The model can be used to quickly estimate the effective radius of influence, defined here as the maximum distance from the well where there is enough air flow to remove the contaminant present within the allowable time. The effective radius of influence is smaller than a radius of influence defined by soil vacuum only. For a case study, in situ bioremediation rates were estimated using the air flow model and compared to independent estimates based on changes in soil temperature. These estimate bioremediation rates for heavy fuel oil ranged from 2.5 to 11 mg oil degraded per kg soil per day, in agreement with values in the literature

  10. Microwave-assisted extraction of metal elements from glass fibrous filters for aerosol sampling

    International Nuclear Information System (INIS)

    Li Dong-Mei; Zhang Li-Xing; Wang Xu-Hui; Liu Long-Bo

    2003-01-01

    Atmospheric aerosols are generally collected on filters according to the International Monitoring System (IMS) designed in the Comprehensive Nuclear-Test-Ban Treaty (CTBT). More information could be revealed when the filter sample is pretreated rather than measured directly by γ-ray spectrometer. Microwave-assisted extraction (MAE) is a suitable method that gives higher recoveries of elements from glass fibrous filters under different conditions. The results indicate that the MAE is a highly efficient and robust method for the treatment of glass fibrous filter samples. The recoveries of potential fission products from glass fibrous filter samples by microwave-assisted extraction meet the efficiency of the extraction by both aqua regia and 2% HCl. (author)

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

    International Nuclear Information System (INIS)

    Alloni, L.; Venturelli, A.; Meloni, S.

    1990-01-01

    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.)

  12. The NYC native air sampling pilot project: using HVAC filter data for urban biological incident characterization.

    Science.gov (United States)

    Ackelsberg, Joel; Leykam, Frederic M; Hazi, Yair; Madsen, Larry C; West, Todd H; Faltesek, Anthony; Henderson, Gavin D; Henderson, Christopher L; Leighton, Terrance

    2011-09-01

    Native air sampling (NAS) is distinguished from dedicated air sampling (DAS) devices (eg, BioWatch) that are deployed to detect aerosol disseminations of biological threat agents. NAS uses filter samples from heating, ventilation, and air conditioning (HVAC) systems in commercial properties for environmental sampling after DAS detection of biological threat agent incidents. It represents an untapped, scientifically sound, efficient, widely distributed, and comparably inexpensive resource for postevent environmental sampling. Calculations predict that postevent NAS would be more efficient than environmental surface sampling by orders of magnitude. HVAC filter samples could be collected from pre-identified surrounding NAS facilities to corroborate the DAS alarm and delineate the path taken by the bioaerosol plume. The New York City (NYC) Native Air Sampling Pilot Project explored whether native air sampling would be acceptable to private sector stakeholders and could be implemented successfully in NYC. Building trade associations facilitated outreach to and discussions with property owners and managers, who expedited contact with building managers of candidate NAS properties that they managed or owned. Nominal NAS building requirements were determined; procedures to identify and evaluate candidate NAS facilities were developed; data collection tools and other resources were designed and used to expedite candidate NAS building selection and evaluation in Manhattan; and exemplar environmental sampling playbooks for emergency responders were completed. In this sample, modern buildings with single or few corporate tenants were the best NAS candidate facilities. The Pilot Project successfully demonstrated that in one urban setting a native air sampling strategy could be implemented with effective public-private collaboration.

  13. Direct Trace Element Analysis of Liquid Blood Samples by In-Air Ion Beam Analytical Techniques (PIXE-PIGE).

    Science.gov (United States)

    Huszank, Robert; Csedreki, László; Török, Zsófia

    2017-02-07

    There are various liquid materials whose elemental composition is of interest in various fields of science and technology. In many cases, sample preparation or the extraction can be complicated, or it would destroy the original environment before the analysis (for example, in the case of biological samples). However, multielement direct analysis of liquid samples can be realized by an external PIXE-PIGE measurement system. Particle-induced X-ray and gamma-ray emission spectroscopy (PIXE, PIGE) techniques were applied in external (in-air) microbeam configuration for the trace and main element determination of liquid samples. The direct analysis of standard solutions of several metal salts and human blood samples (whole blood, blood serum, blood plasma, and formed elements) was realized. From the blood samples, Na, P, S, Cl, K, Ca, Fe, Cu, Zn, and Br elemental concentrations were determined. The focused and scanned ion beam creates an opportunity to analyze very small volume samples (∼10 μL). As the sample matrix consists of light elements, the analysis is possible at ppm level. Using this external beam setup, it was found that it is possible to determine elemental composition of small-volume liquid samples routinely, while the liquid samples do not require any preparation processes, and thus, they can be analyzed directly. In the case of lower concentrations, the method is also suitable for the analysis (down to even ∼1 ppm level) but with less accuracy and longer measurement times.

  14. Solid-phase extraction and determination of trace elements in environmental samples using naphthalene adsorbent

    International Nuclear Information System (INIS)

    Pourreza, N.

    2004-01-01

    Naphthalene co-precipitated with quaternary ammonium salt such as tetraoctyl ammonium bromide and methyltrioctyl ammonium chloride have been used as adsorbent for solid phase extraction of metal ions such as Hg, Cd and Fe. The metal ions are retained on the adsorbent in a column as their complexes with suitable ligands and eluted by an eluent before instrumental measurements. The optimization of the procedures for solid phase extraction and consequent determination of trace elements and application to environmental samples especially water samples will be discussed. (author)

  15. Sample preparation with solid phase microextraction and exhaustive extraction approaches: Comparison for challenging cases.

    Science.gov (United States)

    Boyacı, Ezel; Rodríguez-Lafuente, Ángel; Gorynski, Krzysztof; Mirnaghi, Fatemeh; Souza-Silva, Érica A; Hein, Dietmar; Pawliszyn, Janusz

    2015-05-11

    In chemical analysis, sample preparation is frequently considered the bottleneck of the entire analytical method. The success of the final method strongly depends on understanding the entire process of analysis of a particular type of analyte in a sample, namely: the physicochemical properties of the analytes (solubility, volatility, polarity etc.), the environmental conditions, and the matrix components of the sample. Various sample preparation strategies have been developed based on exhaustive or non-exhaustive extraction of analytes from matrices. Undoubtedly, amongst all sample preparation approaches, liquid extraction, including liquid-liquid (LLE) and solid phase extraction (SPE), are the most well-known, widely used, and commonly accepted methods by many international organizations and accredited laboratories. Both methods are well documented and there are many well defined procedures, which make them, at first sight, the methods of choice. However, many challenging tasks, such as complex matrix applications, on-site and in vivo applications, and determination of matrix-bound and free concentrations of analytes, are not easily attainable with these classical approaches for sample preparation. In the last two decades, the introduction of solid phase microextraction (SPME) has brought significant progress in the sample preparation area by facilitating on-site and in vivo applications, time weighted average (TWA) and instantaneous concentration determinations. Recently introduced matrix compatible coatings for SPME facilitate direct extraction from complex matrices and fill the gap in direct sampling from challenging matrices. Following introduction of SPME, numerous other microextraction approaches evolved to address limitations of the above mentioned techniques. There is not a single method that can be considered as a universal solution for sample preparation. This review aims to show the main advantages and limitations of the above mentioned sample

  16. Elemental analysis of air particulate samples in Jakarta area by x-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Yumiarti; Yusuf, M.; Mellawati, June; Menry, Yulizon; Surtipanti S

    1998-01-01

    Determination of elements in air particulate samples collected from Jakarta, especially from industrial area Pulo Gadung, also from residence, office, and recreation sites had been carried out. The samples collected periodically from August through December 1996. The elements were analyzed by X-ray fluorescence spectrometry method. Quantitative and qualitative analyses were done using QXAS AXIL (Quantitative X-ray Analysis System of x-ray Spectra by Iterative Least squares fitting) and QAES (Quantitative Analyses of Environmental Samples) package program. Results of the analyses showed that the content of heavy metal elements in air particulate samples from all areas studied were still below the maximum permissible concentration. (authors)

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

    International Nuclear Information System (INIS)

    Dmitriev, S.N.; Shishkina, T.V.; Zhuravleva, E.L.; Chimehg, Zh.

    1990-01-01

    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 10 4 , was observed as the most favourable one for the quantitative and selective recovery of gold. For extraction from hydrochloric solutions the D Au 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 5x10 5 at 20 deg C to 9x10 3 at 70 deg C). An anomalously high distribution coefficient of lead (D Pb =10 3 ) 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

  18. 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.

  19. DNA extraction in Echinococcus granulosus and Taenia spp. eggs in dogs stool samples applying thermal shock.

    Science.gov (United States)

    Hidalgo, Alejandro; Melo, Angélica; Romero, Fernando; Hidalgo, Víctor; Villanueva, José; Fonseca-Salamanca, Flery

    2018-03-01

    The extraction of DNA in taeniid eggs shows complications attached to the composition of stool samples and the high resistance of eggs to degradation. The objective of this study was to test a method of DNA extraction in taeniid eggs by applying a thermal shock to facilitate the chemical-enzymatic degradation of these elements. A group of six tubes containing 1 ml of dog stool sample was spiked with eggs of Echinococcus granulosus and another group of six with Taenia pisiformis. Samples were floated with supersaturated sugar solution and centrifuged. The upper portion of each tube (500 μl) was aspirated and deposited in 1.5 ml tubes. Three tubes from each group were incubated at -20 °C and then at 90 °C, the remaining three from each group, incubated at room temperature. Proteinase K and lysis buffer were added to each tube and incubated for 12 h at 58 °C. The lysis effect was evaluated by microscopy at 3, 6 and 12 h and integrity by electrophoresis in 1% agarose gels. With the same experimental scheme, the thermal shock effect was evaluated in extractions of 1, 2, 3 and 4 eggs of each species and the DNA was quantified. Additionally, the protocol was applied in samples of 4 dogs diagnosed with natural infection by Taeniidae worms. Finally, all the extractions were tested by PCR amplification. Both E. granulosus and T. pisiformis eggs showed a similar response in the tests. In samples without treatment, the lysis effect was poor and showed no differences over time, but in those subjected to thermal shock, eggs degradation increased with time. In both treatments, there was no DNA loss integrity. The protocol applied to limited amounts of eggs yielded PCR products in 100% of the samples exposed to thermal shock, allowing PCR amplifications up to 1 egg. In non-exposed samples, the results were not replicable. However, DNA quantification showed low values in both treatments. In turn, DNA extractions with thermal shock in infected dog samples

  20. Simple DNA extraction of urine samples: Effects of storage temperature and storage time.

    Science.gov (United States)

    Ng, Huey Hian; Ang, Hwee Chen; Hoe, See Ying; Lim, Mae-Lynn; Tai, Hua Eng; Soh, Richard Choon Hock; Syn, Christopher Kiu-Choong

    2018-06-01

    Urine samples are commonly analysed in cases with suspected illicit drug consumption. In events of alleged sample mishandling, urine sample source identification may be necessary. A simple DNA extraction procedure suitable for STR typing of urine samples was established on the Promega Maxwell ® 16 paramagnetic silica bead platform. A small sample volume of 1.7mL was used. Samples were stored at room temperature, 4°C and -20°C for 100days to investigate the influence of storage temperature and time on extracted DNA quantity and success rate of STR typing. Samples stored at room temperature exhibited a faster decline in DNA yield with time and lower typing success rates as compared to those at 4°C and -20°C. This trend can likely be attributed to DNA degradation. In conclusion, this study presents a quick and effective DNA extraction protocol from a small urine volume stored for up to 100days at 4°C and -20°C. Copyright © 2018 Elsevier B.V. All rights reserved.

  1. Design of modified annulus air sampling system for the detection of leakage in waste transfer line

    International Nuclear Information System (INIS)

    Deokar, U.V; Khot, A.R.; Mathew, P.; Ganesh, G.; Tripathi, R.M.; Srivastava, Srishti

    2018-01-01

    Various liquid waste streams are generated during the operation of reprocessing plant. The High Level (HL), Intermediate Level (IL) and Low Level (LL) liquid wastes generated, are transferred from reprocessing plant to Waste Management Facility. These respective waste streams are transferred through pipe-in-pipe lines along the shielded concrete trench. For detection of radioactive leakage from primary waste transfer line into secondary line, sampling of the annulus air between the two pipes is carried out. The currently installed pressurized annulus air sampling system did not have online leakage detection provision. Hence, there are chances of personal exposure and airborne activity in the working area. To overcome these design flaws, free air flow modified online annulus air sampling system with more safety features is designed

  2. A rapid and efficient DNA extraction protocol from fresh and frozen human blood samples.

    Science.gov (United States)

    Guha, Pokhraj; Das, Avishek; Dutta, Somit; Chaudhuri, Tapas Kumar

    2018-01-01

    Different methods available for extraction of human genomic DNA suffer from one or more drawbacks including low yield, compromised quality, cost, time consumption, use of toxic organic solvents, and many more. Herein, we aimed to develop a method to extract DNA from 500 μL of fresh or frozen human blood. Five hundred microliters of fresh and frozen human blood samples were used for standardization of the extraction procedure. Absorbance at 260 and 280 nm, respectively, (A 260 /A 280 ) were estimated to check the quality and quantity of the extracted DNA sample. Qualitative assessment of the extracted DNA was checked by Polymerase Chain reaction and double digestion of the DNA sample. Our protocol resulted in average yield of 22±2.97 μg and 20.5±3.97 μg from 500 μL of fresh and frozen blood, respectively, which were comparable to many reference protocols and kits. Besides yielding bulk amount of DNA, our protocol is rapid, economical, and avoids toxic organic solvents such as Phenol. Due to unaffected quality, the DNA is suitable for downstream applications. The protocol may also be useful for pursuing basic molecular researches in laboratories having limited funds. © 2017 Wiley Periodicals, Inc.

  3. High-resolution real-time optical studies of radiological air sample filtration processes in an environmental continuous air monitor

    Science.gov (United States)

    Rodgers, John C.; Wasiolek, Piotr T.; Schery, Stephen D.; Alcantara, Raul E.

    1999-01-01

    The need for a continuous air monitor capable of quick and accurate measurements of airborne radioactivity in close proximity to the work environment during waste management, site restoration, and D&D operations led to the Los Alamos National Laboratory development of an environmental continuous air monitor (ECAM). Monitoring the hostile work environment of waste recovery, for example, presents unique challenges for detector design for detectors previously used for the clean room conditions of the typical plutonium laboratory. The environmental and atmospheric conditions (dust, high wind, etc.) influence aerosol particle penetration into the ECAM sampling head as well as the build-up of deposits on the ECAM filter.

  4. Analytic calculation of radio emission from parametrized extensive air showers: A tool to extract shower parameters

    Science.gov (United States)

    Scholten, O.; Trinh, T. N. G.; de Vries, K. D.; Hare, B. M.

    2018-01-01

    The radio intensity and polarization footprint of a cosmic-ray induced extensive air shower is determined by the time-dependent structure of the current distribution residing in the plasma cloud at the shower front. In turn, the time dependence of the integrated charge-current distribution in the plasma cloud, the longitudinal shower structure, is determined by interesting physics which one would like to extract, such as the location and multiplicity of the primary cosmic-ray collision or the values of electric fields in the atmosphere during thunderstorms. To extract the structure of a shower from its footprint requires solving a complicated inverse problem. For this purpose we have developed a code that semianalytically calculates the radio footprint of an extensive air shower given an arbitrary longitudinal structure. This code can be used in an optimization procedure to extract the optimal longitudinal shower structure given a radio footprint. On the basis of air-shower universality we propose a simple parametrization of the structure of the plasma cloud. This parametrization is based on the results of Monte Carlo shower simulations. Deriving the parametrization also teaches which aspects of the plasma cloud are important for understanding the features seen in the radio-emission footprint. The calculated radio footprints are compared with microscopic CoREAS simulations.

  5. Sample preparation method for the combined extraction of ethyl glucuronide and drugs of abuse in hair.

    Science.gov (United States)

    Meier, Ulf; Briellmann, Thomas; Scheurer, Eva; Dussy, Franz

    2018-04-01

    Often in hair analysis, a small hair sample is available while the analysis of a multitude of structurally diverse substances with different concentration ranges is demanded. The analysis of the different substances often requires different sample preparation methods, increasing the amount of required hair sample. When segmental hair analysis is necessary, the amount of hair sample needed is further increased. Therefore, the required sample amount for a full analysis can quickly exceed what is available. To combat this problem, a method for the combined hair sample preparation using a single extraction procedure for analysis of ethyl glucuronide with liquid chromatography-multistage fragmentation mass spectrometry/multiple reaction monitoring (LC-MS 3 /MRM) and common drugs of abuse with LC-MRM was developed. The combined sample preparation is achieved by separating ethyl glucuronide from the drugs of abuse into separate extracts by fractionation in the solid-phase extraction step during sample clean-up. A full validation for all substances for the parameters selectivity, linearity, limit of detection, limit of quantification, accuracy, precision, matrix effects, and recovery was successfully completed. The following drugs of abuse were included in the method: Amphetamine; methamphetamine; 3,4-methylenedioxy-N-methylamphetamine (MDMA); 3,4-methylenedioxyamphetamine (MDA); 3,4-methylenedioxy-N-ethylamphetamine (MDE); morphine; 6-monoacetylmorphine; codeine; acetylcodeine; cocaine; benzoylecgonine; norcocaine; cocaethylene; methadone; 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP) and methylphenidate. In conclusion, as only 1 sample preparation is needed with 1 aliquot of hair, the presented sample preparation allows an optimal analysis of both ethyl glucuronide and of the drugs of abuse, even when the sample amount is a limiting factor. Copyright © 2017 John Wiley & Sons, Ltd.

  6. The use of cryogenic air sampling in the spectroscopy of airborne gamma-ray emitters

    International Nuclear Information System (INIS)

    Perdue, P.T.; Haywood, F.F.

    1982-01-01

    Wet air can be sampled over a period of four to twelve hours and, with a transfer into a special Marinelli-dewar, can be counted in a spectrometer for several hours. The present minimum detectable amount is about 4 Bq/m 3 for 222 Rn and 220 Rn with liquid air in the counting dewar equivalent to one cubic meter of ambient air. The amount of ambient air sampled can be determined from ambient pressure, temperature, and absolute humidity determinations. Standard meteorological tables are used to determine the weight of ambient air in grams/litre. This quantity divided into the net weight of liquid yields the total litres of ambient air sampled. Tests run so far with 85 Kr indicate that the noble fission gases behave in a manner similar to radon, allowing measurements of stack gases, reactor plumes, etc. The minimum detectable quantity of 85 Kr appears to be about 300 Bq/m 3 , depending upon the 222 Rn and 220 Rn content of the air

  7. Speciation and Determination of Low Concentration of Iron in Beer Samples by Cloud Point Extraction

    Science.gov (United States)

    Khalafi, Lida; Doolittle, Pamela; Wright, John

    2018-01-01

    A laboratory experiment is described in which students determine the concentration and speciation of iron in beer samples using cloud point extraction and absorbance spectroscopy. The basis of determination is the complexation between iron and 2-(5-bromo-2- pyridylazo)-5-diethylaminophenol (5-Br-PADAP) as a colorimetric reagent in an aqueous…

  8. 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...

  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...

  10. Extraction and analysis of 14C-carbofuran radioactivity in soil sample

    International Nuclear Information System (INIS)

    Maizatul Akmam Mhd Nasir; Nashriyah Mat

    2005-01-01

    Carbofuran insecticide or nematicide sprayed onto soil in the agroecosystem will be taken up by plant. Carbofuran residue will pollute the environment and organisms in the food chain. Extraction and analysis of 14 C-carbofuran in soil from lysimeter were carried out. The Liquid Scintillation Counter (LSC) was used to measure radioactivity of 14 C-carbofuran in soil sample. (Author)

  11. A sensitive LC-MS/MS method for measurement of organophosphorus pesticides and their oxygen analogs in air sampling matrices.

    Science.gov (United States)

    Armstrong, Jenna L; Dills, Russell L; Yu, Jianbo; Yost, Michael G; Fenske, Richard A

    2014-01-01

    A rapid liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed for determination of levels of the organophosphorus (OP) pesticides chlorpyrifos (CPF), azinphos methyl (AZM), and their oxygen analogs chlorpyrifos-oxon (CPF-O) and azinphos methyl-oxon (AZM-O) on common active air sampling matrices. XAD-2 resin and polyurethane foam (PUF) matrices were extracted with acetonitrile containing stable-isotope labeled internal standards (ISTD). Analysis was accomplished in Multiple Reaction Monitoring (MRM) mode, and analytes in unknown samples were identified by retention time (±0.1 min) and qualifier ratio (±30% absolute) as compared to the mean of calibrants. For all compounds, calibration linearity correlation coefficients were ≥0.996. Limits of detection (LOD) ranged from 0.15-1.1 ng/sample for CPF, CPF-O, AZM, and AZM-O on active sampling matrices. Spiked fortification recoveries were 78-113% from XAD-2 active air sampling tubes and 71-108% from PUF active air sampling tubes. Storage stability tests also yielded recoveries ranging from 74-94% after time periods ranging from 2-10 months. The results demonstrate that LC-MS/MS is a sensitive method for determining these compounds from two different matrices at the low concentrations that can result from spray drift and long range transport in non-target areas following agricultural applications. In an inter-laboratory comparison, the limit of quantification (LOQ) for LC-MS/MS was 100 times lower than a typical gas chromatography-mass spectrometry (GC-MS) method.

  12. 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

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

    International Nuclear Information System (INIS)

    Lee, Won; Hong, Jee Eun; Park, Song Ja; Pyo, Hee Soo; Kim, In Hwan

    1998-01-01

    The separation and sample extraction methods of 19 polycyclic aromatic hydrocarbons (PAH S ) 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 PAH s was possible by partial variation of oven temperature of GC/MS in temperature range 80∼310.deg.C. Extraction procedures of PAH s in water samples were somewhat modified and com-pared as extraction recoveries and the simplicity of methods. Extraction recoveries of PAH s 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 C 1 8 disk extraction method by filtration. And extraction recoveries of PAH s by C 1 8 solid-phase were in the range of 51.8∼77.9%. Method detection limits (S/N=5) of 19 PAH s 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

  14. Optimization Extracting Technology of Cynomorium songaricum Rupr. Saponins by Ultrasonic and Determination of Saponins Content in Samples with Different Source

    OpenAIRE

    Xiaoli Wang; Qingwei Wei; Xinqiang Zhu; Chunmei Wang; Yonggang Wang; Peng Lin; Lin Yang

    2015-01-01

    Extraction process was optimized by single factor and orthogonal experiment (L9 (34)). Moreover, the content determination was studied in methodology. The optimum ultrasonic extraction conditions were: ethanol concentration of 75%, ultrasonic power of 420 w, the solid-liquid ratio of 1:15, extraction duration of 45 min, extraction temperature of 90°C and extraction for 2 times. Saponins content in Guazhou samples was significantly higher than those in Xinjiang and Inner Mongolia. Meanwhile, G...

  15. Disposable cartridge extraction of retinol and alpha-tocopherol from fatty samples.

    Science.gov (United States)

    Bourgeois, C F; Ciba, N

    1988-01-01

    A new approach is proposed for liquid/solid extraction of retinol and alpha-tocopherol from samples, using a disposable kieselguhr cartridge. The substitution of the mixture methanol-ethanol-n-butanol (4 + 3 + 1) for methanol in the alkaline hydrolysis solution makes it now possible to process fatty samples. Methanol is necessary to solubilize the antioxidant ascorbic acid, and a linear chain alcohol such as n-butanol is necessary to reduce the size of soap micelles so that they can penetrate into the kieselguhr pores. In comparisons of the proposed method with conventional methods on mineral premixes and fatty feedstuffs, recovery and accuracy are at least as good by the proposed method. Advantages are increased rate of determinations and the ability to hydrolyze and extract retinol and alpha-tocopherol together from the same sample.

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

    International Nuclear Information System (INIS)

    Oliveira, Andrea; Cadore, Solange; Baccan, Nivaldo

    2012-01-01

    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)

  17. A technique for extracting blood samples from mice in fire toxicity tests

    Science.gov (United States)

    Bucci, T. J.; Hilado, C. J.; Lopez, M. T.

    1976-01-01

    The extraction of adequate blood samples from moribund and dead mice has been a problem because of the small quantity of blood in each animal and the short time available between the animals' death and coagulation of the blood. These difficulties are particularly critical in fire toxicity tests because removal of the test animals while observing proper safety precautions for personnel is time-consuming. Techniques for extracting blood samples from mice were evaluated, and a technique was developed to obtain up to 0.8 ml of blood from a single mouse after death. The technique involves rapid exposure and cutting of the posterior vena cava and accumulation of blood in the peritoneal space. Blood samples of 0.5 ml or more from individual mice have been consistently obtained as much as 16 minutes after apparent death. Results of carboxyhemoglobin analyses of blood appeared reproducible and consistent with carbon monoxide concentrations in the exposure chamber.

  18. Development of a simple extraction procedure for chlorpyrifos determination in food samples by immunoassay.

    Science.gov (United States)

    Gabaldón, J A; Maquieira, A; Puchades, R

    2007-02-28

    The suitability of immunoassay methodology for rapid and accurate determination of chlorpyrifos in vegetables was tested. The optimised ELISA detection limit was 0.32ng/ml, with a working range from 0.69 to 6.21ng/ml and an immunoassay test-mid point (IC(50)) of 2.08ng/ml. A rapid sample preparation procedure considering different parameters such as the amount of sample, volume of extractant, extraction time and dilution factor was optimised. The developed direct extraction (DE) and multiresidue (ME) standard procedures were performed in different fortified fresh and processed vegetable samples (tomato, bonnet pepper, bean, pea, asparagus, broccoli, watermelon, melon, lettuce, cucumber, celery and red pepper). Recoveries were in all cases in the whole range 85.2-108.9% for both DE and ME extracts. Also, the comparison of the results obtained by both immunochemical and chromatographic methods for spiked fruits and vegetables were good with a correlation coefficient (r) of 0.97.

  19. Multiresidual determination of pesticides in agricultural soil sample using Quechers extraction methodology

    International Nuclear Information System (INIS)

    Castro Garcia, Consuelo del Pilar

    2011-01-01

    To achieve a sustainable agricultural production there are used different organic and inorganic products, among them we found the fertilizers and pesticides. When they are applied most of the product falls to the ground, generating significant sources of pollution in the areas near the application and depending on the mobility of the pesticide, it can reach more remote areas. That is why it is important to determine the pesticide residues in soil after their application, being the selection of the extraction method crucial for the subsequent traces detection. In the present work there was evaluated the QUECHERS extraction technique, a method used in food but modified for a different and complex matrix like soil in order to achieve acceptable efficiencies multi-residue extraction of 20 pesticides and their subsequent determination by gas chromatography with electron capture and mass detection. The method was applied for the determination of pesticides in three soil samples from an agricultural site with different slopes between them. The Results indicated that 75% of the pesticides tested had acceptable efficiencies, thus meeting the objective of achieving multiresidue determination of pesticides in agricultural soil samples by extraction methodology QUECHERS. Besides, the presence of the fungicide penconazole was only detected in the three samples, being the highest concentration of pesticide found in the area with less slope (V_A_B_A_J_O) (author)

  20. Electromembrane extraction of tartrazine from food samples: Effects of nano-sorbents on membrane performance.

    Science.gov (United States)

    Yaripour, Saeid; Mohammadi, Ali; Nojavan, Saeed

    2016-07-01

    In the present study, for the first time electromembrane extraction followed by high-performance liquid chromatography coupled with ultraviolet detection was developed and validated for the determination of tartrazine in some food samples. The parameters influencing electromembrane extraction were evaluated and optimized. The membrane consists of 1-octanol immobilized in the pores of a hollow fiber. As a driving force, a 30 V electrical field was applied to make the analyte migrate from sample solution with pH 3, through the supported liquid membrane into an acceptor solution with pH 10. Best preconcentration (enrichment factor >21) was obtained in extraction duration of 15 min. Effects of some solid nano-sorbents like carbon nanotubes and molecularly imprinted polymers on membrane performance and electromembrane extraction efficiency were evaluated. The method provided the linearity in the range 25-1000 ng/mL for tartrazine (R(2) > 0.9996) with repeatability range (RSD) between 3.8 and 8.5% (n = 3). The limits of detection and quantitation were 7.5 and 25 ng/mL, respectively. Finally, the method was applied to the determination and quantification of tartrazine from some food samples with relative recoveries in the range between 90 and 98%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    International Nuclear Information System (INIS)

    Kanekar, A.S.; Pathak, P.N.; Mohapatra, P.K.

    2014-01-01

    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 137 Cs from soil samples was difficult under the conditions of these studies. However, experiments performed on tissue papers (cellulose matrix) showed quantitative recovery of 137 Cs. On the other hand, 137 Cs recovery from plant samples varied between ∼50 % (for stems) and ∼67.2 % (for leaves) employing 1x10 -3 M CC + 4 M HNO 3 dissolved in acetonitrile. (author)

  2. 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).

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

    Energy Technology Data Exchange (ETDEWEB)

    Schindler, Matthias, E-mail: matthias.schindler@physik.uni-erlangen.de; Kretschmer, Wolfgang; Scharf, Andreas; Tschekalinskij, Alexander

    2016-05-15

    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 CO{sub 2} and reduced to graphite to determine {sup 14}C 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).

  4. Monte Carlo simulation of air sampling methods for the measurement of radon decay products.

    Science.gov (United States)

    Sima, Octavian; Luca, Aurelian; Sahagia, Maria

    2017-08-01

    A stochastic model of the processes involved in the measurement of the activity of the 222 Rn decay products was developed. The distributions of the relevant factors, including air sampling and radionuclide collection, are propagated using Monte Carlo simulation to the final distribution of the measurement results. The uncertainties of the 222 Rn decay products concentrations in the air are realistically evaluated. Copyright © 2017 Elsevier Ltd. All rights reserved.

  5. Actinide nuclides in environmental air and precipitation samples after the Chernobyl accident

    International Nuclear Information System (INIS)

    Rosner, G.; Hoetzl, H.; Winkler, R.

    1988-01-01

    The present paper describes the analysis of isotopes of uranium, neptunium, plutonium, americium and curium, in air and deposition samples taken at our laboratory site 10 km north of Munich, subsequent to the Chernobyl accident. Uranium-234, 237 U, 238 U, 239 Np, 238 Pu, 239+240 Pu and 242 Cm have been identified and upper limits of detection have been established for 241 Am and 244 Cm. Deposition and air concentration values are discussed. 12 refs., 1 fig., 2 tabs

  6. 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.

  7. 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.

  8. 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

  9. 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)

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

    International Nuclear Information System (INIS)

    Nardes, Raysa C.; Santos, Ramon S.; Sanches, Francis A.C.R.A.; Gama Filho, Hamilton S.; Oliveira, Davi F.; Anjos, Marcelino J.

    2015-01-01

    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)

  11. Remote tritium-in-air sampling in reactor building at NAPS

    International Nuclear Information System (INIS)

    Mitra, S.R.; Lal Chand

    2000-01-01

    Tritium-in-air activity is an important parameter in PHW reactors from the point of view of internal exposure and heavy water escape from the system. The sampling technique in vogue in PHWRs, for measurement of tritium-in-air activity, requires collection of on the spot sample from different areas using a portable sampler. This sampler uses the bubbler method of sampling. As the areas of sampling are numerous, this technique is time consuming, laborious and can lead to significant internal exposure in areas where tritium-in-air activity is high. This technique is also error prone due to the heavy workload involved. A new scheme, in which the sampling of all the areas of reactor building is done through a sampling station, has been introduced for the first time in NAPS. This sampling station facilitates collection of samples from all the areas of reactor building, remotely and simultaneously at one place thereby reducing time, labour, exposure and error. This paper gives the details of the sampling system installed at NAPS. (author)

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

    International Nuclear Information System (INIS)

    Gregory, D.C.; Bryan, W.L.; Falter, K.G.

    1993-01-01

    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

  13. Recommended radiological air sampling and internal contamination control at nuclear power plants

    International Nuclear Information System (INIS)

    Rich, B.L.; Ritter, P.D.; Martz, D.E.

    1984-01-01

    It has long been recognized by the NRC Technical Staffs that estimating the quantity of radioactivity inhaled by an individual worker involved large uncertainties. General air samples usually produce concentrations lower than those in the workers Breathing Zone (BZ). NRC guides have recognized this problem by specifying air monitoring programs which sample the Breathing Zone or concentrations known to be higher than that actually inhaled. In addition the availability of suitable samplers to obtain BZ samples and the practicality of requiring their use was somewhat in question to the NRC technical staff. AN NRC development contract was issued to provide a detailed review of the technical aspects of the problems and recommendations for practical upgrade of federal guidance. This project accomplished a review of the nuclear industry experience and knowledge through a literature search, site visits to representative licensed facilities, telephone surveys of many others, laboratory testing of personal air samplers (lapel samplers) and aerosol diffusion experiments to verify key conclusions and assumptions

  14. Sampling for Air Chemical Emissions from the Life Sciences Laboratory II

    Energy Technology Data Exchange (ETDEWEB)

    Ballinger, Marcel Y. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Lindberg, Michael J. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2017-03-30

    Sampling for air chemical emissions from the Life Science Laboratory II (LSL-II) ventilation stack was performed in an effort to determine potential exposure of maintenance staff to laboratory exhaust on the building roof. The concern about worker exposure was raised in December 2015 and several activities were performed to assist in estimating exposure concentrations. Data quality objectives were developed to determine the need for and scope and parameters of a sampling campaign to measure chemical emissions from research and development activities to the outside air. The activities provided data on temporal variation of air chemical concentrations and a basis for evaluating calculated emissions. Sampling for air chemical emissions was performed in the LSL-II ventilation stack over the 6-week period from July 26 to September 1, 2016. A total of 12 sampling events were carried out using 16 sample media. Resulting analysis provided concentration data on 49 analytes. All results were below occupational exposure limits and most results were below detection limits. When compared to calculated emissions, only 5 of the 49 chemicals had measured concentrations greater than predicted. This sampling effort will inform other study components to develop a more complete picture of a worker’s potential exposure from LSL-II rooftop activities. Mixing studies were conducted to inform spatial variation in concentrations at other rooftop locations and can be used in conjunction with these results to provide temporal variations in concentrations for estimating the potential exposure to workers working in and around the LSL-II stack.

  15. Comparison of marine sampling methods for organic contaminants: Passive samplers, water extractions, and live oyster deployment.

    Science.gov (United States)

    Raub, Kristin B; Vlahos, Penny; Whitney, Michael

    2015-08-01

    Laboratory and field trials evaluated the efficacy of three methods of detecting aquatic pesticide concentrations. Currently used pesticides: atrazine, metolachlor, and diazinon and legacy pesticide dieldrin were targeted. Pesticides were extracted using solid-phase extraction (SPE) of water samples, titanium plate passive samplers coated in ethylene vinyl acetate (EVA) and eastern oysters (Crassostrea viginica) as biosamplers. A laboratory study assessed the extraction efficiencies and precision of each method. Passive samplers yielded the highest precision of the three methods (RSD: 3-14% EVA plates; 19-60% oysters; and 25-56% water samples). Equilibrium partition coefficients were derived. A significant relationship was found between the concentration in oyster tissue and the ambient aquatic concentration. In the field (Housatonic River, CT (U.S.)) water sampling (n = 5) detected atrazine at 1.61-7.31 μg L(-1), oyster sampling (n = 2×15) detected dieldrin at n.d.-0.096 μg L(-1) SW and the passive samplers (n = 5×3) detected atrazine at 0.97-3.78 μg L(-1) SW and dieldrin at n.d.-0.68 μg L(-1) SW. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Removal of nitrogen compounds from Brazilian petroleum samples by oxidation followed by liquid-liquid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Conceicao, L.; Pergher, S.B.C. [Universidade Regional Integrada do Alto Uruguai e das Misses (URI), Erechim, RS (Brazil). Dept. de Quimica], E-mail: pergher@uricer.edu.br; Oliveira, J.V. [Universidade Regional Integrada do Alto Uruguai e das Misses (URI), Erechim, RS (Brazil). Dept. de Engenharia dos Alimentos; Souza, W.F. [Petroleo Brasileiro S.A. (CENPES/PETROBRAS), Rio de Janeiro, RJ (Brazil). Centro de Pesquisas

    2009-10-15

    This work reports liquid-liquid extraction of nitrogen compounds from oxidized and non-oxidized Brazilian petroleum samples. The experiments were accomplished in a laboratory-scale liquid-liquid apparatus in the temperature range of 303 K-323 K, using methanol, n-methyl-2-pyrrolidone (NMP) and N,Ndimethylformamide (DMF), and their mixtures as extraction solvents, employing solvent to sample volume ratios of 1:2, 1:1 and 2:1, exploring up to three separation stages. Results show that an increase in temperature, solvent to oil ratio, and number of equilibrium stages greatly improves the nitrogen removal from the oxidized sample (from 2600 to 200 ppm). The employed oxidation scheme is thus demonstrated to be an essential and efficient step of sample preparation for the selective liquid-liquid removal of nitrogen compounds. It is shown that the use of mixtures of DMF and NMP as well their use as co-solvents with methanol did not prove to be useful for selective nitrogen extraction since great oil losses were observed in the final process. (author)

  17. Known volume air sampling pump. Final summary report Jun 1975--Nov 1976

    International Nuclear Information System (INIS)

    McCullough, J.E.; Peterson, A.

    1976-11-01

    The purpose of this development program was to design and develop a known volume air sampling pump for use in measuring the amount of radioactive material in the atmosphere of an underground uranium mine. The principal nuclear radiation hazard to underground uranium mines comes from the mine atmosphere. Daughter products of radon-222 are inhaled by the miner resulting in a relatively high lung cancer rate among these workers. Current exposure control practice employs spot sampling in working areas to measure working level values. Currently available personal air sampling pumps fail to deliver known volumes of air under widely changing differential pressures. A unique type of gas pump known as the scroll compressor, developed by Arthur D. Little, Inc., that has no values and few moving parts is expected to provide a practical, efficient, and dependable air pump for use in dosimeters. The three deliverable known volume air sampling pumps resulting from this work incorporate a scroll pump, drive motor, speed control electronics, and battery pack in a container suitable for attachment to a miner's belt

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

    International Nuclear Information System (INIS)

    Martins, Ana Paula G.; Negri, Elnara M.; Saldiva, Paulo H.N.

    2009-01-01

    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)

  19. Use of a Radon Stripping Algorithm for Retrospective Assessment of Air Filter Samples

    International Nuclear Information System (INIS)

    Hayes, Robert

    2009-01-01

    An evaluation of a large number of air sample filters was undertaken using a commercial alpha and beta spectroscopy system employing a passive implanted planar silicon (PIPS) detector. Samples were only measured after air flow through the filters had ceased. Use of a commercial radon stripping algorithm was implemented to discriminate anthropogenic alpha and beta activity on the filters from the radon progeny. When uncontaminated air filters were evaluated, the results showed that there was a time-dependent bias in both average estimates and measurement dispersion with the relative bias being small compared to the dispersion. By also measuring environmental air sample filters simultaneously with electroplated alpha and beta sources, use of the radon stripping algorithm demonstrated a number of substantial unexpected deviations. Use of the current algorithm is therefore not recommended for assay applications and so use of the PIPS detector should only be utilized for gross counting without appropriate modifications to the curve fitting algorithm. As a screening method, the radon stripping algorithm might be expected to see elevated alpha and beta activities on air sample filters (not due to radon progeny) around the 200 dpm level

  20. Occurrence of commonly used pesticides in personal air samples and their associated health risk among paddy farmers.

    Science.gov (United States)

    Hamsan, Hazwanee; Ho, Yu Bin; Zaidon, Siti Zulfa; Hashim, Zailina; Saari, Nazamid; Karami, Ali

    2017-12-15

    Tanjung Karang, Selangor, is widely known for its paddy cultivation activity and hosts the third largest paddy field in Malaysia. Pesticides contamination in agriculture fields has become an unavoidable problem, as pesticides are used to increase paddy productivity and reduce plant disease. Human exposure to agrichemicals is common and could results in both acute and chronic health effects, such as acute and chronic neurotoxicity. This study aims to determine the concentrations of commonly used pesticides (azoxystrobin, buprofezin, chlorantraniliprole, difenoconazole, fipronil, imidacloprid, isoprothiolane, pretilachlor, propiconazole, pymetrozine, tebuconazole, tricyclazole, and trifloxystrobin) in personal air samples and their associated health risks among paddy farmers. Eighty-three farmers from Tangjung Karang, Selangor were involved in this study. A solid sorbent tube was attached to the farmer's breathing zone with a clip, and an air pump was fastened to the belt to collect personal air samples. Pesticides collected in the XAD-2 resin were extracted with acetone, centrifuged, concentrated via nitrogen blowdown and reconstituted with 1mL of 3:1 ultrapure water/HPLC-grade methanol solution. The extract was analyzed using ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). The target compounds were detected with a maximum concentration reaching up to 462.5ngm -3 (fipronil). The hazard quotient (HQ) was less than 1 and the hazard index (HI) value was 3.86×10 -3 , indicating that the risk of pesticides related diseases was not significant. The lifetime cancer risk (LCR) for pymetrozine was at an acceptable level (LCR<10 -6 ) with 4.10×10 -8 . The results reported in this study can be beneficial in terms of risk management within the agricultural community. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Profiling quinones in ambient air samples collected from the Athabasca region (Canada).

    Science.gov (United States)

    Wnorowski, Andrzej; Charland, Jean-Pierre

    2017-12-01

    This paper presents new findings on polycyclic aromatic hydrocarbon oxidation products-quinones that were collected in ambient air samples in the proximity of oil sands exploration. Quinones were characterized for their diurnal concentration variability, phase partitioning, and molecular size distribution. Gas-phase (GP) and particle-phase (PM) ambient air samples were collected separately in the summer; a lower quinone content was observed in the PM samples from continuous 24-h sampling than from combined 12-h sampling (day and night). The daytime/nocturnal samples demonstrated that nighttime conditions led to lower concentrations and some quinones not being detected. The highest quinone levels were associated with wind directions originating from oil sands exploration sites. The statistical correlation with primary pollutants directly emitted from oil sands industrial activities indicated that the bulk of the detected quinones did not originate directly from primary emission sources and that quinone formation paralleled a reduction in primary source NO x levels. This suggests a secondary chemical transformation of primary pollutants as the origin of the determined quinones. Measurements of 19 quinones included five that have not previously been reported in ambient air or in Standard Reference Material 1649a/1649b and seven that have not been previously measured in ambient air in the underivatized form. This is the first paper to report on quinone characterization in secondary organic aerosols originating from oil sands activities, to distinguish chrysenequinone and anthraquinone positional isomers in ambient air, and to report the requirement of daylight conditions for benzo[a]pyrenequinone and naphthacenequinone to be present in ambient air. Crown Copyright © 2017. Published by Elsevier Ltd. All rights reserved.

  2. Extraction of trace nitrophenols in environmental water samples using boronate affinity sorbent

    International Nuclear Information System (INIS)

    Zhang, Yong; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

    2015-01-01

    In this research, the applicability of a new sorbent based on boronate affinity material is demonstrated. For this purpose, six strong polar nitrophenols were selected as models which are difficult to be extracted in neutral form (only based on hydrophobic interactions). The extracted nitrophenols were separated and determined by high-performance liquid chromatography with diode array detection. The sorbent was synthesized by in situ copolymerization of 3-acrylamidophenylboronic acid and divinylbenzene using dimethyl sulfoxide and azobisisobutyronitrile as porogen solvent and initiator, respectively. The effect of the preparation parameters in the polymerization mixture on extraction performance was investigated in detail. The size and morphology of the sorbent have been characterized via different techniques such as infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. The important parameters influencing the extraction efficiency were studied and optimized thoroughly. Under the optimum extraction conditions, the limits of detection (S/N = 3) and limits of quantification (S/N = 10) for the target nitrophenols were 0.097–0.28 and 0.32–0.92 μg/L, respectively. The precision of the proposed method was evaluated in terms of intra- and inter-assay variability calculated as RSD, and it was found that the RSDs were all below 9%. Finally, the developed method was successfully applied for environmental water samples such as wastewater, tap, lake and river water. The recoveries varied within the range of 71.2–115% with RSD below 11% in all cases. The results well demonstrate that the new boronate affinity sorbent can extract nitrophenols effectively through multi-interactions including boron–nitrogen coordination, hydrogen-bond and hydrophobic interactions between sorbent and analytes. - Highlights: • A new boronate affinity sorbent (BAS) was prepared. • The BAS was used as the extractive medium of stir

  3. An advanced computer-controlled automatic alpha-beta air sample counter

    International Nuclear Information System (INIS)

    Howell, W.P.; Bruinekool, D.J.; Stapleton, E.E.

    1984-01-01

    An improved computer-controlled automatic alpha-beta air sample counter was developed, based upon an earlier automatic air sample counter design. The system consists of an automatic sample changer, an electronic counting system utilizing a large silicon diode detector, a small desk-type microcomputer, a high-speed matrix printer and the necessary data interfaces. The system is operated by commands from the keyboard and programs stored on magnetic tape cassettes. The programs provide for background counting, Chi 2 test, radon subtraction and sample counting for sample periods of one day to one week. Output data are printed by the matrix printer on standard multifold paper. The data output includes gross beta, gross alpha and plutonium results. Data are automatically corrected for background, counter efficiency, and in the gross alpha and plutonium channels, for the presence of radon

  4. Advanced computer-controlled automatic alpha-beta air sample counter

    International Nuclear Information System (INIS)

    Howell, W.P.; Bruinekool, D.J.; Stapleton, E.E.

    1983-01-01

    An improved computer controlled automatic alpha-beta air sample counter was developed, based upon an earlier automatic air sample counter design. The system consists of an automatic sample changer, an electronic counting system utilizing a large silicon diode detector, a small desk-type microcomputer, a high speed matrix printer, and the necessary data interfaces. The system is operated by commands from the keyboard and programs stored on magnetic tape cassettes. The programs provide for background counting, Chi 2 test, radon subtraction, and sample counting for sample periods of one day to one week. Output data are printed by the matrix printer on standard multifold paper. The data output includes gross beta, gross alpha, and plutonium results. Data are automatically corrected for background, counter efficiency, and in the gross alpha and plutonium channels, for the presence of radon

  5. 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

    2016-01-01

    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). 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. 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. Results suggest that FTA® is a practical, safe and economical method to preserve P. jirovecii-DNA in BAL samples for molecular studies.

  6. 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

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

    International Nuclear Information System (INIS)

    Vaikkinen, A.; Kotiaho, T.; Kostiainen, R.; Kauppila, T.J.

    2010-01-01

    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

  8. Ambient air sampling of organic pollutants and heavy metals within the EU/93/AIR/22 PHARE Project

    International Nuclear Information System (INIS)

    Kocan, A.

    1997-01-01

    Within the framework of the project the concentrations of eight heavy metals, vapour mercury, seven polychlorinated dibenzo-p-dioxin's, ten polychlordibenzofuran congeners, eighteen polychlorinated biphenyls, two chlorinated pesticides (hexachlorobenzene, p,p'-DDE and p,p'-DDT), fourteen polycyclic aromatic hydrocarbons, forty-two volatile organic compounds, total suspended particles were analysed. The morphology characterization of collected airborne particles and bioassays aimed at the evaluation of the mutagenic potency of pollutants present in collected air were also performed. Ambient air heavy metals were caught on cellulose filters using the same type of the sampler used for semi-volatile compounds sampling and analysed by atomic spectrometry. Vapour mercury was trapped on gold sand packed in a tube through which about 280 L of ambient air during 24 hours were drawn. On-site analysis was performed by an atomic fluorescence analyzer. Inhalable air particles, i.e particles less than 10 μm in diameter were collected by a sampler equipped with a cascade impactor fractionating into five size fractions involving respirable (<3 μm) fractions. The morphology and composition of the respirable fractions was investigated by scanning electron microscopy and X-ray microanalysis

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

    International Nuclear Information System (INIS)

    Fourcade, N.; Zettwoog, P.; Mery, G.

    1994-01-01

    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

  10. Cloud point extraction, preconcentration and spectrophotometric determination of nickel in water samples using dimethylglyoxime

    Directory of Open Access Journals (Sweden)

    Morteza Bahram

    2013-01-01

    Full Text Available A new and simple method for the preconcentration and spectrophotometric determination of trace amounts of nickel was developed by cloud point extraction (CPE. In the proposed work, dimethylglyoxime (DMG was used as the chelating agent and Triton X-114 was selected as a non-ionic surfactant for CPE. The parameters affecting the cloud point extraction including the pH of sample solution, concentration of the chelating agent and surfactant, equilibration temperature and time were optimized. Under the optimum conditions, the calibration graph was linear in the range of 10-150 ng mL-1 with a detection limit of 4 ng mL-1. The relative standard deviation for 9 replicates of 100 ng mL-1 Ni(II was 1.04%. The interference effect of some anions and cations was studied. The method was applied to the determination of Ni(II in water samples with satisfactory results.

  11. Ambient air sampling for radioactive air contaminants at Los Alamos National Laboratory: A large research and development facility

    International Nuclear Information System (INIS)

    Eberhart, C.F.

    1998-01-01

    This paper describes the ambient air sampling program for collection, analysis, and reporting of radioactive air contaminants in and around Los Alamos National Laboratory (LANL). Particulate matter and water vapor are sampled continuously at more than 50 sites. These samples are collected every two weeks and then analyzed for tritium, and gross alpha, gross beta, and gamma ray radiation. The alpha, beta, and gamma measurements are used to detect unexpected radionuclide releases. Quarterly composites are analyzed for isotopes of uranium ( 234 U, 235 U, 238 U), plutonium ( 238 Pu, 239/249 Pu), and americium ( 241 Am). All of the data is stored in a relational database with hard copies as the official records. Data used to determine environmental concentrations are validated and verified before being used in any calculations. This evaluation demonstrates that the sampling and analysis process can detect tritium, uranium, plutonium, and americium at levels much less than one percent of the public dose limit of 10 millirems. The isotopic results also indicate that, except for tritium, off-site concentrations of radionuclides potentially released from LANL are similar to typical background measurements

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

    International Nuclear Information System (INIS)

    Peters, T.; Fink, S.

    2011-01-01

    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(reg s ign) 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.

  13. Air-sampling inlet contamination by aircraft emissions on the NASA CV-990 aircraft

    Science.gov (United States)

    Condon, E. P.; Vedder, J. F.

    1984-01-01

    Results of an experimental investigation of the contamination of air sampling inlets by aircraft emissions from the NASA CV-990 research aircraft are presented. This four-engine jet aircraft is a NASA facility used for many different atmospheric and meteorological experiments, as well as for developing spacecraft instrumentation for remote measurements. Our investigations were performed to provide information on which to base the selection of sampling locations for a series of multi-instrument missions for measuring tropospheric trace gases. The major source of contamination is the exhaust from the jet engines, which generate many of the same gases that are of interest in atmospheric chemistry, as well as other gases that may interfere with sampling measurements. The engine exhaust contains these gases in mixing ratios many orders of magnitude greater than those that occur in the clean atmosphere which the missions seek to quantify. Pressurized samples of air were collected simultaneously from a scoop located forward of the engines to represent clean air and from other multiport scoops at various aft positions on the aircraft. The air samples were analyzed in the laboratory by gas chromatography for carbon monoxide, an abundant combustion by-product. Data are presented for various scoop locations under various flight conditions.

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

    International Nuclear Information System (INIS)

    MULKEY, C.H.

    1999-01-01

    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

  15. Air pollution impacts due to petroleum extraction in the Norwegian Sea during the ACCESS aircraft campaign

    Directory of Open Access Journals (Sweden)

    P. Tuccella

    2017-06-01

    Full Text Available Emissions from oil/gas extraction activities in the Arctic are already important in certain regions and may increase as global warming opens up new opportunities for industrial development. Emissions from oil/gas extraction are sources of air pollutants, but large uncertainties exist with regard to their amounts and composition. In this study, we focus on detailed investigation of emissions from oil/gas extraction in the Norwegian Sea combining measurements from the EU ACCESS aircraft campaign in July 2012 and regional chemical transport modeling. The goal is to (1 evaluate emissions from petroleum extraction activities and (2 investigate their impact on atmospheric composition over the Norwegian Sea. Numerical simulations include emissions for permanently operating offshore facilities from two datasets: the TNO-MACC inventory and emissions reported by Norwegian Environment Agency (NEA. It was necessary to additionally estimate primary aerosol emissions using reported emission factors since these emissions are not included in the inventories for our sites. Model runs with the TNO-MACC emissions are unable to reproduce observations close to the facilities. Runs using the NEA emissions more closely reproduce the observations although emissions from mobile facilities are missing from this inventory. Measured plumes suggest they are a significant source of pollutants, in particular NOx and aerosols. Sensitivities to NOx and NMVOC emissions show that, close to the platforms, O3 is sensitive to NOx emissions and is much less sensitive to NMVOC emissions. O3 destruction, via reaction with NO, dominates very close to the platforms. Far from the platforms, oil/gas facility emissions result in an average daytime O3 enhancement of +2% at the surface. Larger enhancements are predicted at noon ranging from +7% at the surface to +15% at 600 m. Black carbon is the aerosol species most strongly influenced by petroleum extraction emissions. The results highlight

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

    International Nuclear Information System (INIS)

    Mohammed Salisu Musa; Wan Aini Wan Ibrahim

    2015-01-01

    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, r 2 ≥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)

  17. [Optimization of solid-phase extraction for enrichment of toxic organic compounds in water samples].

    Science.gov (United States)

    Zhang, Ming-quan; Li, Feng-min; Wu, Qian-yuan; Hu, Hong-ying

    2013-05-01

    A concentration method for enrichment of toxic organic compounds in water samples has been developed based on combined solid-phase extraction (SPE) to reduce impurities and improve recoveries of target compounds. This SPE method was evaluated in every stage to identify the source of impurities. Based on the analysis of Waters Oasis HLB without water samples, the eluent of SPE sorbent after dichloromethane and acetone contributed 85% of impurities during SPE process. In order to reduce the impurities from SPE sorbent, soxhlet extraction of dichloromethane followed by acetone and lastly methanol was applied to the sorbents for 24 hours and the results had proven that impurities were reduced significantly. In addition to soxhlet extraction, six types of prevalent SPE sorbents were used to absorb 40 target compounds, the lgK(ow) values of which were within the range of 1.46 and 8.1, and recovery rates were compared. It was noticed and confirmed that Waters Oasis HLB had shown the best recovery results for most of the common testing samples among all three styrenedivinylbenzene (SDB) polymer sorbents, which were 77% on average. Furthermore, Waters SepPak AC-2 provided good recovery results for pesticides among three types of activated carbon sorbents and the average recovery rates reached 74%. Therefore, Waters Oasis HLB and Waters SepPak AC-2 were combined to obtain a better recovery and the average recovery rate for the tested 40 compounds of this new SPE method was 87%.

  18. New sorbent materials for selective extraction of cocaine and benzoylecgonine from human urine samples.

    Science.gov (United States)

    Bujak, Renata; Gadzała-Kopciuch, Renata; Nowaczyk, Alicja; Raczak-Gutknecht, Joanna; Kordalewska, Marta; Struck-Lewicka, Wiktoria; Waszczuk-Jankowska, Małgorzata; Tomczak, Ewa; Kaliszan, Michał; Buszewski, Bogusław; Markuszewski, Michał J

    2016-02-20

    An increase in cocaine consumption has been observed in Europe during the last decade. Benzoylecgonine, as a main urinary metabolite of cocaine in human, is so far the most reliable marker of cocaine consumption. Determination of cocaine and its metabolite in complex biological samples as urine or blood, requires efficient and selective sample pretreatment. In this preliminary study, the newly synthesized sorbent materials were proposed for selective extraction of cocaine and benzoylecgonine from urine samples. Application of these sorbent media allowed to determine cocaine and benzoylecgonine in urine samples at the concentration level of 100ng/ml with good recovery values as 81.7%±6.6 and 73.8%±4.2, respectively. The newly synthesized materials provided efficient, inexpensive and selective extraction of both cocaine and benzoylecgonine from urine samples, which can consequently lead to an increase of the sensitivity of the current available screening diagnostic tests. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

    Hingorani, S.B.; Sathe, A.P.

    1991-01-01

    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 90 Sr through its daughter 90 Y 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

  20. Porphyrin-based magnetic nanocomposites for efficient extraction of polycyclic aromatic hydrocarbons from water samples.

    Science.gov (United States)

    Yu, Jing; Zhu, Shukui; Pang, Liling; Chen, Pin; Zhu, Gang-Tian

    2018-03-09

    Stable and reusable porphyrin-based magnetic nanocomposites were successfully synthesized for efficient extraction of polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. Meso-Tetra (4-carboxyphenyl) porphyrin (TCPP), a kind of porphyrin, can connect the copolymer after amidation and was linked to Fe 3 O 4 @SiO 2 magnetic nanospheres via cross-coupling. Several characteristic techniques such as field emission scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Fourier transform infrared spectrometry, vibrating sample magnetometry and a tensiometer were used to characterize the as-synthesized materials. The structure of the copolymer was similar to that of graphene, possessing sp 2 -conjugated carbon rings, but with an appropriate amount of delocalized π-electrons giving rise to the higher extraction efficiency for heavy PAHs without sacrificing the performance in the extraction of light PAHs. Six extraction parameters, including the TCPP:Fe 3 O 4 @SiO 2 (m:m) ratio, the amount of adsorbents, the type of desorption solvent, the desorption solvent volume, the adsorption time and the desorption time, were investigated. After the optimization of extraction conditions, a comparison of the extraction efficiency of Fe 3 O 4 @SiO 2 -TCPP and Fe 3 O 4 @SiO 2 @GO was carried out. The adsorption mechanism of TCPP to PAHs was studied by first-principles density functional theory (DFT) calculations. Combining experimental and calculated results, it was shown that the π-π stacking interaction was the main adsorption mechanism of TCPP for PAHs and that the amount of delocalized π-electrons plays an important role in the elution process. Under the optimal conditions, Fe 3 O 4 @SiO 2 -porphyrin showed good precision in intra-day (<8.9%) and inter-day (<13.0%) detection, low method detection limits (2-10 ng L -1 ), and wide linearity (10-10000 ng L -1 ). The method was applied to simultaneous analysis of 15 PAHs with

  1. 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...... that the system entails many advantages such as being fully automated, and besides being characterised by rapidity, ease of operation and robustness, it is less prone to risks of contamination and personal errors as encountered in traditional batch systems. Moreover, improvement of the precision and accuracy...... of the chemical fractionation of metal in solids as compared with previous reports are obtained. The system ensures that extraction is performed at designated pH values. Variation of sample weight to column volume ratios do not affect the amounts of extractable metals, nor do extraction flow rates ranging from 50...

  2. Dioxin emission factors for automobiles from tunnel air sampling in Northern Taiwan.

    Science.gov (United States)

    Chang, Moo Been; Chang, Shu Hao; Chen, Yuan Wu; Hsu, Hsuan Chien

    2004-06-05

    This study measured PCDD/F concentrations in tunnel air and vehicle exhaust. The ambient air samples were collected with air samplers (Tisch PS-1) complying with USEPA TO-9A. The results indicate that the tunnel air had a PCDD/F TEQ concentration about two times as high as that of outside air (47.3 and 57.1 fg-I-TEQ/m3 for tunnel air vs. 37.1 fg-I-TEQ/m3 and 23.3 fg-I-TEQ/m3 for outside air, respectively). This provides the direct evidence that PCDD/F compounds are emitted from the combustion processes in gasoline- and diesel-fueled engines. According to the tunnel study, the emission factors ranged from 5.83 to 59.2 pg I-TEQ/km for gasoline vehicles and 23.32 to 236.65 pg I-TEQ/km of diesel vehicles. This indicates that the dioxin emission factor in Taiwan is lower than that measured in USA, Norway and Germany. When the speed of the diesel vehicle was set at 40 km/h, the dioxin concentration emitted from diesel vehicle was 278 pg/m3 (6.27 pg-I-TEQ/m3) from tailpipe testing. However, when the diesel vehicle was idled, the dioxin concentration increased greatly to 4078 pg/m3 (41.9 pg-I-TEQ/m3). From the results of tunnel air sampling, the PCDD/Fs emission from automobiles in Taiwan was estimated as 3.69 g I-TEQ per year. Copryright 2003 Elsevier B.V.

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

    International Nuclear Information System (INIS)

    Kohara, Eri; Muronoi, Naohiro

    2015-01-01

    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. Simple and rapid measurement of α-rays on smear samples using air luminescence

    International Nuclear Information System (INIS)

    Takiue, M.

    1980-01-01

    The α-activity collected on smear samples has been measured indirectly using an air luminescence counting method and a liquid scintillation spectrometer. In this method, air luminescence, attributed to the fluorescence emitted by nitrogen molecules excited by α-rays in air, serves to detect α-rays. Thus, sample preparation and α-ray measurement are simple and rapid, and moreover, no radioactive waste solution is produced. Taking into account a low background and a counting efficiency between 10 and 20%, it is estimated that the detectable limit for α-ray measurement is about 1 x 10 -7 μCi/cm 2 for loose contamination. This method is convenient to use in the routine analysis of α-ray-emitting nuclides on smear paper. (author)

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

    International Nuclear Information System (INIS)

    McGuire, S.; Hickey, E.E.; Knox, W.

    1991-01-01

    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

  6. Distribution of Gas Phase Polycyclic Aromatic Hydrocarbons (PAHs in Selected Indoor and Outdoor Air Samples of Malaysia: a Case Study in Serdang, Selangor and Bachang, Malacca

    Directory of Open Access Journals (Sweden)

    Haris Hafizal Abd Hamid

    2017-07-01

    Full Text Available Distribution of 10 polycyclic aromatic hydrocarbons (PAHs in the gas phase of air from selected indoor and outdoor areas of Selangor and Malacca, Malaysia has been investigated. A locally designed Semi Permeable Membrane Device (SPMD was applied for passive air sampling for 37 days at selected locations. Cleanup was carried out with Gas Purge - Micro Syringe Extraction (GP-MSE and the final analysis was using Gas Chromatography-Mass Spectrometry (GC-MS. In this study, 6 indoor and 12 outdoor locations were selected for air sampling. A total of 10 compounds of PAHs (Ʃ10PAHs were determined in the range of 0.218 ng/m3 - 1.692 ng/m3 and 0.378 ng/m3 - 1.492 ng/m3 in outdoor and indoor samples respectively. In the outdoor samples, locations such as near a petrol station and heavy traffic showed the maximum levels of Ʃ10PAHs, while rooftop samples showed the lowest Ʃ10PAHs. The distribution of gas phase Ʃ10PAHs was influenced by vehicular emission. Low molecular weight (LMW compounds (2-3 rings were dominant in all samples (>70% indicating that SPMD has successfully sampled the gas phase of the air.

  7. Evaluation and optimization of DNA extraction and purification procedures for soil and sediment samples.

    Science.gov (United States)

    Miller, D N; Bryant, J E; Madsen, E L; Ghiorse, W C

    1999-11-01

    We compared and statistically evaluated the effectiveness of nine DNA extraction procedures by using frozen and dried samples of two silt loam soils and a silt loam wetland sediment with different organic matter contents. The effects of different chemical extractants (sodium dodecyl sulfate [SDS], chloroform, phenol, Chelex 100, and guanadinium isothiocyanate), different physical disruption methods (bead mill homogenization and freeze-thaw lysis), and lysozyme digestion were evaluated based on the yield and molecular size of the recovered DNA. Pairwise comparisons of the nine extraction procedures revealed that bead mill homogenization with SDS combined with either chloroform or phenol optimized both the amount of DNA extracted and the molecular size of the DNA (maximum size, 16 to 20 kb). Neither lysozyme digestion before SDS treatment nor guanidine isothiocyanate treatment nor addition of Chelex 100 resin improved the DNA yields. Bead mill homogenization in a lysis mixture containing chloroform, SDS, NaCl, and phosphate-Tris buffer (pH 8) was found to be the best physical lysis technique when DNA yield and cell lysis efficiency were used as criteria. The bead mill homogenization conditions were also optimized for speed and duration with two different homogenizers. Recovery of high-molecular-weight DNA was greatest when we used lower speeds and shorter times (30 to 120 s). We evaluated four different DNA purification methods (silica-based DNA binding, agarose gel electrophoresis, ammonium acetate precipitation, and Sephadex G-200 gel filtration) for DNA recovery and removal of PCR inhibitors from crude extracts. Sephadex G-200 spin column purification was found to be the best method for removing PCR-inhibiting substances while minimizing DNA loss during purification. Our results indicate that for these types of samples, optimum DNA recovery requires brief, low-speed bead mill homogenization in the presence of a phosphate-buffered SDS-chloroform mixture, followed

  8. ENVIRONMENTAL SAMPLING USING LOCATION SPECIFIC AIR MONITORING IN BULK HANDLING FACILITIES

    Energy Technology Data Exchange (ETDEWEB)

    Sexton, L.; Hanks, D.; Degange, J.; Brant, H.; Hall, G.; Cable-Dunlap, P.; Anderson, B.

    2011-06-07

    Since the introduction of safeguards strengthening measures approved by the International Atomic Energy Agency (IAEA) Board of Governors (1992-1997), international nuclear safeguards inspectors have been able to utilize environmental sampling (ES) (e.g. deposited particulates, air, water, vegetation, sediments, soil and biota) in their safeguarding approaches at bulk uranium/plutonium handling facilities. Enhancements of environmental sampling techniques used by the IAEA in drawing conclusions concerning the absence of undeclared nuclear materials or activities will soon be able to take advantage of a recent step change improvement in the gathering and analysis of air samples at these facilities. Location specific air monitoring feasibility tests have been performed with excellent results in determining attribute and isotopic composition of chemical elements present in an actual test-bed sample. Isotopic analysis of collected particles from an Aerosol Contaminant Extractor (ACE) collection, was performed with the standard bulk sampling protocol used throughout the IAEA network of analytical laboratories (NWAL). The results yielded bulk isotopic values expected for the operations. Advanced designs of air monitoring instruments such as the ACE may be used in gas centrifuge enrichment plants (GCEP) to detect the production of highly enriched uranium (HEU) or enrichments not declared by a State. Researchers at Savannah River National Laboratory in collaboration with Oak Ridge National Laboratory are developing the next generation of ES equipment for air grab and constant samples that could become an important addition to the international nuclear safeguards inspector's toolkit. Location specific air monitoring to be used to establish a baseline environmental signature of a particular facility employed for comparison of consistencies in declared operations will be described in this paper. Implementation of air monitoring will be contrasted against the use of smear

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

    International Nuclear Information System (INIS)

    Olsen, P.A.

    1995-01-01

    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

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

    International Nuclear Information System (INIS)

    BAUMANN, B.L.

    2003-01-01

    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

  11. Probe sampling measurements and modeling of nitric oxide formation in ethane + air flames

    NARCIS (Netherlands)

    Dyakov, I.V.; Ruyck, de J.; Konnov, A.A.

    2007-01-01

    Burning velocity and probe sampling measurements of the concentrations of O2, CO2, CO and NO in the post-flame zone of ethane + air flames are reported. The heat flux method was used for stabilization of laminar, premixed, non-stretched flames on a perforated plate burner at 1 atm. Axial profiles of

  12. The sampling of sulfur dioxide in air with impregnated filter paper

    NARCIS (Netherlands)

    Huygen, C.

    1963-01-01

    A method is suggested for the sampling of sulfur dioxide in air with impregnated filter paper instead of bubblers. The best aqueous impregnating solution contained potassium hydroxide with glycerol or triethanolamine. The possibilities and limitations of the method are discussed. High collection

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

    International Nuclear Information System (INIS)

    Olivier, A.; Tenailleau, L.; Baron, Y.; Maro, D.

    2004-01-01

    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 Na 2 CO 3 . In the first method the Na 2 CO 3 solution is mixed with a liquid scintillate and is directly analysed by liquid scintillation counting (LSC). The detection limit is approximately 1 Bq/m 3 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/m 3 of air samples). In the third method, Na 2 CO 3 is precipitated into CaCO 3 in presence of CaCl 2 . CaCO 3 is then analysed by LSC. This method appear to be the most appropriate, the detection limit is 0.05 Bq/m 3 of air samples. (author)

  14. Automated CO2 extraction from air for clumped isotope analysis in the atmo- and biosphere

    Science.gov (United States)

    Hofmann, Magdalena; Ziegler, Martin; Pons, Thijs; Lourens, Lucas; Röckmann, Thomas

    2015-04-01

    The conventional stable isotope ratios 13C/12C and 18O/16O in atmospheric CO2 are a powerful tool for unraveling the global carbon cycle. In recent years, it has been suggested that the abundance of the very rare isotopologue 13C18O16O on m/z 47 might be a promising tracer to complement conventional stable isotope analysis of atmospheric CO2 [Affek and Eiler, 2006; Affek et al. 2007; Eiler and Schauble, 2004; Yeung et al., 2009]. Here we present an automated analytical system that is designed for clumped isotope analysis of atmo- and biospheric CO2. The carbon dioxide gas is quantitatively extracted from about 1.5L of air (ATP). The automated stainless steel extraction and purification line consists of three main components: (i) a drying unit (a magnesium perchlorate unit and a cryogenic water trap), (ii) two CO2 traps cooled with liquid nitrogen [Werner et al., 2001] and (iii) a GC column packed with Porapak Q that can be cooled with liquid nitrogen to -30°C during purification and heated up to 230°C in-between two extraction runs. After CO2 extraction and purification, the CO2 is automatically transferred to the mass spectrometer. Mass spectrometric analysis of the 13C18O16O abundance is carried out in dual inlet mode on a MAT 253 mass spectrometer. Each analysis generally consists of 80 change-over-cycles. Three additional Faraday cups were added to the mass spectrometer for simultaneous analysis of the mass-to-charge ratios 44, 45, 46, 47, 48 and 49. The reproducibility for δ13C, δ18O and Δ47 for repeated CO2 extractions from air is in the range of 0.11o (SD), 0.18o (SD) and 0.02 (SD)o respectively. This automated CO2 extraction and purification system will be used to analyse the clumped isotopic signature in atmospheric CO2 (tall tower, Cabauw, Netherlands) and to study the clumped isotopic fractionation during photosynthesis (leaf chamber experiments) and soil respiration. References Affek, H. P., Xu, X. & Eiler, J. M., Geochim. Cosmochim. Acta 71, 5033

  15. Surgical Emphysema: A Rare Complication of a Simple Surgical Dental Extraction Without the Use of an Air-Driven Rotor.

    Science.gov (United States)

    Gowans, Keegan; Patel, Muneer; Lewis, Khari

    2017-03-01

    Surgical emphysema is a rare complication of dental extractions, often associated with the use of high-speed air rotors. This report describes a case of extensive surgical emphysema following a simple surgical extraction of a LL6 under local anaesthetic. There was no use of air-driven handpieces during the procedure. The patient developed extensive surgical emphysema bi-laterally in both cervical neck and facial planes. After prophylactic antibiotics with careful monitoring in a secondary care setting, the patient made a full unremarkable recovery. Clinical relevance: Simple extraction of teeth is a procedure carried out daily by most general dental practitioners. However, the risk of surgical emphysema without the use of high-speed air rotors or instruments using pressurized air/water is not well known or documented.

  16. Dispersive liquid-liquid microextraction coupled with magnetic nanoparticles for extraction of zearalenone in wheat samples

    Directory of Open Access Journals (Sweden)

    Mitra Amoli-Diva

    2017-01-01

    Full Text Available A new, sensitive and fast dispersive liquid-liquid microextraction (DLLME coupled with micro-solid phase extraction (μ-SPE was developed for determination of zearalenone (ZEN in wheat samples. The DLLME was performed using acetonitrile/water (80:20 v/v as the disperser solvent and 1-octanol as the extracting solvent.  The acetonitrile/water (80:20 v/v solvent was also used to extract ZEN from solid wheat matrix, and was directly applied as the disperser solvent for DLLME process. Additionally, hydrophobic oleic-acid-modified magnetic nanoparticles were used in μ-SPE approach to retrieve the analyte from the DLLME step. So, the method uses high surface area and strong magnetism properties of these nanoparticles to avoid time-consuming column-passing processes in traditional SPE. Main parameters affecting the extraction efficiency and signal enhancement were investigated and optimized. Under the optimum conditions, the calibration curve showed a good linearity in the range of 0.1-500 μg kg−1 (R2=0.9996 with low detection limit of 83 ng g−1. The intra-day and inter-day precisions (as RSD % in the range of 2.6-4.3 % and high recoveries ranging from 91.6 to 99.1 % were obtained. The pre-concentration factor was 3. The method is simple, inexpensive, accurate and remarkably free from interference effects.

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

    International Nuclear Information System (INIS)

    Montes, R.; Rodriguez, I.; Rubi, E.; Bollain, M.H.; Cela, R.

    2007-01-01

    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

  18. Antimicrobial potential and phyto chemical analysis of different solvent extracted samples of viola pilosa

    International Nuclear Information System (INIS)

    Bakht, J.; Panni, M. K.; Shafi, M.

    2017-01-01

    Investigation of susceptibility of medicinal plants for bacterial pathogens is significant for suitable choice of treatment. Different solvent extracted samples of Viola pilosa shoots were investigated for their antibacterial and phytochemical activities using 0.5, 1 and 2 mg disc-1 concentrations. The antibacterial bioassay was assayed by disc diffusion method against six microbes. The studies revealed that ethyl acetate extracted fractions resulted in maximum growth inhibition of Pseudomonas aeruginosa and Staphylococcus aureus at 2000 mu g disc-1 concentration. Similarly, Xanthomonas campestris and Klebsiella pneumonia were found more susceptible to n-butanol extract. Maximum reduction in the activity of B. subtilis and E. coli was recorded by n-hexane fractions at two mg per disc. The most susceptible microbe was Pseudomonas aeruginosa. The results further revealed that all the tested microbes were found completely resistant to water extracted fractions at all the tested concentrations measuring 0% ZI. Phytochemical analysis showed the presence of various bioactive compounds including flavonoids, glycosides, proteins, fats, alkaloids, steroids, saponins, carbohydrates and tannins. (author)

  19. 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.

  20. Automated sample preparation using membrane microtiter extraction for bioanalytical mass spectrometry.

    Science.gov (United States)

    Janiszewski, J; Schneider, P; Hoffmaster, K; Swyden, M; Wells, D; Fouda, H

    1997-01-01

    The development and application of membrane solid phase extraction (SPE) in 96-well microtiter plate format is described for the automated analysis of drugs in biological fluids. The small bed volume of the membrane allows elution of the analyte in a very small solvent volume, permitting direct HPLC injection and negating the need for the time consuming solvent evaporation step. A programmable liquid handling station (Quadra 96) was modified to automate all SPE steps. To avoid drying of the SPE bed and to enhance the analytical precision a novel protocol for performing the condition, load and wash steps in rapid succession was utilized. A block of 96 samples can now be extracted in 10 min., about 30 times faster than manual solvent extraction or single cartridge SPE methods. This processing speed complements the high-throughput speed of contemporary high performance liquid chromatography mass spectrometry (HPLC/MS) analysis. The quantitative analysis of a test analyte (Ziprasidone) in plasma demonstrates the utility and throughput of membrane SPE in combination with HPLC/MS. The results obtained with the current automated procedure compare favorably with those obtained using solvent and traditional solid phase extraction methods. The method has been used for the analysis of numerous drug prototypes in biological fluids to support drug discovery efforts.

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

    International Nuclear Information System (INIS)

    Ometakova, J.

    2009-01-01

    We studied the use of an extraction chromatography for determination of 90 Sr 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 90 Sr. The water sample was used in radiochemical analysis for determination volume activity of 90 Sr. A radiochemical strontium yield was traced by using radionuclide 85 Sr. Samples were counted over a two week period to monitor the ingrowth of 90 Y on TRI CARB LSC counter. Samples were measured using an HPGe detector to find out 85 Sr recoveries at 514 keV line and they were counted directly by Cherenkov counting after the growth of 90 Y using TriCarb LSC counter after a two- week period (author)

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

    International Nuclear Information System (INIS)

    Litovitz, Aviva; Abramzon, Shmuel; Curtright, Aimee; Samaras, Constantine; Burger, Nicholas

    2013-01-01

    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, NO x 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 NO x . 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)

  3. Impact of natural gas extraction on PAH levels in ambient air.

    Science.gov (United States)

    Paulik, L Blair; Donald, Carey E; Smith, Brian W; Tidwell, Lane G; Hobbie, Kevin A; Kincl, Laurel; Haynes, Erin N; Anderson, Kim A

    2015-04-21

    Natural gas extraction, often referred to as "fracking," has increased rapidly in the U.S. in recent years. To address potential health impacts, passive air samplers were deployed in a rural community heavily affected by the natural gas boom. Samplers were analyzed for 62 polycyclic aromatic hydrocarbons (PAHs). Results were grouped based on distance from each sampler to the nearest active well. PAH levels were highest when samplers were closest to active wells. Additionally, PAH levels closest to natural gas activity were an order of magnitude higher than levels previously reported in rural areas. Sourcing ratios indicate that PAHs were predominantly petrogenic, suggesting that elevated PAH levels were influenced by direct releases from the earth. Quantitative human health risk assessment estimated the excess lifetime cancer risks associated with exposure to the measured PAHs. Closest to active wells, the risk estimated for maximum residential exposure was 2.9 in 10 000, which is above the U.S. EPA's acceptable risk level. Overall, risk estimates decreased 30% when comparing results from samplers closest to active wells to those farthest. This work suggests that natural gas extraction may be contributing significantly to PAHs in air, at levels that are relevant to human health.

  4. Impact of natural gas extraction on Pah levels in ambient air

    Science.gov (United States)

    Paulik, L. Blair; Donald, Carey E.; Smith, Brian W.; Tidwell, Lane G.; Hobbie, Kevin A.; Kincl, Laurel; Haynes, Erin N.; Anderson, Kim A.

    2015-01-01

    Natural gas extraction, often referred to as “fracking,” has increased rapidly in the U.S. in recent years. To address potential health impacts, passive air samplers were deployed in a rural community heavily affected by the natural gas boom. Samplers were analyzed for 62 polycyclic aromatic hydrocarbons (PAHs). Results were grouped based on distance from each sampler to the nearest active well. PAH levels were highest when samplers were closest to active wells. Additionally, PAH levels closest to natural gas activity were an order of magnitude higher than levels previously reported in rural areas. Sourcing ratios indicate that PAHs were predominantly petrogenic, suggesting that elevated PAH levels were influenced by direct releases from the earth. Quantitative human health risk assessment estimated the excess lifetime cancer risks associated with exposure to the measured PAHs. Closest to active wells, the risk estimated for maximum residential exposure was 2.9 in 10,000, which is above the U.S. EPA's acceptable risk level. Overall, risk estimates decreased 30% when comparing results from samplers closest to active wells to those farthest. This work suggests that natural gas extraction may be contributing significantly to PAHs in air, at levels that are relevant to human health. PMID:25810398

  5. Effect of DNA extraction and sample preservation method on rumen bacterial population.

    Science.gov (United States)

    Fliegerova, Katerina; Tapio, Ilma; Bonin, Aurelie; Mrazek, Jakub; Callegari, Maria Luisa; Bani, Paolo; Bayat, Alireza; Vilkki, Johanna; Kopečný, Jan; Shingfield, Kevin J; Boyer, Frederic; Coissac, Eric; Taberlet, Pierre; Wallace, R John

    2014-10-01

    The comparison of the bacterial profile of intracellular (iDNA) and extracellular DNA (eDNA) isolated from cow rumen content stored under different conditions was conducted. The influence of rumen fluid treatment (cheesecloth squeezed, centrifuged, filtered), storage temperature (RT, -80 °C) and cryoprotectants (PBS-glycerol, ethanol) on quality and quantity parameters of extracted DNA was evaluated by bacterial DGGE analysis, real-time PCR quantification and metabarcoding approach using high-throughput sequencing. Samples clustered according to the type of extracted DNA due to considerable differences between iDNA and eDNA bacterial profiles, while storage temperature and cryoprotectants additives had little effect on sample clustering. The numbers of Firmicutes and Bacteroidetes were lower (P rumen fluid subjected to the eDNA isolation procedure considerably changed the ratio of molecular operational taxonomic units (MOTUs) of Bacteroidetes and Firmicutes. Intracellular DNA extraction using bead-beating method from cheesecloth sieved rumen content mixed with PBS-glycerol and stored at -80 °C was found as the optimal method to study ruminal bacterial profile. Copyright © 2013 Elsevier Ltd. All rights reserved.

  6. High-throughput liquid-absorption air-sampling apparatus and methods

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2000-07-11

    A portable high-throughput liquid-absorption air sampler [PHTLAAS] has an asymmetric air inlet through which air is drawn upward by a small and light-weight centrifugal fan driven by a direct current motor that can be powered by a battery. The air inlet is so configured as to impart both rotational and downward components of motion to the sampled air near said inlet. The PHTLAAS comprises a glass tube of relatively small size through which air passes at a high rate in a swirling, highly turbulent motion, which facilitates rapid transfer of vapors and particulates to a liquid film covering the inner walls of the tube. The pressure drop through the glass tube is < 10 cm of water, usually < 5 cm of water. The sampler's collection efficiency is usually > 20% for vapors or airborne particulates in the 2--3 microns range and > 50% for particles larger than 4 microns. In conjunction with various analyzers, the PHTLAAS can serve to monitor a variety of hazardous or illicit airborne substances, such as lead-containing particulates, tritiated water vapor, biological aerosols, or traces of concealed drugs or explosives.

  7. High-throughput liquid-absorption air-sampling apparatus and methods

    Science.gov (United States)

    Zaromb, Solomon

    2000-01-01

    A portable high-throughput liquid-absorption air sampler [PHTLAAS] has an asymmetric air inlet through which air is drawn upward by a small and light-weight centrifugal fan driven by a direct current motor that can be powered by a battery. The air inlet is so configured as to impart both rotational and downward components of motion to the sampled air near said inlet. The PHTLAAS comprises a glass tube of relatively small size through which air passes at a high rate in a swirling, highly turbulent motion, which facilitates rapid transfer of vapors and particulates to a liquid film covering the inner walls of the tube. The pressure drop through the glass tube is 20% for vapors or airborne particulates in the 2-3.mu. range and >50% for particles larger than 4.mu.. In conjunction with various analyzers, the PHTLAAS can serve to monitor a variety of hazardous or illicit airborne substances, such as lead-containing particulates, tritiated water vapor, biological aerosols, or traces of concealed drugs or explosives.

  8. High-throughput liquid-absorption air-sampling apparatus and methods

    International Nuclear Information System (INIS)

    2000-01-01

    A portable high-throughput liquid-absorption air sampler [PHTLAAS] has an asymmetric air inlet through which air is drawn upward by a small and light-weight centrifugal fan driven by a direct current motor that can be powered by a battery. The air inlet is so configured as to impart both rotational and downward components of motion to the sampled air near said inlet. The PHTLAAS comprises a glass tube of relatively small size through which air passes at a high rate in a swirling, highly turbulent motion, which facilitates rapid transfer of vapors and particulates to a liquid film covering the inner walls of the tube. The pressure drop through the glass tube is 20% for vapors or airborne particulates in the 2--3 microns range and > 50% for particles larger than 4 microns. In conjunction with various analyzers, the PHTLAAS can serve to monitor a variety of hazardous or illicit airborne substances, such as lead-containing particulates, tritiated water vapor, biological aerosols, or traces of concealed drugs or explosives

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

    Energy Technology Data Exchange (ETDEWEB)

    Washington, A. L. II [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Peters, T. B. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    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.

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

    International Nuclear Information System (INIS)

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

    2014-01-01

    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

  11. 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.

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

    International Nuclear Information System (INIS)

    MULKEY, C.H.

    1999-01-01

    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

  13. Data Quality Objectives for Regulatory Requirements for Hazardous and Radioactive Air Emissions Sampling and Analysis; FINAL

    International Nuclear Information System (INIS)

    MULKEY, C.H.

    1999-01-01

    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

  14. Effect of DNA extraction methods and sampling techniques on the apparent structure of cow and sheep rumen microbial communities.

    Directory of Open Access Journals (Sweden)

    Gemma Henderson

    Full Text Available 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 considerably, depending on the DNA extraction method used. DNA extracts from nine extraction methods that passed these first quality criteria were evaluated further by quantitative PCR enumeration of microbial marker loci. Absolute microbial numbers, determined on the same rumen samples, differed by more than 100-fold, depending on the DNA extraction method used. The apparent compositions of the archaeal, bacterial, ciliate protozoal, and fungal communities in identical rumen samples were assessed using 454 Titanium pyrosequencing. Significant differences in microbial community composition were observed between extraction methods, for example in the relative abundances of members of the phyla Bacteroidetes and Firmicutes. Microbial communities in parallel samples collected from cows by oral stomach-tubing or through a rumen fistula, and in liquid and solid rumen digesta fractions, were compared using one of the DNA extraction methods. Community representations were generally similar, regardless of the rumen sampling technique used, but significant differences in the abundances of some microbial taxa such as the Clostridiales and the Methanobrevibacter ruminantium clade were observed. The apparent microbial community composition differed between rumen sample fractions, and Prevotellaceae were most abundant in the liquid fraction. DNA extraction methods that involved phenol-chloroform extraction and mechanical lysis steps tended to be more comparable. However

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

    International Nuclear Information System (INIS)

    Thakur, Smita S.; Yadav, J.R.; Rao, D.D.

    2012-01-01

    Internal exposure monitoring for alpha emitting radionuclides is carried out by bioassay samples analysis. For occupational radiation workers handling uranium in reprocessing or fuel fabrication facilities, there exists a possibility of internal exposure and urine assay is the preferred method for monitoring such exposure. Estimation of lower concentration of uranium at mBq level by alpha spectrometry requires preconcentration and its separation from large volume of urine sample. For this purpose, urine samples collected from non radiation workers were spiked with 232 U tracer at mBq level to estimate the chemical yield. Uranium in urine sample was pre-concentrated by calcium phosphate coprecipitation and separated by extraction chromatography resin U/TEVA. In this resin extractant was DAAP (Diamylamylphosphonate) supported on inert Amberlite XAD-7 support material. After co-precipitation, precipitate was centrifuged and dissolved in 10 ml of 1M Al(NO 3 ) 3 prepared in 3M HNO 3 . The sample thus prepared was loaded on extraction chromatography resin, pre-conditioned with 10 ml of 3M HNO 3 . Column was washed with 10 ml of 3M HNO 3 . Column was again rinsed with 5 ml of 9M HCl followed by 20 ml of 0.05 M oxalic acid prepared in 5M HCl to remove interference due to Th and Np if present in the sample. Uranium was eluted from U/TEVA column with 15 ml of 0.01M HCl. The eluted uranium fraction was electrodeposited on stainless steel planchet and counted by alpha spectrometry for 360000 sec. Approximate analysis time involved from sample loading to stripping is 2 hours when compared with the time involved of 3.5 hours by conventional ion exchange method. Seven urine samples from non radiation worker were radio chemically analyzed by this technique and the radiochemical yield was found in the range of 69-91 %. Efficacy of this method against conventional anion exchange technique earlier standardized at this laboratory is also being highlighted. Minimum detectable activity

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

    International Nuclear Information System (INIS)

    Barnett, J.M.

    2008-01-01

    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(reg s ign) 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

  17. Coacervative extraction as a green technique for sample preparation for the analysis of organic compounds.

    Science.gov (United States)

    Melnyk, A; Wolska, L; Namieśnik, J

    2014-04-25

    One of the present trends in analytical chemistry is miniaturization, which is one of the methods of green analytical chemistry application. A particular emphasis is placed on the elimination of the use of large amounts of organic solvents which are toxic and harmful to the environment, maintaining high efficiency of the extraction process, high recovery values and low values of quantification (LOQ) and detection (LOD) limits. These requirements are fulfilled by coacervative extraction (CAE) technique. In this review, theoretical aspects of the coacervation process are presented along with environmental and bioanalytical applications of this technique, its advantages, limitations and competitiveness with other techniques. Due to its simplicity and rapidity, CAE is an excellent alternative for currently practiced procedures of sample preparation for the analysis of organic compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Quantitative analysis of untreated oil samples in in-air PIXE

    International Nuclear Information System (INIS)

    Sera, K.; Goto, S.; Takahashi, C.; Saitoh, Y.

    2010-01-01

    The method of quantitative analysis of oil samples in in-air PIXE has been developed on the basis of a standard-free method. The components of the continuous X-rays originated from air and backing film can be exactly subtracted using a blank spectrum after normalization by the yields of Ar K-α X-rays. The method was developed using nine oil samples including standard oils and its accuracy was confirmed by comparing the results with those obtained by the internal-standard method. Validity of the method for practical oil samples was confirmed for various kinds of oils such as engine, machine and cooking oils. It was found that the method is effective for various kinds of oils whatever elements we designate as an index element. (author)

  19. Mathematical estimation of the level of microbial contamination on spacecraft surfaces by volumetric air sampling

    Science.gov (United States)

    Oxborrow, G. S.; Roark, A. L.; Fields, N. D.; Puleo, J. R.

    1974-01-01

    Microbiological sampling methods presently used for enumeration of microorganisms on spacecraft surfaces require contact with easily damaged components. Estimation of viable particles on surfaces using air sampling methods in conjunction with a mathematical model would be desirable. Parameters necessary for the mathematical model are the effect of angled surfaces on viable particle collection and the number of viable cells per viable particle. Deposition of viable particles on angled surfaces closely followed a cosine function, and the number of viable cells per viable particle was consistent with a Poisson distribution. Other parameters considered by the mathematical model included deposition rate and fractional removal per unit time. A close nonlinear correlation between volumetric air sampling and airborne fallout on surfaces was established with all fallout data points falling within the 95% confidence limits as determined by the mathematical model.

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

    International Nuclear Information System (INIS)

    Helsen, Lieve

    2005-01-01

    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

  1. Passive air sampling for persistent organic pollutants: Introductory remarks to the special issue

    International Nuclear Information System (INIS)

    Harner, Tom; Bartkow, Michael; Holoubek, Ivan; Klanova, Jana; Wania, Frank; Gioia, Rosalinda; Moeckel, Claudia; Sweetman, Andrew J.; Jones, Kevin C.

    2006-01-01

    There have been a number of developments in the need, design and use of passive air samplers (PAS) for persistent organic pollutants (POPs). This article is the first in a Special Issue of the journal to review these developments and some of the data arising from them. We explain the need and benefit of developing PAS for POPs, the different approaches that can be used, and highlight future developments and needs. - The context, needs and state-of-the-art of passive air sampling techniques for atmospheric persistent organic pollutants are discussed

  2. Actinide nuclides in environmental air and precipitation samples after the Chernobyl accident

    Energy Technology Data Exchange (ETDEWEB)

    Rosner, G.; Hoetzl, H.; Winkler, R. (Gesellschaft fuer Strahlen- und Umweltforschung mbH Muenchen (West Germany))

    1988-01-01

    The present paper describes the analysis of isotopes of uranium, neptunium, plutonium, americium and curium, in air and deposition samples taken at our laboratory site 10 km north of Munich, subsequent to the Chernobyl accident. Uranium-234, {sup 237}U, {sup 238}U, {sup 239}Np, {sup 238}Pu, {sup 239+240}Pu and {sup 242}Cm have been identified and upper limits of detection have been established for {sup 241}Am and {sup 244}Cm. Deposition and air concentration values are discussed. 12 refs., 1 fig., 2 tabs.

  3. The application of x-ray fluorescence spectrometry for multielemental analysis of air particulate samples

    International Nuclear Information System (INIS)

    Mohamad Rashid Mohamad Yusoff

    1986-01-01

    The performance of XRF spectrometer as a tool for multielemental analysis of air pollution samples was discussed. The non-destructive couples with multielemental nature of the technique satisfactory sensitivity for most elements were the most important characteristics for its popularity as a method of analysis. Thus, the technique promises a significant reduction in cost and time of analysis. As a result, more extensive and revealing air particulates survey should be possible, with consequent improvements in the discovery and positive identification of particulate pollution sources. (author)

  4. Membrane solid-phase extraction: Field application for isolation of polycyclic aromatic hydrocarbons from water samples

    International Nuclear Information System (INIS)

    Furlong, E.T.; Koleis, J.C.; Gates, P.M.

    1995-01-01

    Solid-phase extraction (SPE) membranes (M-SPE) were used to isolate microgram-per-liter to nanogram-per-liter quantities of polycyclic aromatic hydrocarbons (PAH) in 4- to 8-liter ground-water samples from a crude-oil-contaminated ground-water site near Bemidji, Minnesota. The M-SPE method was evaluated (1) under laboratory conditions using reagent water fortified with individual PAH at 1.23 micrograms per liter, and (2) at the Bemidji site. At the site, ground-water samples were processed and PAH isolated using a M-SPE system connected directly to the well pump. Following sample isolation, all M-SPE samples were extracted using dichloromethane and analyzed by gas chromatography-mass spectrometry with selected-ion monitoring. Operationally, the M-SPE method provided a simple means to isolate PAH on site at the wellhead, particularly for anoxic water samples. Acceptable recoveries, ranging from 56 to over 100 percent, were observed for lower molecular weight PAH (naphthalene to pyrene) using the M-SPE method. Recoveries using M-SPE were somewhat lower, but reproducible, for higher molecular weight PAH (chrysene to benzo[ghi]perylene), ranging from 18 to 56 percent. M-SPE provides the capability to collect and field isolate PAH from a sufficiently large number of samples to identify environmental chemical processes occurring at individual compound concentrations of 50 to 1,200 nanograms per liter. Using M-SPE, the potential for facilitated transport of PAH by in situ-derived dissolved organic carbon (DOC) was evaluated at the site. Plots comparing DOC and PAH concentrations indicate that PAH concentrations increase exponentially with linear increases in DOC concentrations

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

    International Nuclear Information System (INIS)

    Ocaña-González, Juan Antonio; Villar-Navarro, Mercedes; Ramos-Payán, María; Fernández-Torres, Rut; Bello-López, Miguel Angel

    2015-01-01

    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

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

    International Nuclear Information System (INIS)

    Ali, Z.M.; Soomro, A.S.A.

    2007-01-01

    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)

  7. 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.

  8. A newly developed grab sampling system for collecting stratospheric air over Antarctica

    Directory of Open Access Journals (Sweden)

    Hideyuki Honda

    1996-07-01

    Full Text Available In order to measure the concentrations of various minor constituents and their isotopic ratios in the stratosphere over Antarctica, a simple grab sampling system was newly developed. The sampling system was designed to be launched by a small number of personnel using a rubber balloon under severe experimental conditions. Special attention was paid to minimize the contamination of sample air, as well as to allow easy handling of the system. The sampler consisted mainly of a 15l sample container with electromagnetic and manual valves, control electronics for executing the air sampling procedures and sending the position and status information of the sampler to the ground station, batteries and a transmitter. All these parts were assembled in an aluminum frame gondola with a shock absorbing system for landing. The sampler was equipped with a turn-over mechanism of the gondola to minimize contamination from the gondola, as well as with a GPS receiver and a rawinsonde for its tracking. Total weight of the sampler was about 11kg. To receive, display and store the position and status data of the sampling system at the ground station, a simple data acquisition system with a portable receiver and a microcomputer was also developed. A new gas handling system was prepared to simplify the injection of He gas into the balloon. For air sampling experiments, three sampling systems were launched at Syowa Station (69°00′S, 39°35′E, Antarctica and then recovered on sea ice near the station on January 22 and 25,1996.

  9. Extraction and Determination of Crocin in Saffron Samples by Dispersive Liquid-Liquid Microextraction

    Directory of Open Access Journals (Sweden)

    Somayeh Heydari

    2016-11-01

    Full Text Available The main component responsible for color in saffron is crocin with the chemical formula of C44H64O24. Crocin is one of several carotenoids in nature that is soluble in water. This solubility is one of the reasons for its widespread usage as a colorant in food and medicine compared to other carotenoids. The coloring strength of saffron is one of the major factors that determine the quality of the saffron stigma. It will be evaluated with measuring of crocin. Microextraction is the newest and easiest method that can be successfully applied for the preconcentration and separation of crocin in saffron samples. The advantages of this method are faster, cheaper and easier analysis by UV-Vis spectrophotometry in measurement of crocin compared to the chromatographic analysis methods. The studies showed that the type and volume of disperser and extractant solvent have a significant effect on the efficiency of crocin extraction. In this work, acetone as the disperser solvent and dichlorometane as the extractant solvent were found to be suitable combinations. Under the optimal conditions, the calibration curve was linear in the range of 0.15-0.00001 μg mL-1 and the limit of detection (LOD was calculated based on 3 Sb/m (where, Sb and m are the standard deviation of the blank and slop ratio of the calibration curve respectively was 0.000008 μg mL-1. The procedure was applied to saffron samples and the good recovery percent for the saffron samples was obtained.

  10. 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. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. MPLEx: a method for simultaneous pathogen inactivation and extraction of samples for multi-omics profiling

    Energy Technology Data Exchange (ETDEWEB)

    Burnum-Johnson, Kristin E.; Kyle, Jennifer E.; Eisfeld, Amie J.; Casey, Cameron P.; Stratton, Kelly G.; Gonzalez, Juan F.; Habyarimana, Fabien; Negretti, Nicholas M.; Sims, Amy C.; Chauhan, Sadhana; Thackray, Larissa B.; Halfmann, Peter J.; Walters, Kevin B.; Kim, Young-Mo; Zink, Erika M.; Nicora, Carrie D.; Weitz, Karl K.; Webb-Robertson, Bobbie-Jo M.; Nakayasu, Ernesto S.; Ahmer, Brian; Konkel, Michael E.; Motin, Vladimir; Baric, Ralph S.; Diamond, Michael S.; Kawaoka, Yoshihiro; Waters, Katrina M.; Smith, Richard D.; Metz, Thomas O.

    2017-01-01

    The continued emergence and spread of infectious agents is of increasing concern due to increased population growth and the associated increased livestock production to meet food demands, increased urbanization and land-use changes, and greater travel. A systems biology approach to infectious disease research can significantly advance our understanding of host-pathogen relationships and facilitate the development of new therapies and vaccines. Molecular characterization of infectious samples outside of appropriate biosafety containment can only take place subsequent to pathogen inactivation. Herein, we describe a modified Folch extraction using chloroform/methanol that facilitates the molecular characterization of infectious samples by enabling simultaneous pathogen inactivation and extraction of proteins, metabolites, and lipids for subsequent mass spectrometry-based multi-omics measurements. This metabolite, protein and lipid extraction (MPLEx) method resulted in complete inactivation of bacterial and viral pathogens with exposed lipid membranes, including Yersinia pestis, Salmonella Typhimurium, and Campylobacter jejuni in pure culture, and Yersinia pestis, Campylobacter jejuni, West Nile, MERS-CoV, Ebola, and influenza H7N9 viruses in infection studies. Partial inactivation was observed for pathogens without exposed lipid membranes including 99.99% inactivation of community-associated methicillin-resistant Staphylococcus aureus, 99.6% and >99% inactivation of Clostridium difficile spores and vegetative cells, respectively, and 50% inactivation of adenovirus type 5. To demonstrate that MPLEx yields biomaterial of sufficient quality for subsequent multi-omics analyses, we highlight select proteomics, metabolomics and lipidomics data from human epithelial lung cells infected with wild-type and mutant forms of influenza H7N9. We believe that MPLEx will facilitate systems biology studies of infectious samples by enabling simultaneous pathogen inactivation and multi

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

    International Nuclear Information System (INIS)

    Zhang Huaiqin; Su Jingling; Yao Wanyuan; Liu Jinhua

    1989-01-01

    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 CaSO 4 (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/m 3 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/m 3 , as the sampling time being 6 hours. It weights only about 0.35 kg

  13. Ten-year mortality in a sample of an adult population in relation to air pollution

    Energy Technology Data Exchange (ETDEWEB)

    Krzyzanowski, M; Wojtyniak, B

    1982-12-01

    The 10-year mortality in a sample of adult inhabitants of Cracow, Poland, was analysed according to the levels of air pollution in the area of residence. Smoking habit and several social and occupational factors were considered in the analysis, which was carried out with the use of a multivariate method for categorical variables. Among men the main effect of air pollution was marginally significant, but there was a significant interaction between air pollution and smoking. Among women no such relation could be detected. Also, the association between female mortality and smoking was not significant. From other factors considered in the analysis, only exposure at work to dust, high humidity, and variable temperature was related to mortality in both men and women. In addition among women higher mortality was related to a lower level of education.

  14. Gel-aided sample preparation (GASP)--a simplified method for gel-assisted proteomic sample generation from protein extracts and intact cells.

    Science.gov (United States)

    Fischer, Roman; Kessler, Benedikt M

    2015-04-01

    We describe a "gel-assisted" proteomic sample preparation method for MS analysis. Solubilized protein extracts or intact cells are copolymerized with acrylamide, facilitating denaturation, reduction, quantitative cysteine alkylation, and matrix formation. Gel-aided sample preparation has been optimized to be highly flexible, scalable, and to allow reproducible sample generation from 50 cells to milligrams of protein extracts. This methodology is fast, sensitive, easy-to-use on a wide range of sample types, and accessible to nonspecialists. © 2014 The Authors. PROTEOMICS published by Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. 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

    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...

  16. Determination of colloidal and dissolved silver in water samples using colorimetric solid-phase extraction.

    Science.gov (United States)

    Hill, April A; Lipert, Robert J; Porter, Marc D

    2010-03-15

    The increase in bacterial resistance to antibiotics has led to resurgence in the use of silver as a biocidal agent in applications ranging from washing machine additives to the drinking water treatment system on the International Space Station (ISS). However, growing concerns about the possible toxicity of colloidal silver to bacteria, aquatic organisms and humans have led to recently issued regulations by the US EPA and FDA regarding the usage of silver. As part of an ongoing project, we have developed a rapid, simple method for determining total silver, both ionic (silver(I)) and colloidal, in 0.1-1mg/L aqueous samples, which spans the ISS potable water target of 0.3-0.5mg/L (total silver) and meets the US EPA limit of 0.1mg/L in drinking water. The method is based on colorimetric solid-phase extraction (C-SPE) and involves the extraction of silver(I) from water samples by passage through a solid-phase membrane impregnated with the colorimetric reagent DMABR (5-[4-(dimethylamino)benzylidene]rhodanine). Silver(I) exhaustively reacts with impregnated DMABR to form a colored compound, which is quantified using a handheld diffuse reflectance spectrophotometer. Total silver is determined by first passing the sample through a cartridge containing Oxone, which exhaustively oxidizes colloidal silver to dissolved silver(I). The method, which takes less than 2 min to complete and requires only approximately 1 mL of sample, has been validated through a series of tests, including a comparison with the ICP-MS analysis of a water sample from ISS that contained both silver(I) and colloidal silver. Potential earth-bound applications are also briefly discussed. Copyright (c) 2009 Elsevier B.V. All rights reserved.

  17. Air exposure and sample storage time influence on hydrogen release from tungsten

    Energy Technology Data Exchange (ETDEWEB)

    Moshkunov, K.A., E-mail: moshkunov@gmail.co [National Research Nuclear University ' MEPhI' , Kashirskoe sh. 31, 115409 Moscow (Russian Federation); Schmid, K.; Mayer, M. [Max-Planck-Institut fuer Plasmaphysik, EURATOM Association, Boltzmannstrasse 2, D-85748 Garching (Germany); Kurnaev, V.A.; Gasparyan, Yu.M. [National Research Nuclear University ' MEPhI' , Kashirskoe sh. 31, 115409 Moscow (Russian Federation)

    2010-09-30

    In investigations of hydrogen retention in first wall components the influence of the conditions of the implanted target storage prior to analysis and the storage time is often neglected. Therefore we have performed a dedicated set of experiments. The release of hydrogen from samples exposed to ambient air after irradiation was compared to samples kept in vacuum. For air exposed samples significant amounts of HDO and D{sub 2}O are detected during TDS. Additional experiments have shown that heavy water is formed by recombination of releasing D and H atoms with O on the W surface. This water formation can alter hydrogen retention results significantly, in particular - for low retention cases. In addition to the influence of ambient air exposure also the influence of storage time in vacuum was investigated. After implantation at 300 K the samples were stored in vacuum for up to 1 week during which the retained amount decreased significantly. The subsequently measured TDS spectra showed that D was lost from both the high and low energy peaks during storage at ambient temperature of {approx}300 K. An attempt to simulate this release from both peaks during room temperature storage by TMAP 7 calculations showed that this effect cannot be explained by conventional diffusion/trapping models.

  18. Air exposure and sample storage time influence on hydrogen release from tungsten

    International Nuclear Information System (INIS)

    Moshkunov, K.A.; Schmid, K.; Mayer, M.; Kurnaev, V.A.; Gasparyan, Yu.M.

    2010-01-01

    In investigations of hydrogen retention in first wall components the influence of the conditions of the implanted target storage prior to analysis and the storage time is often neglected. Therefore we have performed a dedicated set of experiments. The release of hydrogen from samples exposed to ambient air after irradiation was compared to samples kept in vacuum. For air exposed samples significant amounts of HDO and D 2 O are detected during TDS. Additional experiments have shown that heavy water is formed by recombination of releasing D and H atoms with O on the W surface. This water formation can alter hydrogen retention results significantly, in particular - for low retention cases. In addition to the influence of ambient air exposure also the influence of storage time in vacuum was investigated. After implantation at 300 K the samples were stored in vacuum for up to 1 week during which the retained amount decreased significantly. The subsequently measured TDS spectra showed that D was lost from both the high and low energy peaks during storage at ambient temperature of ∼300 K. An attempt to simulate this release from both peaks during room temperature storage by TMAP 7 calculations showed that this effect cannot be explained by conventional diffusion/trapping models.

  19. Air exposure and sample storage time influence on hydrogen release from tungsten

    Science.gov (United States)

    Moshkunov, K. A.; Schmid, K.; Mayer, M.; Kurnaev, V. A.; Gasparyan, Yu. M.

    2010-09-01

    In investigations of hydrogen retention in first wall components the influence of the conditions of the implanted target storage prior to analysis and the storage time is often neglected. Therefore we have performed a dedicated set of experiments. The release of hydrogen from samples exposed to ambient air after irradiation was compared to samples kept in vacuum. For air exposed samples significant amounts of HDO and D 2O are detected during TDS. Additional experiments have shown that heavy water is formed by recombination of releasing D and H atoms with O on the W surface. This water formation can alter hydrogen retention results significantly, in particular - for low retention cases. In addition to the influence of ambient air exposure also the influence of storage time in vacuum was investigated. After implantation at 300 K the samples were stored in vacuum for up to 1 week during which the retained amount decreased significantly. The subsequently measured TDS spectra showed that D was lost from both the high and low energy peaks during storage at ambient temperature of ˜300 K. An attempt to simulate this release from both peaks during room temperature storage by TMAP 7 calculations showed that this effect cannot be explained by conventional diffusion/trapping models.

  20. Solid phase extraction for the speciation and preconcentration of inorganic selenium in water samples: a review.

    Science.gov (United States)

    Herrero Latorre, C; Barciela García, J; García Martín, S; Peña Crecente, R M

    2013-12-04

    Selenium is an essential element for the normal cellular function of living organisms. However, selenium is toxic at concentrations of only three to five times higher than the essential concentration. The inorganic forms (mainly selenite and selenate) present in environmental water generally exhibit higher toxicity (up to 40 times) than organic forms. Therefore, the determination of low levels of different inorganic selenium species in water is an analytical challenge. Solid-phase extraction has been used as a separation and/or preconcentration technique prior to the determination of selenium species due to the need for accurate measurements for Se species in water at extremely low levels. The present paper provides a critical review of the published methods for inorganic selenium speciation in water samples using solid phase extraction as a preconcentration procedure. On the basis of more than 75 references, the different speciation strategies used for this task have been highlighted and classified. The solid-phase extraction sorbents and the performance and analytical characteristics of the developed methods for Se speciation are also discussed. Copyright © 2013 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

    Zal U'yun Wan Mahmood

    2002-01-01

    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 Ca 2+ and other major ions (Na + , Mg 2+ 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 85 Sr 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-HNO 3 method) - 279 ± 11 Bq/kg ash. (Author)

  2. Determination of air-loop volume and radon partition coefficient for measuring radon in water sample.

    Science.gov (United States)

    Lee, Kil Yong; Burnett, William C

    A simple method for the direct determination of the air-loop volume in a RAD7 system as well as the radon partition coefficient was developed allowing for an accurate measurement of the radon activity in any type of water. The air-loop volume may be measured directly using an external radon source and an empty bottle with a precisely measured volume. The partition coefficient and activity of radon in the water sample may then be determined via the RAD7 using the determined air-loop volume. Activity ratios instead of absolute activities were used to measure the air-loop volume and the radon partition coefficient. In order to verify this approach, we measured the radon partition coefficient in deionized water in the temperature range of 10-30 °C and compared the values to those calculated from the well-known Weigel equation. The results were within 5 % variance throughout the temperature range. We also applied the approach for measurement of the radon partition coefficient in synthetic saline water (0-75 ppt salinity) as well as tap water. The radon activity of the tap water sample was determined by this method as well as the standard RAD-H 2 O and BigBottle RAD-H 2 O. The results have shown good agreement between this method and the standard methods.

  3. Determination of air-loop volume and radon partition coefficient for measuring radon in water sample

    International Nuclear Information System (INIS)

    Kil Yong Lee; Burnett, W.C.

    2013-01-01

    A simple method for the direct determination of the air-loop volume in a RAD7 system as well as the radon partition coefficient was developed allowing for an accurate measurement of the radon activity in any type of water. The air-loop volume may be measured directly using an external radon source and an empty bottle with a precisely measured volume. The partition coefficient and activity of radon in the water sample may then be determined via the RAD7 using the determined air-loop volume. Activity ratios instead of absolute activities were used to measure the air-loop volume and the radon partition coefficient. In order to verify this approach, we measured the radon partition coefficient in deionized water in the temperature range of 10-30 deg C and compared the values to those calculated from the well-known Weigel equation. The results were within 5 % variance throughout the temperature range. We also applied the approach for measurement of the radon partition coefficient in synthetic saline water (0-75 ppt salinity) as well as tap water. The radon activity of the tap water sample was determined by this method as well as the standard RAD-H 2 O and BigBottle RAD-H 2 O. The results have shown good agreement between this method and the standard methods. (author)

  4. Rapid column extraction method for actinides and strontium in fish and other animal tissue samples

    International Nuclear Information System (INIS)

    Maxwell III, S.L.; Faison, D.M.

    2008-01-01

    The analysis of actinides and radiostrontium in animal tissue samples is very important for environmental monitoring. There is a need to measure actinide isotopes and strontium with very low detection limits in animal tissue samples, including fish, deer, hogs, beef and shellfish. A new, rapid separation method has been developed that allows the measurement of plutonium, neptunium, uranium, americium, curium and strontium isotopes in large animal tissue samples (100-200 g) with high chemical recoveries and effective removal of matrix interferences. This method uses stacked TEVA Resin R , TRU Resin R and DGA Resin R cartridges from Eichrom Technologies (Darien, IL, USA) that allows the rapid separation of plutonium (Pu), neptunium (Np), uranium (U), americium (Am), and curium (Cm) using a single multi-stage column combined with alphaspectrometry. Strontium is collected on Sr Resin R from Eichrom Technologies (Darien, IL, USA). After acid digestion and furnace heating of the animal tissue samples, the actinides and 89/90 Sr are separated using column extraction chromatography. This method has been shown to be effective over a wide range of animal tissue matrices. Vacuum box cartridge technology with rapid flow rates is used to minimize sample preparation time. (author)

  5. Decontamination of the extraction sample aisle at the West Valley Demonstration Project

    International Nuclear Information System (INIS)

    Vance, R.F.

    1986-09-01

    This report describes the decontamination and decommissioning (D and D) of the Extraction Sample Aisle (XSA) at the West Valley Demonstration Project. The XSA is one of several areas in the former reprocessing plant required for use in support of the solidification of high-level waste. The XSA contained three glove boxes which housed sample stations. It became radioactively contaminated during fuel reprocessing from 1966 to 1972. This report describes the work performed to accomplish the D and D objectives of removing existing piping and equipment and of reducing radiation and contamination levels, to As-Low-As-Reasonably-Achievable (ALARA) levels for the installation of new equipment. Also reported are pre- and post-radiological conditions, personnel exposure, radioactive waste volume collected, cost and schedule data, and lessons learned

  6. Preliminary evaluation of new polymer matrix for solid-phase extraction of nonylphenol from water samples.

    Science.gov (United States)

    Guerreiro, António; Soares, Ana; Piletska, Elena; Mattiasson, Bo; Piletsky, Sergey

    2008-03-31

    Molecularly imprinted (MIP) and blank polymers with affinity for nonylphenol were designed using computational modelling. Chromatographic tests demonstrated higher affinity of imprinted polymers towards the template nonylphenol as compared with blank polymers. The performance of both polymers in solid-phase extraction was however very similar. Both blank and imprinted polymers appeared to be suitable for the removal and pre-concentration of nonylphenol from contaminated water samples with 99% efficiency of the recovery. The commercial resins PH(EC) (Biotage) and C18 (Varian) tested in the same conditions used for comparative purposes had recovery rate <84%. The polymer capacity for nonylphenol was 231 mg g(-1) for blank and 228 mg g(-1) for MIP. The synthesised materials can have significance for sample pre-concentration and environmental analysis of this class of compounds.

  7. Environmental and emergency response capabilities of Los Alamos Scientific Laboratory's radiological air sampling program

    International Nuclear Information System (INIS)

    Gunderson, T.C.

    1980-05-01

    Environmental and emergency response radiological air sampling capabilities of the Environmental Surveillance Group at Los Alamos Scientific Laboratory are described. The air sampling program provides a supplementary check on the adequacy of containment and effluent controls, determines compliance with applicable protection guides and standards, and assesses potential environmental impacts on site environs. It also allows evaluation of potential individual and total population doses from airborne radionuclides that may be inhaled or serve as a source of external radiation. The environmental program is sufficient in scope to detect fluctuations and long-term trends in atmospheric levels of radioactivity originating onsite. The emergency response capabilities are designed to respond to both onsite unplanned releases and atmospheric nuclear tests

  8. Polyaniline-coated cigarette filters as a solid-phase extraction sorbent for the extraction and enrichment of polycyclic aromatic hydrocarbon in water samples.

    Science.gov (United States)

    Bunkoed, Opas; Rueankaew, Thanaschaphorn; Nurerk, Piyaluk; Kanatharana, Proespichaya

    2016-06-01

    Polyaniline coated cigarette filters were successfully synthesized and used as a solid-phase extraction sorbent for the extraction and preconcentration of polycyclic aromatic hydrocarbons in water samples. The polyaniline helped to enhance the adsorption ability of polycyclic aromatic hydrocarbons on the sorbent through π-π interactions. The high porosity and large surface area of the cigarette filters helped to reduce backpressure and can be operated with high sample flow rate without loss of extraction efficiency. The developed sorbent was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The parameters that affected the extraction efficiencies, i.e. polymerization time, type of desorption solvent and its volume, sample flow rate, sample volume, sample pH, ionic strength, and organic modifier were investigated. Under the optimal conditions, the method was linear over the range of 0.5-10 μg/L and a detection limit of 0.5 ng/L. This simple, rapid, and cost-effective method was successfully applied to the preconcentration of polycyclic aromatic hydrocarbons from water samples. The developed method provided a high enrichment factor with good extraction efficiency (85-98%) and a relative standard deviation <10%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. 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.)

  10. Development of a cloud-point extraction method for copper and nickel determination in food samples

    International Nuclear Information System (INIS)

    Azevedo Lemos, Valfredo; Selis Santos, Moacy; Teixeira David, Graciete; Vasconcelos Maciel, Mardson; Almeida Bezerra, Marcos de

    2008-01-01

    A new, simple and versatile cloud-point extraction (CPE) methodology has been developed for the separation and preconcentration of copper and nickel. The metals in the initial aqueous solution were complexed with 2-(2'-benzothiazolylazo)-5-(N,N-diethyl)aminophenol (BDAP) and Triton X-114 was added as surfactant. Dilution of the surfactant-rich phase with acidified methanol was performed after phase separation, and the copper and nickel contents were measured by flame atomic absorption spectrometry. The variables affecting the cloud-point extraction were optimized using a Box-Behnken design. Under the optimum experimental conditions, enrichment factors of 29 and 25 were achieved for copper and nickel, respectively. The accuracy of the method was evaluated and confirmed by analysis of the followings certified reference materials: Apple Leaves, Spinach Leaves and Tomato Leaves. The limits of detection expressed to solid sample analysis were 0.1 μg g -1 (Cu) and 0.4 μg g -1 (Ni). The precision for 10 replicate measurements of 75 μg L -1 Cu or Ni was 6.4 and 1.0, respectively. The method has been successfully applied to the analysis of food samples

  11. Development of ion imprinted polymers for the selective extraction of lanthanides from environmental samples

    International Nuclear Information System (INIS)

    Moussa, Manel

    2016-01-01

    The analysis of the lanthanide ions present at trace level in complex environmental matrices requires often a purification and preconcentration step. The solid phase extraction (SPE) is the most used sample preparation technique. To improve the selectivity of this step, Ion Imprinted Polymers (IIPs) can be used as SPE solid supports. The aim of this work was the development of IIPs for the selective extraction of lanthanide ions from environmental samples. In a first part, IIPs were prepared according to the trapping approach using 5,7-dichloroquinoline-8-ol as non-vinylated ligand. For the first time, the loss of the trapped ligand during template ion removal and sedimentation steps was demonstrated by HPLC-UV. Moreover, this loss was not repeatable, which led to a lack of repeatability of the SPE profiles. It was then demonstrated that the trapping approach is not appropriate for the IIPs synthesis. In a second part, IIPs were synthesized by chemical immobilization of methacrylic acid as vinylated monomer. The repeatability of the synthesis and the SPE protocol were confirmed. A good selectivity of the IIPs for all the lanthanide ions was obtained. IIPs were successfully used to selectively extract lanthanide ions from tap and river water. Finally, IIPs were synthesized by chemical immobilization of methacrylic acid and 4-vinylpyridine as functional monomers and either a light (Nd 3+ ) or a heavy (Er 3+ ) lanthanide ion as template. Both kinds of IIPs led to a similar selectivity for all lanthanide ions. Nevertheless, this selectivity can be modified by changing the nature and the pH of the washing solution used in the SPE protocol. (author)

  12. Testing sequential extraction methods for the analysis of multiple stable isotope systems from a bone sample

    Science.gov (United States)

    Sahlstedt, Elina; Arppe, Laura

    2017-04-01

    Stable isotope composition of bones, analysed either from the mineral phase (hydroxyapatite) or from the organic phase (mainly collagen) carry important climatological and ecological information and are therefore widely used in paleontological and archaeological research. For the analysis of the stable isotope compositions, both of the phases, hydroxyapatite and collagen, have their more or less well established separation and analytical techniques. Recent development in IRMS and wet chemical extraction methods have facilitated the analysis of very small bone fractions (500 μg or less starting material) for PO43-O isotope composition. However, the uniqueness and (pre-) historical value of each archaeological and paleontological finding lead to preciously little material available for stable isotope analyses, encouraging further development of microanalytical methods for the use of stable isotope analyses. Here we present the first results in developing extraction methods for combining collagen C- and N-isotope analyses to PO43-O-isotope analyses from a single bone sample fraction. We tested sequential extraction starting with dilute acid demineralization and collection of both collagen and PO43-fractions, followed by further purification step by H2O2 (PO43-fraction). First results show that bone sample separates as small as 2 mg may be analysed for their δ15N, δ13C and δ18OPO4 values. The method may be incorporated in detailed investigation of sequentially developing skeletal material such as teeth, potentially allowing for the investigation of interannual variability in climatological/environmental signals or investigation of the early life history of an individual.

  13. 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.

  14. 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.

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

    International Nuclear Information System (INIS)

    Olsen, P.A.

    1994-01-01

    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

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

    International Nuclear Information System (INIS)

    Butler, J.D.

    1995-01-01

    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

  17. 2017 Annual Terrestrial Sampling Plan for Sandia National Laboratories/New Mexico on Kirtland Air Force Base

    Energy Technology Data Exchange (ETDEWEB)

    Griffith, Stacy R. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2017-02-01

    The 2017 Annual Terrestrial Sampling Plan for Sandia National Laboratories/New Mexico on Kirtland Air Force Base has been prepared in accordance with the “Letter of Agreement Between Department of Energy, National Nuclear Security Administration, Sandia Field Office (DOE/NNSA/SFO) and 377th Air Base Wing (ABW), Kirtland Air Force Base (KAFB) for Terrestrial Sampling” (signed January 2017), Sandia National Laboratories, New Mexico (SNL/NM). The Letter of Agreement requires submittal of an annual terrestrial sampling plan.

  18. 2018 Annual Terrestrial Sampling Plan for Sandia National Laboratories/New Mexico on Kirtland Air Force Base.

    Energy Technology Data Exchange (ETDEWEB)

    Griffith, Stacy R. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2018-01-01

    The 2018 Annual Terrestrial Sampling Plan for Sandia National Laboratories/New Mexico on Kirtland Air Force Base has been prepared in accordance with the “Letter of Agreement Between Department of Energy, National Nuclear Security Administration, Sandia Field Office (DOE/NNSA/SFO) and 377th Air Base Wing (ABW), Kirtland Air Force Base (KAFB) for Terrestrial Sampling” (signed January 2017), Sandia National Laboratories, New Mexico (SNL/NM). The Letter of Agreement requires submittal of an annual terrestrial sampling plan.

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

    NARCIS (Netherlands)

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

    2009-01-01

    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

  20. Comparison of Passive and Active Air Sampling (PAAS) Methods for PCBs – A Pilot Study in New York City Schools

    Science.gov (United States)

    PCBs were used extensively in school building materials (caulk and lighting fixture ballasts) during the approximate period of 1950-1978. Most of the schools built nationwide during this period have not had indoor air sampling conducted for PCBs. Passive air sampling holds promi...

  1. Innovative sampling and extraction methods for the determination of nonsteroidal anti-inflammatory drugs in water.

    Science.gov (United States)

    Tanwar, Shivani; Di Carro, Marina; Magi, Emanuele

    2015-03-15

    Two different innovative approaches were used for the determination of nonsteroidal anti-inflammatory drugs (NSAIDs) in water: stir bar sorptive extraction (SBSE) and passive sampling, followed by electrospray ionization liquid chromatography-tandem mass spectrometry. SBSE was developed by comparing EG-Silicone and PDMS stir bars and optimizing main parameters to attain high preconcentration. Quantitative analysis was carried out by mass spectrometry in negative ionization mode and multiple reaction monitoring. The SBSE-LC-MS/MS method provided satisfactory figures of merit with LOD (7.5-71 ng L(-1)) and LOQ (22.5-213 ng L(-1)). The developed method was successfully applied to real samples collected from river water and wastewater effluents. The obtained results showed the presence of all analytes at trace levels, in a wide range of concentrations. The passive sampling approach was carried out by using Polar Organic Chemical Integrative Sampler (POCIS); samplers were deployed for 15 days in river and tap water, allowing to detect analytes at ultra-trace levels. Time-Weighted Average concentration of NSAIDs in river water was estimated in the range 0.33-0.46 ng L(-1), using the sampling rates previously obtained by means of a simple calibration system. Copyright © 2014 Elsevier B.V. All rights reserved.

  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. Occurrence of benzothiazole, benzotriazole and benzenesulfonamide derivates in outdoor air particulate matter samples and human exposure assessment.

    Science.gov (United States)

    Maceira, Alba; Marcé, Rosa Maria; Borrull, Francesc

    2018-02-01

    Benzothiazole (BTHs), benzotriazole (BTRs) and benzenesulfonamide (BSAs) derivates are high production volume chemicals and they are used in several industrial and household applications, therefore it is expected their occurrence in various environments, especially water and air. In this study we developed a method based on gas chromatography-mass spectrometry (GC-MS) combined with pressurised liquid extraction (PLE) to simultaneously determine four BTR, five BTH and six BSA derivates in the particulate matter (PM 10 ) of outdoor air samples collected in quartz fibre filters (QFFs). To the best of our knowledge, this is the first time these compounds have been determined in open ambient environments. Under optimised conditions, method recoveries at the lower and upper concentration levels (0.8 and 4.2 ng m -3 ) ranged from 70 to 120%, except for 1-H-benzothiazole and 2-chlorobenzothiazole, which were about 50%. The repeatability of the method was usually below 20% (n = 3, %RSD) for both concentration levels. This method enables the contaminants to be detected at pg m -3 concentration levels. Several samples from two different sites influenced by local industries showed that BTRs, followed by BTHs, were the most detected compounds, whereas BSAs were hardly found. The most frequently determined compounds were 1-H-benzothiazole, 2-chlorobenzothiazole, 1-H-benzotriazole, 2-hydroxibenzothiazole, 5,6-dimethyl-1-H-benzotriazole and the isomers 4- and 5-methyl-1-H-benzotriazole. With the concentrations found, the human exposure assessment and health risk characterization via ambient inhalation were also evaluated taking into account different subpopulation groups classified by age for the two sampling points. Copyright © 2017 Elsevier Ltd. All rights reserved.

  4. Airborne detection and quantification of swine influenza a virus in air samples collected inside, outside and downwind from swine barns.

    Directory of Open Access Journals (Sweden)

    Cesar A Corzo

    Full Text Available Airborne transmission of influenza A virus (IAV in swine is speculated to be an important route of virus dissemination, but data are scarce. This study attempted to detect and quantify airborne IAV by virus isolation and RRT-PCR in air samples collected under field conditions. This was accomplished by collecting air samples from four acutely infected pig farms and locating air samplers inside the barns, at the external exhaust fans and downwind from the farms at distances up to 2.1 km. IAV was detected in air samples collected in 3 out of 4 farms included in the study. Isolation of IAV was possible from air samples collected inside the barn at two of the farms and in one farm from the exhausted air. Between 13% and 100% of samples collected inside the barns tested RRT-PCR positive with an average viral load of 3.20E+05 IAV RNA copies/m³ of air. Percentage of exhaust positive air samples also ranged between 13% and 100% with an average viral load of 1.79E+04 RNA copies/m³ of air. Influenza virus RNA was detected in air samples collected between 1.5 and 2.1 Km away from the farms with viral levels significantly lower at 4.65E+03 RNA copies/m³. H1N1, H1N2 and H3N2 subtypes were detected in the air samples and the hemagglutinin gene sequences identified in the swine samples matched those in aerosols providing evidence that the viruses detected in the aerosols originated from the pigs in the farms under study. Overall our results indicate that pigs can be a source of IAV infectious aerosols and that these aerosols can be exhausted from pig barns and be transported downwind. The results from this study provide evidence of the risk of aerosol transmission in pigs under field conditions.

  5. 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

    2016-08-11

    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 (malachite green in various aqueous media, indicating its potential for online real-time monitoring of real life samples.

  6. Metal-organic framework based in-syringe solid-phase extraction for the on-site sampling of polycyclic aromatic hydrocarbons from environmental water samples.

    Science.gov (United States)

    Zhang, Xiaoqiong; Wang, Peiyi; Han, Qiang; Li, Hengzhen; Wang, Tong; Ding, Mingyu

    2018-04-01

    In-syringe solid-phase extraction is a promising sample pretreatment method for the on-site sampling of water samples because of its outstanding advantages of portability, simple operation, short extraction time, and low cost. In this work, a novel in-syringe solid-phase extraction device using metal-organic frameworks as the adsorbent was fabricated for the on-site sampling of polycyclic aromatic hydrocarbons from environmental waters. Trace polycyclic aromatic hydrocarbons were effectively extracted through the self-made device followed by gas chromatography with mass spectrometry analysis. Owing to the excellent adsorption performance of metal-organic frameworks, the analytes could be completely adsorbed during one adsorption cycle, thus effectively shortening the extraction time. Moreover, the adsorbed analytes could remain stable on the device for at least 7 days, revealing the potential of the self-made device for on-site sampling of degradable compounds in remote regions. The limit of detection ranged from 0.20 to 1.9 ng/L under the optimum conditions. Satisfactory recoveries varying from 84.4 to 104.5% and relative standard deviations below 9.7% were obtained in real samples analysis. The results of this study promote the application of metal-organic frameworks in sample preparation and demonstrate the great potential of in-syringe solid-phase extraction for the on-site sampling of trace contaminants in environmental waters. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. 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......-herd prevalence ⩾25%]. The results indicate that taking swabs of skin behind the ears (ten pools of five) was even more sensitive than taking nasal swabs (ten pools of five) at the herd level and detected significantly more positive samples. spa types t011, t034 and t4208 were observed. In 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....

  8. 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...

  9. 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...

  10. 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

    2016-01-01

    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.

  11. Carbon coated magnetic nanoparticles as a novel magnetic solid phase extraction adsorbent for simultaneous extraction of methamphetamine and ephedrine from urine samples.

    Science.gov (United States)

    Taghvimi, Arezou; Hamishehkar, Hamed

    2017-01-15

    This paper develops a highly selective, specific and efficient method for simultaneous determination of ephedrine and methamphetamine by a new carbon coated magnetic nanoparticles (C/MNPs) as a magnetic solid phase extraction (MSPE) adsorbent in biological urine medium. The characterization of synthesized magnetic nano adsorbent was completely carried out by various characterization techniques like Fourier transform infrared (FT-IR) spectroscopy, powder x-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). Nine important parameters influencing extraction efficiency including amount of adsorbent, amounts of sample volume, pH, type and amount of extraction organic solvent, time of extraction and desorption, agitation rate and ionic strength of extraction medium, were studied and optimized. Under optimized extraction conditions, a good linearity was observed in the concentration range of 100-2000ng/mL for ephedrine and 100-2500ng/mL for methamphetamine. Analysis of positive urine samples was carried out by proposed method with the recovery of 98.71 and 97.87% for ephedrine and methamphetamine, respectively. The results indicated that carbon coated magnetic nanoparticles could be applied in clinical and forensic laboratories for simultaneous determination of abused drugs in urine media. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Apparatus and method for maintaining multi-component sample gas constituents in vapor phase during sample extraction and cooling

    Science.gov (United States)

    Felix, Larry Gordon; Farthing, William Earl; Irvin, James Hodges; Snyder, Todd Robert

    2010-05-11

    A dilution apparatus for diluting a gas sample. The apparatus includes a sample gas conduit having a sample gas inlet end and a diluted sample gas outlet end, and a sample gas flow restricting orifice disposed proximate the sample gas inlet end connected with the sample gas conduit and providing fluid communication between the exterior and the interior of the sample gas conduit. A diluted sample gas conduit is provided within the sample gas conduit having a mixing end with a mixing space inlet opening disposed proximate the sample gas inlet end, thereby forming an annular space between the sample gas conduit and the diluted sample gas conduit. The mixing end of the diluted sample gas conduit is disposed at a distance from the sample gas flow restricting orifice. A dilution gas source connected with the sample gas inlet end of the sample gas conduit is provided for introducing a dilution gas into the annular space, and a filter is provided for filtering the sample gas. The apparatus is particularly suited for diluting heated sample gases containing one or more condensable components.

  13. Preparation of alumina-coated magnetite nanoparticle for extraction of trimethoprim from environmental water samples based on mixed hemimicelles solid-phase extraction.

    Science.gov (United States)

    Sun, Lei; Zhang, Chuanzhou; Chen, Ligang; Liu, Jun; Jin, Haiyan; Xu, Haoyan; Ding, Lan

    2009-04-13

    In this study, a new type of alumina-coated magnetite nanoparticles (Fe(3)O(4)/Al(2)O(3) NPs) modified by the surfactant sodium dodecyl sulfate (SDS) has been successfully synthesized and applied for extraction of trimethoprim (TMP) from environmental water samples based on mixed hemimicelles solid-phase extraction (MHSPE). The coating of alumina on Fe(3)O(4) NPs not only avoids the dissolving of Fe(3)O(4) NPs in acidic solution, but also extends their application without sacrificing their unique magnetization characteristics. Due to the high surface area of these new sorbents and the excellent adsorption capacity after surface modification by SDS, satisfactory concentration factor and extraction recoveries can be produced with only 0.1g Fe(3)O(4)/Al(2)O(3) NPs. Main factors affecting the adsolubilization of TMP such as the amount of SDS, pH value, standing time, desorption solvent and maximal extraction volume were optimized. Under the selected conditions, TMP could be quantitatively extracted. The recoveries of TMP by analyzing the four spiked water samples were between 67 and 86%, and the relative standard deviation (RSD) ranged from 2 to 6%. Detection and quantification limits of the proposed method were 0.09 and 0.24 microg L(-1), respectively. Concentration factor of 1000 was achieved using this method to extract 500 mL of different environmental water samples. Compared with conventional SPE methods, the advantages of this new Fe(3)O(4)/Al(2)O(3) NPs MHSPE method still include easy preparation and regeneration of sorbents, short times of sample pretreatment, high extraction yields, and high breakthrough volumes. It shows great analytical potential in preconcentration of organic compounds from large volume water samples.

  14. Micro-Sample Extraction System for In-Situ Missions to Planets, Planetary Satellites, and Primitive Bodies

    Data.gov (United States)

    National Aeronautics and Space Administration — We propose to develop a proof-of-concept Micro-Sample Extraction System (µSES) to enable microfluidic instruments, currently under development at NASA Goddard Space...

  15. Subcritical water extraction combined with molecular imprinting technology for sample preparation in the detection of triazine herbicides.

    Science.gov (United States)

    Zhao, Fengnian; Wang, Shanshan; She, Yongxin; Zhang, Chao; Zheng, Lufei; Jin, Maojun; Shao, Hua; Jin, Fen; Du, Xinwei; Wang, Jing

    2017-09-15

    A selective, environmentally friendly, and cost-effective sample extraction method based on a combination of subcritical water extraction (SWE) and molecularly imprinted solid-phase extraction (MISPE) was developed for the determination of eight triazine herbicides in soil samples by liquid chromatography-tandem mass spectrometry (LC-MS/MS). In SWE, the highest extraction yields of triazine herbicides were obtained under 150°C for 15min using 20% ethanol as the organic modifier. Addition of MIP during SWE increased the extraction efficiency, and using MIP as a selective SPE sorbent improved the enrichment capability. Soil samples were treated with the optimized extraction MIP/SWE-MISPE method and analyzed by LC-MS/MS. The novel technique was then applied to soil samples for the determination of triazine herbicides, and better recoveries (78.9%-101%) were obtained compared with using SWE-MISPE (30%-67%). Moreover, this newly developed method displayed good linearity (R 2 >0.99) and precision (2.7-9.8%), and low enough detection limits (0.4-3.3μgkg -1 ). This combination of SWE and MIP technology is a simple, effective and promising method to selectively extract class-specific compounds in complex samples. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2003-01-01

    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

  17. Ultrasound extraction and thin layer chromatography-flame ionization detection analysis of the lipid fraction in marine mucilage samples.

    Science.gov (United States)

    Mecozzi, M; Amici, M; Romanelli, G; Pietrantonio, E; Deluca, A

    2002-07-19

    This paper reports an analytical procedure based on ultrasound to extract lipids in marine mucilage samples. The experimental conditions of the ultrasound procedure (solvent and time) were identified by a FT-IR study performed on different standard samples of lipids and of a standard humic sample, before and after the sonication treatment. This study showed that diethyl ether was a more suitable solvent than methanol for the ultrasonic extraction of lipids from environmental samples because it allowed to minimize the possible oxidative modifications of lipids due to the acoustic cavitation phenomena. The optimized conditions were applied to the extraction of total lipid amount in marine mucilage samples and TLC-flame ionization detection analysis was used to identify the relevant lipid sub-fractions present in samples.

  18. High efficiency mixed species radioiodine air sampling, readout, and dose assessment system

    International Nuclear Information System (INIS)

    Distenfeld, C.; Klemish, J.

    1976-05-01

    Reactor accidents require monitoring to assess the impact to persons in the environment. This implies methods and apparatus to accurately and economically sample and evaluate possible released activity. The development of a prototype iodine air sampling system that can differentiate against noble gas activity and be evaluated by standard Civil Defense instrumentation is reported. The apparatus can efficiently (95 percent) collect organic or inorganic, particulate or gaseous radioiodine in concentrations below stable atmospheric iodine, and under severe ambient conditions. Response to noble fission gases was reduced to less than 4 x 10 -4 of an equal iodine airborne activity by heating the collector to approximately 100 0 C. Reliable sample size, +-5 percent, was achieved by using a simple air flow regulator. Thyroid dose commitment was mathematically and graphically related to the iodine isotope distribution expected in the environment and to the response of the Civil Defense CDV-700 instrument used to evaluate the sample. Sensitivity of the method allows dose assessment of 1 to 2 rads to a child's thyroid

  19. Radiological air monitoring and sample analysis research and development progress report

    International Nuclear Information System (INIS)

    1992-01-01

    Sponsored by a Department Of Energy (DOE) research and development grant, the State of Idaho INEL Oversight Program (OP) personnel designed an independent air monitoring system that provides detection of the presence of priority airborne contaminants potentially migrating beyond INEL boundaries. Initial locations for off-site ambient air monitoring stations were chosen in consultation with: DOE and NOAA reports; Mesodif modeling; review of the relevant literature; and communication with private contractors and experts in pertinent fields. Idaho State University (ISU) has initiated an Environmental Monitoring Program (EMP). The EMP provides an independent monitoring function as well as a training ground for students. Students learn research techniques dedicated to environmental studies and learn analytical skills and rules of compliance related to monitoring. ISU-EMP assisted OP in specific aspects of identifying optimum permanent monitoring station locations, and in selecting appropriate sample collection equipment for each station. The authorization to establish, prepare and install sampling devices on selected sites was obtained by OP personnel in conjunction with ISU-EMP personnel. All samples described in this program are collected by OP or ISU-EMP personnel and returned to the ISU for analysis. This report represents the summary of results of those samples collected and analyzed for radioactivity during the year of 1992

  20. An assessment of air sampling location for stack monitoring in nuclear facility

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Jung Bok [University of Science and Technology, Daejeon (Korea, Republic of); Kim, Tae Hyoung; Lee, Jong Il; Kim, Bong Hwan [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2017-06-15

    In this study, air sampling locations in the stack of the Advanced Fuel Science Building (AFSB) at the Korea Atomic Energy Research Institute (KAERI) were assessed according to the ANSI/HPS N13.1-1999 specification. The velocity profile, flow angle and 10 μm aerosol particle profile at the cross-section as functions of stack height L and stack diameter D (L/D) were assessed according to the sampling location criteria using COMSOL. The criteria for the velocity profile were found to be met at 5 L/D or more for the height, and the criteria for the average flow angle were met at all locations through this assessment. The criteria for the particle profile were met at 5 L/D and 9 L/D. However, the particle profile at the cross-section of each sampling location was found to be non-uniform. In order to establish uniformity of the particle profile, a static mixer and a perimeter ring were modeled, after which the degrees of effectiveness of these components were compared. Modeling using the static mixer indicated that the sampling locations that met the criteria for the particle profile were 5-10 L/D. When modeling using the perimeter ring, the sampling locations that met the criteria for particle profile were 5 L/D and 7-10 L/D. The criteria for the velocity profile and the average flow angle were also met at the sampling locations that met the criteria for the particle profile. The methodologies used in this study can also be applied during assessments of air sampling locations when monitoring stacks at new nuclear facilities as well as existing nuclear facilities.

  1. Ultrasound-assisted extraction and solid-phase extraction for the simultaneous determination of five amide herbicides in fish samples by gas chromatography with electron capture detection.

    Science.gov (United States)

    Qu, Zhipeng; Bai, Xiuzhi; Zhang, Ting; Yang, Zhaoguang

    2017-03-01

    An efficient sample extraction and clean-up method was developed for simultaneous determination of five amide herbicides (alachlor, acetochlor, propisochlor, metazachlor, and butachlor) in fish samples. The protocol consisted of ultrasound-assisted solvent extraction and solid-phase extraction clean-up. In detail, aliquots of homogenized fish flesh were thoroughly mixed with 20 mL of n-hexane and then extracted with ultrasonication for 40 min. Each sample was centrifuged and the supernatant was collected for the subsequent clean-up. For the sample preparation, the above supernatant was processed with a C 18 column with 3 mL of dichloromethane/n-hexane (1:1, v/v) as the eluant. Then the samples were analyzed by gas chromatography with electron capture detection. The correlation coefficients of the five calibration curves were 0.9976-0.9998 (n = 3). The limits of detection (S/N = 3, n = 11) and limits of quantification (S/N = 10, n = 11) were 0.19-0.42 and 0.63-1.39 μg/kg, respectively. The recoveries of this method were 71.2-92.6% with good precision (<4.7% relative standard deviations, n = 6). The developed method was successfully applied to monitor the five amide herbicides in fish samples collected from different cities. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Mass spectrometry of solid samples in open air using combined laser ionization and ambient metastable ionization

    International Nuclear Information System (INIS)

    He, X.N.; Xie, Z.Q.; Gao, Y.; Hu, W.; Guo, L.B.; Jiang, L.; Lu, Y.F.

    2012-01-01

    Mass spectrometry of solid samples in open air was carried out using combined laser ionization and metastable ionization time-of-flight mass spectrometry (LI-MI-TOFMS) in ambient environment for qualitative and semiquantitative (relative analyte information, not absolute information) analysis. Ambient metastable ionization using a direct analysis in realtime (DART) ion source was combined with laser ionization time-of-flight mass spectrometry (LI-TOFMS) to study the effects of combining metastable and laser ionization. A series of metallic samples from the National Institute of Standards and Technology (NIST 494, 495, 498, 499, and 500) and a pure carbon target were characterized using LI-TOFMS in open air. LI-MI-TOFMS was found to be superior to laser-induced breakdown spectroscopy (LIBS). Laser pulse energies between 10 and 200 mJ at the second harmonic (532 nm) of an Nd:YAG laser were applied in the experiment to obtain a high degree of ionization in plasmas. Higher laser pulse energy improves signal intensities of trace elements (such as Fe, Cr, Mn, Ni, Ca, Al, and Ag). Data were analyzed by numerically calculating relative sensitivity coefficients (RSCs) and limit of detections (LODs) from mass spectrometry (MS) and LIBS spectra. Different parameters, such as boiling point, ionization potential, RSC, LOD, and atomic weight, were shown to analyze the ionization and MS detection processes in open air.

  3. Solid phase extraction for sample preparation in trace analysis of ionogenic compounds by capillary isotachophoresis

    International Nuclear Information System (INIS)

    Hutta, M.; Kaniansky, D.; Simunicova, E.; Zelenska, V.; Madajova, V.; Siskova, A.

    1992-01-01

    Various sorbents recommended for solid phase extraction (SPE) in sample preparation procedures were studied for use in combination with capillary isotachophoresis (ITP). They were very efficient in achieving trace concentration levels (low ppb, i.e., low parts per 10 9 ) for different types of ITP analytes present in environmental and biological matrices. A macroporous carbon sorbent was convenient for sample preparation in ITP analysis of short chain fatty acids (C 4 -C 9 ) in drinking water. Chelating sorbents based on hydroxyalkyl methacrylate matrix with salicylate, thioglycolate and 8-hydroxyquinolinate functionalities were found to be very suitable for preconcentration of heavy metals with an inherent sample clean-up. An octadecyl-bonded silica sorbent enabled in ITP a photometric detection of γ-aminobutyrate (labeled with a 2,4,6-trinitrophenyl group) at concentrations considerably lower than required for the determination of this amino acid in cerebrospinal fluid (∼5*10 -8 mol/l). (author) 34 refs.; 3 figs.; 1 tab

  4. Incidence of two canals in extracted mandibular incisors teeth of Saudi Arabian samples

    Directory of Open Access Journals (Sweden)

    Khalid S Al-Fouzan

    2012-01-01

    Full Text Available Aim: The purpose of this in vitro study is to provide clinical data on the presence of the second canal in mandibular incisor teeth of Saudi Arabian Samples. Materials and Methods: Eighty extracted human mandibular incisors were collected from Saudi patients. The teeth were accessed by small round bur then placed in 5.25% sodium hypochlorite for 24 hours to dissolve the organic debris. Indian ink was injected inside the root canal systems under negative pressure. The teeth were decalcified in 5% nitric acid for three days then dehydrated in different concentrations of ethyl alcohol. Following the decalcification process, the teeth were cleared in methyl salicylate and evaluated according to Vertucci′s classification. Result: Fifty six of both mandibular central and lateral incisor teeth (70% had type I canal configuration (one main canal and one main apical foramen, while the remaining 30% of the sample (24 teeth had a type III canal configuration (two separate canals and merged into one canal before exiting the tooth through single apical foramen. Conclusion : The incidence of two canals in mandibular incisor teeth is about one third of the examined Saudi Arabian samples with no difference between the centrals and laterals. The clinician should deal with these teeth as if they have two canals unless it is proved otherwise.

  5. 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.

  6. Study on Solid Phase Extraction and Spectrophotometric Determination of Nickel in Waters and Biological Samples

    International Nuclear Information System (INIS)

    Hu, Qiufen; Yang, Guangyu; Huang, Zhangjie; Yin, Jiayuan

    2004-01-01

    A sensitive, selective and rapid method for the determination of nickel based on the rapid reaction of nickel(II) with QADMAA and the solid phase extraction of the Ni(II)-QADMAA chelate with C 18 membrane disks has been developed. In the presence of pH 6.0 buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with nickel to form a violet complex of a molar ratio of 1 : 2 (nickel to QADMAA). This chelate was enriched by solid phase extraction with C 18 membrane disks. An enrichment factor of 50 was obtained by elution of the chelates form the disks with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate was 1.32 x 10 5 L mol -1 cm -1 at 590 nm in the measured solution. Beer's law was obeyed in the range of 0.01-0.6 μg/mL. This method was applied to the determination of nickel in water and biological samples with good results

  7. Simultaneous multicopter-based air sampling and sensing of meteorological variables

    Science.gov (United States)

    Brosy, Caroline; Krampf, Karina; Zeeman, Matthias; Wolf, Benjamin; Junkermann, Wolfgang; Schäfer, Klaus; Emeis, Stefan; Kunstmann, Harald

    2017-08-01

    The state and composition of the lowest part of the planetary boundary layer (PBL), i.e., the atmospheric surface layer (SL), reflects the interactions of external forcing, land surface, vegetation, human influence and the atmosphere. Vertical profiles of atmospheric variables in the SL at high spatial (meters) and temporal (1 Hz and better) resolution increase our understanding of these interactions but are still challenging to measure appropriately. Traditional ground-based observations include towers that often cover only a few measurement heights at a fixed location. At the same time, most remote sensing techniques and aircraft measurements have limitations to achieve sufficient detail close to the ground (up to 50 m). Vertical and horizontal transects of the PBL can be complemented by unmanned aerial vehicles (UAV). Our aim in this case study is to assess the use of a multicopter-type UAV for the spatial sampling of air and simultaneously the sensing of meteorological variables for the study of the surface exchange processes. To this end, a UAV was equipped with onboard air temperature and humidity sensors, while wind conditions were determined from the UAV's flight control sensors. Further, the UAV was used to systematically change the location of a sample inlet connected to a sample tube, allowing the observation of methane abundance using a ground-based analyzer. Vertical methane gradients of about 0.3 ppm were found during stable atmospheric conditions. Our results showed that both methane and meteorological conditions were in agreement with other observations at the site during the ScaleX-2015 campaign. The multicopter-type UAV was capable of simultaneous in situ sensing of meteorological state variables and sampling of air up to 50 m above the surface, which extended the vertical profile height of existing tower-based infrastructure by a factor of 5.

  8. 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. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

  9. Determination of decamethylcyclopentasiloxane in air using commercial solid phase extraction cartridges.

    Science.gov (United States)

    Kierkegaard, Amelie; McLachlan, Michael S

    2010-05-21

    Decamethylcyclopentasiloxane (D(5)), a high production volume chemical used in personal care products, has been designated for regulation in Canada and is under review in the EU because of concerns about its persistence and potential for bioaccumulation in the environment. D(5) is a volatile compound expected to be found primarily in air, but there is little information on atmospheric concentrations due to the lack of sensitive analytical methods. Here a simple and sensitive method to determine D(5) in ambient air is presented. The challenge in the environmental analysis of D(5) is avoiding contamination. Our method is based on the high trapping efficiency of the sorbent Isolute ENV+, combined with a comparably high sampling rate. A small amount of sorbent (10 mg) is eluted in a small volume of n-hexane (0.1-0.6 mL), which is injected onto a GC/MS system without further processing. The simplicity of the method enables the use of a field blank for every sample to trace contamination. The method provides low limits of quantification (approximately 0.3 ng/m(3)), good repeatability and limited breakthrough (approximately 1%). By lowering the limit of quantification compared to published work by almost two orders of magnitude, it became possible to quantify D(5) in ambient air at locations remote from strong point sources. The concentrations at a rural Swedish site ranged from 0.7 to 8 ng/m(3) over a period of 4 months. 2010 Elsevier B.V. All rights reserved.

  10. Radiation damage of paper samples in in-air PIXE analysis

    International Nuclear Information System (INIS)

    Matsuyama, S.; Endo, H.; Ishii, K.; Yamazaki, H.; Tokai, Y.; Sugimoto, A.; Yamamoto, K.; Satoh, T.; Orihara, H.

    1999-01-01

    Degradation of paper caused by beam irradiation was investigated from a viewpoint of discoloration in PIXE analysis and its application to the paper samples of archaeology. Two types of paper (Japanese paper and fine quality paper) were tested in in-air PIXE analysis with 3 MeV protons. The degree of discoloration was quantitatively measured by the use of a colorimeter. The degree of discoloration was different for each tested paper and corresponded to the radiation dose of ions. It is resulted that even the in-air PIXE analysis should be carefully applied to archaeological treasures. Because discoloration of all tested paper decreased gradually at first but then increased after a few weeks. However, this phenomenon can be used to develop a technique of funny coloration. (author)

  11. Radiation damage of paper samples in in-air PIXE analysis

    Energy Technology Data Exchange (ETDEWEB)

    Matsuyama, S.; Endo, H.; Ishii, K.; Yamazaki, H.; Tokai, Y.; Sugimoto, A.; Yamamoto, K.; Satoh, T. [Department of Quantum Science and Energy Engineering, Tohoku University, Sendai, Miyagi (Japan); Orihara, H. [Tohoku Univ., Sendai (Japan). Cyclotron and Radioisotope Center

    1999-07-01

    Degradation of paper caused by beam irradiation was investigated from a viewpoint of discoloration in PIXE analysis and its application to the paper samples of archaeology. Two types of paper (Japanese paper and fine quality paper) were tested in in-air PIXE analysis with 3 MeV protons. The degree of discoloration was quantitatively measured by the use of a colorimeter. The degree of discoloration was different for each tested paper and corresponded to the radiation dose of ions. It is resulted that even the in-air PIXE analysis should be carefully applied to archaeological treasures. Because discoloration of all tested paper decreased gradually at first but then increased after a few weeks. However, this phenomenon can be used to develop a technique of funny coloration. (author)

  12. Molecularly imprinted solid-phase extraction of glutathione from urine samples

    International Nuclear Information System (INIS)

    Song, Renyuan; Hu, Xiaoling; Guan, Ping; Li, Ji; Zhao, Na; Wang, Qiaoli

    2014-01-01

    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 −1 . The relative standard deviations (RSDs) for 10 replicate detections of 50 mg·L −1 of glutathione were 5.76%, and the linear range of the calibration curve was 0.5 mg·L −1 to 200 mg·L −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

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

    International Nuclear Information System (INIS)

    Cong Khanh Huynh; Trinh Vu Duc

    2009-01-01

    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.

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

    International Nuclear Information System (INIS)

    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

  15. Optimization of pressurized liquid extraction (PLE) of dioxin-furans and dioxin-like PCBs from environmental samples.

    Science.gov (United States)

    Antunes, Pedro; Viana, Paula; Vinhas, Tereza; Capelo, J L; Rivera, J; Gaspar, Elvira M S M

    2008-05-30

    Pressurized liquid extraction (PLE) applying three extraction cycles, temperature and pressure, improved the efficiency of solvent extraction when compared with the classical Soxhlet extraction. Polychlorinated-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and dioxin-like PCBs (coplanar polychlorinated biphenyls (Co-PCBs)) in two Certified Reference Materials [DX-1 (sediment) and BCR 529 (soil)] and in two contaminated environmental samples (sediment and soil) were extracted by ASE and Soxhlet methods. Unlike data previously reported by other authors, results demonstrated that ASE using n-hexane as solvent and three extraction cycles, 12.4 MPa (1800 psi) and 150 degrees C achieves similar recovery results than the classical Soxhlet extraction for PCDFs and Co-PCBs, and better recovery results for PCDDs. ASE extraction, performed in less time and with less solvent proved to be, under optimized conditions, an excellent extraction technique for the simultaneous analysis of PCDD/PCDFs and Co-PCBs from environmental samples. Such fast analytical methodology, having the best cost-efficiency ratio, will improve the control and will provide more information about the occurrence of dioxins and the levels of toxicity and thereby will contribute to increase human health.

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

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Xiao Jin [Department of Environment and Climate Change, Environmental Forensic and Analytical Science Section, New South Wales (Australia); Department of Applied Chemistry, College of Chemical Engineering, Beijing University of Chemical Technology, Beijing (China); Wan, Pingyu [Department of Applied Chemistry, College of Chemical Engineering, Beijing University of Chemical Technology, Beijing (China); Foley, Roy [Department of Environment and Climate Change, Environmental Forensic and Analytical Science Section, New South Wales (Australia)

    2012-11-15

    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)

  17. 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)

    Yang, Xiao Jin; Wan, Pingyu; Foley, Roy

    2012-01-01

    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)

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

    International Nuclear Information System (INIS)

    Barnett, J.M.; Cullinan, Valerie I.; Barnett, Debra S.; Trang-Le, Truc LT; Bliss, Mary; Greenwood, Lawrence R.; Ballinger, Marcel Y.

    2009-01-01

    Since the mid-1980s, Pacific Northwest National Laboratory (PNNL) has used a value of 0.85 as the correction factor for self absorption of activity for particulate radioactive air samples collected from building exhaust for environmental monitoring. This value accounts for activity that cannot be detected by direct counting of alpha and beta particles. Emissions can be degraded or blocked by filter fibers for particles buried in the filter material or by inactive dust particles collected with the radioactive particles. These filters are used for monitoring air emissions from PNNL stacks for radioactive particles. This paper describes an effort to re-evaluate self-absorption effects in particulate radioactive air sample filters (Versapor(reg s ign) 3000, 47 mm diameter) used at PNNL. There were two methods used to characterize the samples. Sixty samples were selected from the archive for acid digestion to compare the radioactivity measured by direct gas-flow proportional counting of filters to the results obtained after acid digestion of the filter and counting again by gas-flow proportional detection. Thirty different sample filters were selected for visible light microscopy to evaluate filter loading and particulate characteristics. Mass-loading effects were also considered. Filter ratios were calculated by dividing the initial counts by the post-digestion counts with the expectation that post-digestion counts would be higher because digestion would expose radioactivity embedded in the filter in addition to that on top of the filter. Contrary to expectations, the post digestion readings were almost always lower than initial readings and averaged approximately half the initial readings for both alpha and beta activity. Before and after digestion readings appeared to be related to each other, but with a low coefficient of determination (R 2 ) value. The ratios had a wide range of values indicating that this method did not provide sufficient precision to quantify

  19. Determination of Zinc Ions in Environmental Samples by Dispersive Liquid- Liquid Micro Extraction and Atomic Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    F. Arabi

    2012-11-01

    Full Text Available In this work preconcentration of the Zn ions was investigated in water sample by Dispersive liquid- liquid micro extraction (DLLME using chloroform as an extraction solvent, methanol as a disperser solvent and 8-Hydroxyquinoline as a chelating agent. The determination of extracted ions was done by graphite furnace atomic absorption spectrometry. The influence of various analytical parameters including pH, extraction and disperser solvent type and volume and concentration of the chelating agent on the extraction efficiency of analyses was investigated. After extraction, the enrichment factor was 26 and the detection limit of the method was 0.0033 µg l-1 and the relative standard deviations (R.S.D for five determinations of 1 ng/ml Zn were 7.41%. 

  20. Microwave assisted aqua regia extraction of thallium from sediment and coal fly ash samples and interference free determination by continuum source ETAAS after cloud point extraction.

    Science.gov (United States)

    Meeravali, Noorbasha N; Madhavi, K; Kumar, Sunil Jai

    2013-01-30

    A simple cloud point extraction method is described for the separation and pre-concentration of thallium from the microwave assisted aqua regia extracts of sediment and coal fly ash samples. The method is based on the formation of extractable species of thallium and its interaction with hydrophobic solubilizing sites of Triton X-114 micelles in the presence of aqua regia and electrolyte NaCl. These interactions of micelles are used for extraction of thallium from a bulk aqueous phase into a small micelles-rich phase. The potential chloride interferences are eliminated effectively, which enabled interference free determination of thallium from aqua regia extracts using continuum source ETAAS. The parameters affecting the extraction process are optimized. Under the optimized conditions, pre-concentration factor and limit of detection are 40 and 0.2 ng g(-1), respectively. The recoveries are in the range of 95-102%. A characteristic mass, 13 pg was obtained. The accuracy of the method is verified by analyzing certified reference materials such as NIST 1633b coal fly ash, NIST 1944 marine sediment and GBW 07312 stream sediments. The results obtained are in good agreement with the certified values and method is also applied to real samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  1. Passive air sampling of polychlorinated biphenyls, organochlorine compounds, and polybrominated diphenyl ethers across Asia.

    Science.gov (United States)

    Jaward, Foday M; Zhang, Gan; Nam, Jae Jak; Sweetman, Andrew J; Obbard, Jeffrey P; Kobara, Yuso; Jones, Kevin C

    2005-11-15

    Asia is of global importance economically, yet data on ambient persistent organic pollutant levels are still sparse for the region, despite international efforts under the Stockholm Convention to identify and reduce emissions. A large-scale passive air sampling survey was therefore conducted in Asia, specifically in China, Japan, South Korea, and Singapore. Polyurethane foam disks were deployed simultaneously at 77 sites, between Sept 21 and Nov 16, 2004, and analyzed for polychlorinated biphenyls (PCBs), organochlorine compounds (hexachlorobenzene (HCB), dichlorodiphenyltrichloroethanes (DDTs), chlordane), and polybrominated diphenyl ethers (PBDEs). The meteorological conditions prevailing in the region at this time facilitated the assessment of local/regional differences in atmospheric emissions, because large-scale advection effects due to monsoons or dust storms did not occur. Air concentrations estimated assuming an average sampler uptake rate of 3.5 m3/day ranged as follows (pg m(-3)): PCBs, 5-340; HCB, 10-460; DDTs, 0.4-1800; chlordanes, 1-660; PBDEs, < 0.13-340. South Korea and Singapore generally had regionally low concentrations. Elevated concentrations of PCBs, DDTs, and HCB occurred at sites in China, higher than reported in a similar recent sampling campaign in Europe. Chlordane was highest in samples from Japan (which also had elevated levels of PCBs and DDTs) and was also elevated in some Chinese locations. PBDE levels were generally low in the region.

  2. HPLC determination of chlorine in air and water samples following precolumn derivatization to 4-bromoacetanilide

    Energy Technology Data Exchange (ETDEWEB)

    Jain, A. (Rani Durgavati Univ., Jabalpur (India). Dept. of Chemistry); Verma, K.K. (Rani Durgavati Univ., Jabalpur (India). Dept. of Chemistry)

    1993-11-01

    Chlorine has been determined in air and water samples by a rapid and sensitive method entailing precolumn derivatization to 4-bromoacetanilide. A mixed potassium bromide - acetanilide reagent was used as a trapping agent for chlorine in air, and for its derivatization. The 4-bromoacetanilide formed was determined by reversed-phase HPLC on an ODS column, using methanol-water, 65:35 (v/v) as mobile phase; detection was at 240 nm. A rectilinear calibration graph was obtained for the range 0.1-30 [mu]g mL[sup -1] chlorine; the limit of detection found to be 0.01 [mu]g mL[sup -1]. The precolumn derivative has been found to have a shelf-life of at least 21 days; this enables the use of the method for samples transported from the field to the analytical laboratory, or the testing of a variety of conditions for chlorine scrubbing studies without the need for immediate analysis of samples. Humic substances do not cause any interference with the proposed method and the presence of nitrite does not lead to artificially high results and consequent misleading conclusions of the presence of high levels of chlorine. (orig.)

  3. HPLC determination of chlorine in air and water samples following precolumn derivatization to 4-bromoacetanilide

    International Nuclear Information System (INIS)

    Jain, A.; Verma, K.K.

    1993-01-01

    Chlorine has been determined in air and water samples by a rapid and sensitive method entailing precolumn derivatization to 4-bromoacetanilide. A mixed potassium bromide - acetanilide reagent was used as a trapping agent for chlorine in air, and for its derivatization. The 4-bromoacetanilide formed was determined by reversed-phase HPLC on an ODS column, using methanol-water, 65:35 (v/v) as mobile phase; detection was at 240 nm. A rectilinear calibration graph was obtained for the range 0.1-30 μg mL -1 chlorine; the limit of detection found to be 0.01 μg mL -1 . The precolumn derivative has been found to have a shelf-life of at least 21 days; this enables the use of the method for samples transported from the field to the analytical laboratory, or the testing of a variety of conditions for chlorine scrubbing studies without the need for immediate analysis of samples. Humic substances do not cause any interference with the proposed method and the presence of nitrite does not lead to artificially high results and consequent misleading conclusions of the presence of high levels of chlorine. (orig.)

  4. Residues of 2, 4-D in air samples from Saskatchewan: 1966-1975.

    Science.gov (United States)

    Grover, R; Kerr, L A; Wallace, K; Yoshida, K; Maybank, J

    1976-01-01

    Residues of 2,4-D (2,4-dichlorophenoxyacetic acid) in air samples from several sampling sites in central and southern Saskatchewan during the spraying seasons in the 1966-68 and 1970-75 periods were determined by gas-liquid chromatographic techniques. Initially, individual esters of 2,4-D were characterized by retention times and confirmed further by co-injection and dual column procedures. Since 1973, however, only total 2,4-D acid levels in air samples have been determined after esterification to the methyl ester and confirmed by gc/ms techniques whenever possible. Up to 50% of the daily samples collected during the spraying season at any of the locations and during any given year contained 2,4-D, with butyl esters being found most frequently. The daily 24-hr mean atmospheric concentrations of 2,4-D ranged from 0.01 to 1.22 mug/m3, 0.01 to 13.50 mug/m3, and 0.05 to 0.59 mug/m3 for the iso-propyl, mixed butyl and iso-octyl esters, respectively. Even when the samples were analysed for the total 2,4-D content, i.e. from 1973 onwards, the maximum level of the total acid reached only 23.14 mug/m3. In any given year and at any of the sampling sites, about 30% of the samples contained less than 0.01 mug/m3 of 2,4-D. In another 40% of the samples, the levels of 2,4-D ranged from 0.01 to 0.099 mug/m3. Only about 30% of the samples contained 2,4-D concentrations higher than 0.1 mug/m3, with only 10% or less exceeding 1 mug/m3. None of the samples, obtained with the high volume particulate sampler, showed any detectable levels of 2,4-D, indicating little or no transport of 2,4-D adsorbed on dust particles or as crystals of amine salts.

  5. Evaluation of active sampling strategies for the determination of 1,3-butadiene in air

    Science.gov (United States)

    Vallecillos, Laura; Maceira, Alba; Marcé, Rosa Maria; Borrull, Francesc

    2018-03-01

    Two analytical methods for determining levels of 1,3-butadiene in urban and industrial atmospheres were evaluated in this study. Both methods are extensively used for determining the concentration of volatile organic compounds in the atmosphere and involve collecting samples by active adsorptive enrichment on solid sorbents. The first method uses activated charcoal as the sorbent and involves liquid desorption with carbon disulfide. The second involves the use of a multi-sorbent bed with two graphitised carbons and a carbon molecular sieve as the sorbent, with thermal desorption. Special attention was paid to the optimization of the sampling procedure through the study of sample volume, the stability of 1,3-butadiene once inside the sampling tube and the humidity effect. In the end, the thermal desorption method showed better repeatability and limits of detection and quantification for 1,3-butadiene than the liquid desorption method, which makes the thermal desorption method more suitable for analysing air samples from both industrial and urban atmospheres. However, sampling must be performed with a pre-tube filled with a drying agent to prevent the loss of the adsorption capacity of the solid adsorbent caused by water vapour. The thermal desorption method has successfully been applied to determine of 1,3-butadiene inside a 1,3-butadiene production plant and at three locations in the vicinity of the same plant.

  6. 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)

    He Juan; Lv Ruihe; Zhan Haijun; Wang Huizhi; Cheng Jie; Lu Kui; Wang Fengcheng

    2010-01-01

    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.

  7. The determination of volatile chlorinated hydrocarbons in air. Sampling rate and efficiency of diffuse samplers

    Energy Technology Data Exchange (ETDEWEB)

    Giese, U.; Stenner, H.; Kettrup, A.

    1989-05-01

    When applicating diffusive sampling-systems to workplace air-monitoring it is necessary to know the behaviour of the diffusive-rate and the efficiency in dependence of concentration, exposition time and the type of pollutant. Especially concerning mixtures of pollutants there are negative influences by competition and mutual displacement possible. Diffusive-rate and discovery for CH/sub 2/Cl/sub 2/ and CHCl/sub 3/ were investigated using two different types of diffuse samplers. For this it was necessary to develop suitable defices for standard gas generation and for the exposition of diffusive-samplers to a standard gas mixture. (orig.).

  8. Integration of ceramic membrane and compressed air-assisted solvent extraction (CASX) for metal recovery.

    Science.gov (United States)

    Li, Chi-Wang; Chiu, Chun-Hao; Lee, Yu-Cheng; Chang, Chia-Hao; Lee, Yu-Hsun; Chen, Yi-Ming

    2010-01-01

    In our previous publications, compressed air-assisted solvent extraction process (CASX) was developed and proved to be kinetically efficient process for metal removal. In the current study, CASX with a ceramic MF membrane integrated for separation of spent solvent was employed to remove and recover metal from wastewater. MF was operated either in crossflow mode or dead-end with intermittent flushing mode. Under crossflow mode, three distinct stages of flux vs. TMP (trans-membrane pressure) relationship were observed. In the first stage, flux increases with increasing TMP which is followed by the stage of stable flux with increasing TMP. After reaching a threshold TMP which is dependent of crossflow velocity, flux increases again with increasing TMP. At the last stage, solvent was pushed through membrane pores as indicated by increasing permeate COD. In dead-end with intermittent flushing mode, an intermittent flushing flow (2 min after a 10-min or a 30-min dead-end filtration) was incorporated to reduce membrane fouling by flush out MSAB accumulated on membrane surface. Effects of solvent concentration and composition were also investigated. Solvent concentrations ranging from 0.1 to 1% (w/w) have no adverse effect in terms of membrane fouling. However, solvent composition, i.e. D(2)EHPA/kerosene ratio, shows impact on membrane fouling. The type of metal extractants employed in CASX has significant impact on both membrane fouling and the quality of filtrate due to the differences in their viscosity and water solubility. Separation of MSAB was the limiting process controlling metal removal efficiency, and the removal efficiency of Cd(II) and Cr(VI) followed the same trend as that for COD.

  9. Ultrasound-air-assisted demulsified liquid-liquid microextraction by solidification of a floating organic droplet for determination of three antifungal drugs in water and biological samples.

    Science.gov (United States)

    Ezoddin, Maryam; Shojaie, Mehran; Abdi, Khosrou; Karimi, Mohammad Ali

    2017-03-01

    A novel ultrasound-air-assisted demulsified liquid-liquid microextraction by solidification of a floating organic droplet (UAAD-LLM-SFO) followed by HPLC-UV detection was developed for the analysis of three antifungal drugs in water and biological samples. In this method, 1-dodecanol was used as the extraction solvent. The emulsion was rapidly formed by pulling in and pushing out the mixture of sample solution and extraction solvent for 5 times repeatedly using a 10-mL glass syringe while sonication was performed. Therefore, an organic dispersive solvent required in common microextraction methods was not used in the proposed method. After dispersing, an aliquot of acetonitrile was introduced as a demulsifier solvent into the sample solution to separate two phases. Therefore, some additional steps, such as the centrifugation, ultrasonication, or agitation of the sample solution, are not needed. Parameters influencing the extraction recovery were investigated. The proposed method showed a good linearity for the three antifungal drugs studied with the correlation coefficients (R 2  > 0.9995). The limits of detection (LODs) and the limits of the quantification (LOQs) were between 0.01-0.03 μg L -1 and 0.03-0.08 μg L -1 , respectively. The preconcentration factors (PFs) were in the range of 107-116, respectively. The precisions, as the relative standard deviations (RSDs) (n = 5), for inter-day and intra-day analysis were in the range of 2.1-4.5% and 6.5-8.5%, respectively. This method was successfully applied to determine the three antifungal drugs in tap water and biological samples. The recoveries of antifungal drugs in these samples were 92.4-98.5%. Graphical abstract Ultrasound-air-assisted demulsified liquid-liquid microextraction by solidification of a floating organic droplet for the analysis of three antifungal drugs prior HPLC-UV.

  10. Selective extraction of dimethoate from cucumber samples by use of molecularly imprinted microspheres

    Directory of Open Access Journals (Sweden)

    Jiao-Jiao Du

    2015-06-01

    Full Text Available Molecularly imprinted polymers for dimethoate recognition were synthesized by the precipitation polymerization technique using methyl methacrylate (MMA as the functional monomer and ethylene glycol dimethacrylate (EGDMA as the cross-linker. The morphology, adsorption and recognition properties were investigated by scanning electron microscopy (SEM, static adsorption test, and competitive adsorption test. To obtain the best selectivity and binding performance, the synthesis and adsorption conditions of MIPs were optimized through single factor experiments. Under the optimized conditions, the resultant polymers exhibited uniform size, satisfactory binding capacity and significant selectivity. Furthermore, the imprinted polymers were successfully applied as a specific solid-phase extractants combined with high performance liquid chromatography (HPLC for determination of dimethoate residues in the cucumber samples. The average recoveries of three spiked samples ranged from 78.5% to 87.9% with the relative standard deviations (RSDs less than 4.4% and the limit of detection (LOD obtained for dimethoate as low as 2.3 μg/mL. Keywords: Molecularly imprinted polymer, Precipitation polymerization, Dimethoate, Cucumber, HPLC

  11. 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

  12. Modified Dispersive Liquid-Liquid Micro Extraction Using Green Solvent for Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Vegetable Samples

    International Nuclear Information System (INIS)

    Kin, C.M.; Shing, W.L.

    2016-01-01

    According to International Agency for Research on Cancer (IARC), most of Polycyclic Aromatic Hydrocarbons (PAHs) known as genotoxic human carcinogen and mutagenic. PAHs represent as poorly degradable pollutants that exist in soils, sediments, surface water and atmosphere. A simple, rapid and sensitive extraction method termed modified Dispersive Liquid-Liquid Micro extraction (DLLME) using green solvent was developed to determine PAHs in vegetable samples namely radish, cabbage and cucumber prior to Gas Chromatography Flame Ionization Detection (GC-FID). The extraction method is based on replacing chlorinated organic extraction solvent in the conventional DLLME with low toxic solvent, 1-bromo-3-methylbutane without using dispersive solvent. Several experimental factors such as type and volume of extraction solvents, extraction time, confirmation of 12 PAHs by GC-MS, recovery percentages on vegetable samples and the comparative analysis with conventional DLLME were carried out. Both DLLME were successfully extracted 12 types of PAHs. In modified DLLME, the recoveries of the analytes obtained were in a range of 72.72 - 88.07 % with RSD value below 7.5 % which is comparable to the conventional DLLME. The use of microliter of low toxic extraction solvent without addition of dispersive solvent caused the method is economic and environmental friendly which is fulfill the current requirement, green chemistry based analytical method. (author)

  13. 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.

  14. 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

    2017-08-01

    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.

  15. BIBLE A whole-air sampling as a window on Asian biogeochemistry

    Science.gov (United States)

    Elliott, Scott; Blake, Donald R.; Blake, Nicola J.; Dubey, Manvendra K.; Rowland, F. Sherwood; Sive, Barkley C.; Smith, Felisa A.

    2003-02-01

    Asian trace gas and aerosol emissions into carbon, nitrogen, and other elemental cycles will figure prominently in near term Earth system evolution. Atmospheric hydrocarbon measurements resolve numerous chemical species and can be used to investigate sourcing for key geocarriers. A recent aircraft study of biomass burning and lightning (BIBLE A) explored the East Asian atmosphere and was unique in centering on the Indonesian archipelago. Samples of volatile organics taken over/between the islands of Japan, Saipan, Java, and Borneo are here examined as a guide to whole-air-based studies of future Asian biogeochemistry. The midlatitude onshore/offshore pulse and tropical convection strongly influence concentration distributions. As species of increasing molecular weight are considered, rural, combustion, and industrial source regimes emerge. Methane-rich inputs such as waste treatment and rice cultivation are evidenced in the geostrophic outflow. The Indonesian atmosphere is rich in biomass burning markers and also those of vehicular activity. Complexity of air chemistry in the archipelago is a direct reflection of diverse topography, land use, and local economies in a rapidly developing nation. Conspicuous in its absence is the fingerprint for liquefied petroleum gas leakage, but it can be expected to appear as demand for clean fossil fuels rises along with per capita incomes. Combustion tracers indicate high nitrogen mobilization rates, linking regional terrestrial geocycles with open marine ecosystems. Sea to air fluxes are superimposed on continental and marine backgrounds for the methyl halides. However, ocean hot spots are not coordinated and suggest an intricate subsurface kinetics. Levels of long-lived anthropogenic halocarbons attest to the success of international environmental treaties while reactive chlorine containing species track industrial air masses. The dozens of hydrocarbons resolvable by gas chromatographic methods will enable monitoring of

  16. [An AIDS-related cognitive map in a sample of drug abusers in Buenos Aires City].

    Science.gov (United States)

    Kornblit, A L; Bilyk, A

    1990-01-01

    This paper is an approach to AIDS as a topic among a drug abusers sample of the city of Buenos Aires. Research was carried out on the basis of a qualitative methodology. In an attempt at surveying opinions and attitudes of such a sample as regards AIDS (i.e. subjects' cognitive map), 21 drug abusers from three different rehabilitation programs operating in the B.A. area were interviewed. On the basis of the research performed, the authors elaborate communication strategies among drug abusers that would be helpful for authorities engaged in AIDS prevention to adopt. To boost a strategy likely to break up the AIDS-drug association existing in the mind of many an abuser would be highly advisable so that a separation be settled between both representations, thus giving drug abusers a higher motivation for self-care practice.

  17. Ram-air sample collection device for a chemical warfare agent sensor

    Science.gov (United States)

    Megerle, Clifford A.; Adkins, Douglas R.; Frye-Mason, Gregory C.

    2002-01-01

    In a surface acoustic wave sensor mounted within a body, the sensor having a surface acoustic wave array detector and a micro-fabricated sample preconcentrator exposed on a surface of the body, an apparatus for collecting air for the sensor, comprising a housing operatively arranged to mount atop the body, the housing including a multi-stage channel having an inlet and an outlet, the channel having a first stage having a first height and width proximate the inlet, a second stage having a second lower height and width proximate the micro-fabricated sample preconcentrator, a third stage having a still lower third height and width proximate the surface acoustic wave array detector, and a fourth stage having a fourth height and width proximate the outlet, where the fourth height and width are substantially the same as the first height and width.

  18. Air-segmented continuous-flow analysis for molybdenum in various geochemical samples

    International Nuclear Information System (INIS)

    Harita, Y.; Sugiyama, M.; Hori, T.

    2003-01-01

    An air-segmented continuous-flow method has been developed for the determination of molybdenum at ultra trace levels using the catalytic effect of molybdate during the oxidation of L-ascorbic acid by hydrogen peroxide. Incorporation of an on-line ion exchange column improved the tolerance limit for various ions. The detection limits with and without the column were 64 pmol L m1 and 17 pmol L m1 , and the reproducibilities at 10 nmol L m1 were 2.1 % and 0.2 %, respectively. The proposed method was applied to the determination of molybdenum in seawater and lake water as well as in rock and sediment samples. This method has the highest sensitivity among the available literature to our knowledge, and is also convenient for routine analysis of molybdenum in various natural samples. (author)

  19. Hot air vapor extraction system for remediation of petroleum contaminated sites

    International Nuclear Information System (INIS)

    Pal, D.; Karr, L.; Fann, S.; Mathews, A.P.; Price, P.A.; Linginemi, S.

    1996-01-01

    This paper describes the results of a demonstration of a technology entitled ''Hot Air Vapor Extraction (HAVE)'' at the Hydrocarbon National Test Site (HNTS), Port Hueneme, California. The demonstration of the HAVE technology at HNTS was conducted over a 3-month period between August 21, 1995 and November 22, 1995 and the lessons learned from the demonstration are discussed in details to guide the Department of Defense decision makers in analyzing the applicability of this technology to their contaminated sites. This technology demonstration was conducted under the Department of Defense Strategic Environmental Research and Development Program (SERDP) as part of the National Environmental Technology Demonstration Program (NETDP). The primary objectives of the demonstration were to (1) validate the efficacy of the HAVE technology to treat a wide range of hydrocarbons contaminated soils, (2) gather data to estimate treatment costs, and (3) develop engineering guidance needed to apply this remediation technology DoD-wide. Test runs were made on 5 different treatment cells containing various fuel hydrocarbons, ranging from gasoline to heavier petroleum fractions such as lubricating oil. Computer modeling was conducted to analyze the test results and also to optimize the HAVE system design. An economic analysis conducted for various remediation project sizes ranging from 750 to 9,000 cubic yards, the per cubic yard treatment costs are found to vary from $64.05 down to $36.54 respectively

  20. EPA's Response to the February 2014 Release of Radioactive Material from the Waste Isolation Pilot Plant (WIPP): EPA's WIPP Air Sampling Data from April 2014

    Science.gov (United States)

    In April 2014, U.S. Environmental Protection Agency (EPA) environmental monitoring and assessment team members reviewed DOE's air sampling plan, visited DOE's air samplers and placed air samplers onsite near existing DOE samplers to corroborate results.

  1. NH4NO3 extractable trace element contents of soil samples prepared for proficiency testing--a stability study.

    Science.gov (United States)

    Traub, H; Scharf, H

    2001-06-01

    In view of its intended use as a sample for proficiency testing or as a reference material the stability of the extractable trace element contents of a soil from an irrigation field was tested using the extraction with 1 mol/L ammonium nitrate solution according to DIN 19730. Therefore, changes of the extractability of sterilized and non sterilized soil samples stored at different temperatures were evaluated over a period of 18 months. Sets of bottles were kept at -20 degrees C, +4 degrees C, about +20 degrees C and +40 degrees C, respectively. The NH4NO3 extractable contents of Cd, Cr, Cu, Ni, Pb and Zn were determined immediately after bottling and then after 3, 6, 12 and 18 months with ICP-AES or ETAAS. Appropriate storage conditions are of utmost importance to prevent deterioration of soil samples prepared for the determination of NH4NO3 extractable trace element contents. Temperatures above +20 degrees C must be avoided. The observed changes in the extractability of the metals (especially for Cr and Cu) most likely could be related to thermal degradation of the organic matter of the soil. There is no need to sterilize dry soil samples, because microbiological activity in soils with a low moisture content appears to be negligible with regard to trace element mobilization.

  2. 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)

  3. Evaluation of physical sampling efficiency for cyclone-based personal bioaerosol samplers in moving air environments.

    Science.gov (United States)

    Su, Wei-Chung; Tolchinsky, Alexander D; Chen, Bean T; Sigaev, Vladimir I; Cheng, Yung Sung

    2012-09-01

    The need to determine occupational exposure to bioaerosols has notably increased in the past decade, especially for microbiology-related workplaces and laboratories. Recently, two new cyclone-based personal bioaerosol samplers were developed by the National Institute for Occupational Safety and Health (NIOSH) in the USA and the Research Center for Toxicology and Hygienic Regulation of Biopreparations (RCT & HRB) in Russia to monitor bioaerosol exposure in the workplace. Here, a series of wind tunnel experiments were carried out to evaluate the physical sampling performance of these two samplers in moving air conditions, which could provide information for personal biological monitoring in a moving air environment. The experiments were conducted in a small wind tunnel facility using three wind speeds (0.5, 1.0 and 2.0 m s(-1)) and three sampling orientations (0°, 90°, and 180°) with respect to the wind direction. Monodispersed particles ranging from 0.5 to 10 μm were employed as the test aerosols. The evaluation of the physical sampling performance was focused on the aspiration efficiency and capture efficiency of the two samplers. The test results showed that the orientation-averaged aspiration efficiencies of the two samplers closely agreed with the American Conference of Governmental Industrial Hygienists (ACGIH) inhalable convention within the particle sizes used in the evaluation tests, and the effect of the wind speed on the aspiration efficiency was found negligible. The capture efficiencies of these two samplers ranged from 70% to 80%. These data offer important information on the insight into the physical sampling characteristics of the two test samplers.

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

    International Nuclear Information System (INIS)

    Sudheendran, V.; Baburajan, A.; Gaikwad, R.H.; Ravi, P.M.; Tripathi, R.M.

    2015-01-01

    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 241 Am and 90 Sr/ 90 Y 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)

  5. 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.)

  6. 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.

  7. 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. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Liquid-solid extraction of uranium (VI) with TOPO - molten naphthalene and determination by laser fluorimetry in geological samples

    International Nuclear Information System (INIS)

    Kumar, Sanjay; Krishnakumar, M.; Patwardhan, A.A.

    2007-01-01

    A simple, rapid, sensitive, cost-effective and efficient method for separation of uranium using tri-n-octylphosphine oxide (TOPO)-molten naphthalene as solid phase extractant and its determination by laser fluorimetry in geological samples (rock, soil, sediment) was developed. Under optimum conditions, using 50 mg TOPO and 100 mg naphthalene, 50 - 5000 ng of uranium in 10 ml sample solution (3% (v/v) HNO 3 ) could be extracted quantitatively. The extracted uranium was stripped using tetra sodium pyrophosphate (5% (v/v) solution, pH adjusted to 7.0 with H 3 PO 4 ) and determined by laser fluorimetry. The influence of different acid concentrations, the amount of solid phase extractant, sample volumes, different stripping reagents, their volumes and effect of foreign ions on the extraction and determination of uranium (VI) were investigated. Synthetic samples of varying concentration as regards uranium were prepared and analysed. Recoveries ranging from 90% to 105% were obtained. The method was validated by analyzing four certified reference materials namely, BL-5, DH-1a, SY-2, SY-3 and the values obtained for uranium agreed well with the certified values. The method was also applied to the determination of uranium in geological samples (rock, soil and sediment) by laser fluorimetry and the results obtained compared favorably with those obtained from the pellet fluorimetry method. Following the proposed method, determination limit for uranium was found to be 1 μg/g with RSD ± 10%. (author)

  9. Liquid-liquid extraction assisted by a carbon nanoparticles interface. Electrophoretic determination of atrazine in environmental samples.

    Science.gov (United States)

    Caballero-Díaz, Encarnación; Simonet, Bartolomé; Valcárcel, Miguel

    2013-10-21

    A novel method for the determination of atrazine, using liquid-liquid extraction assisted by a nanoparticles film formed in situ and composed of organic solvent stabilized-carbon nanoparticles, is described. The presence of nanoparticles located at the liquid-liquid interface reinforced the extraction of analyte from matrix prior to capillary electrophoresis (CE) analysis. Some influential experimental variables were optimized in order to enhance the extraction efficiency. The developed procedure confirmed that carbon nanoparticles, especially multi-walled carbon nanotubes, are suitable to be used in sample treatment processes introducing new mechanisms of interaction with the analyte. The application of the proposed preconcentration method followed by CE detection enabled the determination of atrazine in spiked river water providing acceptable RSD values (11.6%) and good recoveries (about 87.0-92.0%). Additionally, a similar extraction scheme was tested in soil matrices with a view to further applications in real soil samples.

  10. Development of cloud point extraction - UV-visible spectrophotometric method for vanadium (V) determination in hydrogeochemical samples

    International Nuclear Information System (INIS)

    Durani, Smeer; Mathur, Neerja; Chowdary, G.S.

    2007-01-01

    The cloud point extraction behavior (CPE) of vanadium (V) using 5,7 dibromo 8-hydroxyquinoline (DBHQ) and triton X 100 was investigated. Vanadium (V) was extracted with 4 ml of 0.5 mg/ml DBHQ and 6 ml of 8% (V/V) triton X 100 at the pH 3.7. A few hydrogeochemical samples were analysed for vanadium using the above method. (author)

  11. Cloud point extraction and spectrophotometric determination of mercury species at trace levels in environmental samples.

    Science.gov (United States)

    Ulusoy, Halil İbrahim; Gürkan, Ramazan; Ulusoy, Songül

    2012-01-15

    A new micelle-mediated separation and preconcentration method was developed for ultra-trace quantities of mercury ions prior to spectrophotometric determination. The method is based on cloud point extraction (CPE) of Hg(II) ions with polyethylene glycol tert-octylphenyl ether (Triton X-114) in the presence of chelating agents such as 1-(2-pyridylazo)-2-naphthol (PAN) and 4-(2-thiazolylazo) resorcinol (TAR). Hg(II) ions react with both PAN and TAR in a surfactant solution yielding a hydrophobic complex at pH 9.0 and 8.0, respectively. The phase separation was accomplished by centrifugation for 5 min at 3500 rpm. The calibration graphs obtained from Hg(II)-PAN and Hg(II)-TAR complexes were linear in the concentration ranges of 10-1000 μg L(-1) and 50-2500 μg L(-1) with detection limits of 1.65 and 14.5 μg L(-1), respectively. The relative standard deviations (RSDs) were 1.85% and 2.35% in determinations of 25 and 250 μg L(-1) Hg(II), respectively. The interference effect of several ions were studied and seen commonly present ions in water samples had no significantly effect on determination of Hg(II). The developed methods were successfully applied to determine mercury concentrations in environmental water samples. The accuracy and validity of the proposed methods were tested by means of five replicate analyses of the certified standard materials such as QC Metal LL3 (VWR, drinking water) and IAEA W-4 (NIST, simulated fresh water). Copyright © 2011 Elsevier B.V. All rights reserved.

  12. Homogeneous liquid-liquid extraction (HoLLE) via flotation combined with gas chromatography-flame ionization detection as a very simple, rapid and sensitive method for the determination of fenitrothion in water samples.

    Science.gov (United States)

    Mashayekhi, Hossein Ali

    2013-01-01

    Homogeneous liquid-liquid extraction via flotation assistance (HoLLE-FA) and gas chromatography-flame ionization detection (GC-FID) was presented for the extraction and determination of fenitrothion in water samples. In this work, a rapid, simple and efficient HoLLE-FA method was developed based on applying low-density organic solvents without employing centrifugation. A special extraction cell was designed to facilitate the collection of low-density solvent extraction in the determination of fenitrothion in water samples. The water sample solution was added into an extraction cell that contained an appropriate mixture of extraction and homogeneous solvents. By using air flotation, the organic solvent was collected at the conical part of the designed cell. Under the optimum conditions, the method performance was studied in terms of the linear dynamic range (LDR from 1.0 up to 100 μg L⁻¹), linearity (r² > 0.998), and precision (repeatability extraction and determination of fenitrothion in three different water samples.

  13. 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.

  14. 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)

    You, Xiangwei; Xing, Zhuokan; Liu, Fengmao; Zhang, Xu

    2015-01-01

    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

  15. Some triterpenic compounds in extracts of Cecropia and Bauhinia species for different sampling years

    Directory of Open Access Journals (Sweden)

    Marcella Emilia Pietra Schmidt

    Full Text Available ABSTRACT The aim of this paper is to provide an overview on the chemical composition of triterpenes in widespread used folk medicine species, through the development and validation of eleven compounds using HPLC-UV detection. The compounds were separated using isocratic elution, on a reverse phase column (Kinetex C18, 250 mm × 4.6 mm, 5 µm with mobile phase consisted of acetonitrile:tetrahydrofuran (90:10, v/v, flow-rate of 0.5 ml/min and detection in 210 nm. Diverse validation parameters were successfully evaluated. The samples of Bauhinia variegata L., B. variegata var. candida Voigt, Fabaceae, Cecropia palmata Willd. and C. obtusa Trécul, Urticaceae, collected in 2012, 2013 and 2014 from Amazon were treated with two different solvents (ethyl acetate and chloroform and analyzed by the proposed method. Stigmasterol, lupeol, β-sitosterol, β-amirin and α-amirin were found in all the studied plants. Highlighting the presence of oleanolic acid, maslinic acid in C. obtusa and C. palmata extracts, erythrodiol only in C. palmata, stigmasteol in B. variegata and α-amirin in B. variegata var. candida. Overall, ethyl acetate showed better performance as the extractor solvent than chloroform. Moreover, it could be used for the quality control of medicinal plants and to assess potential marker compounds.

  16. Determination of cadmium in real water samples by flame atomic absorption spectrometry after cloud point extraction

    International Nuclear Information System (INIS)

    Naeemullah, A.; Kazi, T.G.

    2011-01-01

    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)

  17. Application of 241Am EDXRF to the determination of rare earth samples of solvent extraction processes

    International Nuclear Information System (INIS)

    Yan Chunhua; Jia Jiangtao; Liao Chunsheng; Li Biaoguo

    1998-01-01

    A rapid energy dispersive X-ray fluorescence spectroscopy (EDXRF) analysis system is established to determine rare earth concentrations. The characteristic K-shell series X-rays of rare earths were excited by a 1.1 x 10 9 Bq 241 Am radioisotope source. The spectra were recorded and analyzed using a multi-channel analyzer, employing a high-purity Ge detector. In this method, the Compton scattering peak, absorption of elements, and specific simplification are considered. Samples of light, middle and heavy rare earths during separation processes in both hydrochloride solution and rare earth loaded organic phases were analyzed off-line. Some comparative results measured by ICP are also given. The results show that the method can be used for a wide range of rare earth concentrations (0.1-300 g l -1 rare earth oxide). Being rapid, effective, precise and non-destructive, the method can be applied to on-line analysis to determine rare earth concentrations during separation by solvent extraction. (orig.)

  18. Solvent effects on extraction of polycyclic aromatic hydrocarbons in ambient aerosol samples

    Directory of Open Access Journals (Sweden)

    Flasch Mira

    2016-01-01

    Full Text Available Polycyclic Aromatic Hydrocarbons (PAHs in the ambient particulate matter pose one of the most important issues in the focus of environmental management. The concentration of their representative, Benzo(apyrene (BaP, undergoes limitations according to European Union directive. However, a successful control over the pollution levels and their sources is limited by the high uncertainty of analytical and statistical approaches used for their characterization. Here we compare differences in PAH concentrations related to the use of different solvents in the course of ultrasonic extraction of a certified reference material (PM10-like PAH mixture and filter samples of ambient particulate matter collected in Austria for the CG-MS PAH analysis. Using solvents of increasing polarity: Cyclohexane (0,006, Toluene (0,099, Dichloromethane (0,309, Acetone (0,43 and Acetonitrile (0,460, as well as mixtures of those, filters representing high and low concentrations of particulate matter were investigated. Although some scatter of the obtained concentrations was observed no trend related to the polarity of the solvent became visible. Regarding the reproducibility, which can be expected of PAH analysis no significant difference between the different solvents was determined. This result is valid for all compounds under investigation.

  19. [Extracting THz absorption coefficient spectrum based on accurate determination of sample thickness].

    Science.gov (United States)

    Li, Zhi; Zhang, Zhao-hui; Zhao, Xiao-yan; Su, Hai-xia; Yan, Fang

    2012-04-01

    Extracting absorption spectrum in THz band is one of the important aspects in THz applications. Sample's absorption coefficient has a complex nonlinear relationship with its thickness. However, as it is not convenient to measure the thickness directly, absorption spectrum is usually determined incorrectly. Based on the method proposed by Duvillaret which was used to precisely determine the thickness of LiNbO3, the approach to measuring the absorption coefficient spectra of glutamine and histidine in frequency range from 0.3 to 2.6 THz(1 THz = 10(12) Hz) was improved in this paper. In order to validate the correctness of this absorption spectrum, we designed a series of experiments to compare the linearity of absorption coefficient belonging to one kind amino acid in different concentrations. The results indicate that as agreed by Lambert-Beer's Law, absorption coefficient spectrum of amino acid from the improved algorithm performs better linearity with its concentration than that from the common algorithm, which can be the basis of quantitative analysis in further researches.

  20. 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.

  1. Efficient sample preparation method based on solvent-assisted dispersive solid-phase extraction for the trace detection of butachlor in urine and waste water samples.

    Science.gov (United States)

    Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

    2016-10-01

    In this work, an efficient sample preparation method termed solvent-assisted dispersive solid-phase extraction was applied. The used sample preparation method was based on the dispersion of the sorbent (benzophenone) into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was achieved 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 butachlor, the cloudy solution was centrifuged and butachlor in the sediment phase dissolved in ethanol and determined by gas chromatography with flame ionization detection. Under the optimized conditions (solution pH = 7.0, sorbent: benzophenone, 2%, disperser solvent: ethanol, 500 μL, centrifuged at 4000 rpm for 3 min), the method detection limit for butachlor was 2, 3 and 3 μg/L for distilled water, waste water, and urine sample, respectively. Furthermore, the preconcentration factor was 198.8, 175.0, and 174.2 in distilled water, waste water, and urine sample, respectively. Solvent-assisted dispersive solid-phase extraction was successfully used for the trace monitoring of butachlor in urine and waste water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Method and apparatus maintaining multi-component sample gas constituents in vapor phase during sample extraction and cooling

    Science.gov (United States)

    Farthing, William Earl; Felix, Larry Gordon; Snyder, Todd Robert

    2009-12-15

    An apparatus and method for diluting and cooling that is extracted from high temperature and/or high pressure industrial processes. Through a feedback process, a specialized, CFD-modeled dilution cooler is employed along with real-time estimations of the point at which condensation will occur within the dilution cooler to define a level of dilution and diluted gas temperature that results in a gas that can be conveyed to standard gas analyzers that contains no condensed hydrocarbon compounds or condensed moisture.

  3. Method and apparatus for maintaining multi-component sample gas constituents in vapor phase during sample extraction and cooling

    Science.gov (United States)

    Farthing, William Earl [Pinson, AL; Felix, Larry Gordon [Pelham, AL; Snyder, Todd Robert [Birmingham, AL

    2008-02-12

    An apparatus and method for diluting and cooling that is extracted from high temperature and/or high pressure industrial processes. Through a feedback process, a specialized, CFD-modeled dilution cooler is employed along with real-time estimations of the point at which condensation will occur within the dilution cooler to define a level of dilution and diluted gas temperature that results in a gas that can be conveyed to standard gas analyzers that contains no condensed hydrocarbon compounds or condensed moisture.

  4. 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.

  5. Determination of vanadium in steel and geological samples by its extraction and spectrophotometric determination using 2,3-dihydroxynaphthalene

    International Nuclear Information System (INIS)

    Mondal, R.K.; Tarafder, P.K.; Rathore, D.P.S.

    2013-01-01

    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 10 4 Lmol -1 cm -1 . For samples having >5 fold excess concentration of TiO 2 , a prior separation of TiO 2 as its (Ti (OH) (HND) 3 ) complex is a must. The method has been successfully applied to different rock, soil and steel samples. (author)

  6. Cloud point extraction and flame atomic absorption spectrometric determination of cadmium and nickel in drinking and wastewater samples.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem G; Shah, Faheem; Afridi, Hassan I; Baig, Jameel Ahmed; Soomro, Abdul Sattar

    2013-01-01

    A simple method for the preconcentration of cadmium (Cd) and nickel (Ni) in drinking and wastewater samples was developed. Cloud point extraction has been used for the preconcentration of both metals, after formation of complexes with 8-hydroxyquinoline (8-HQ) and extraction with the surfactant octylphenoxypolyethoxyethanol (Triton X-114). Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation, and the Cd and Ni contents were measured by flame atomic absorption spectrometry. The experimental variables, such as pH, amounts of reagents (8-HQ and Triton X-114), temperature, incubation time, and sample volume, were optimized. After optimization of the complexation and extraction conditions, enhancement factors of 80 and 61, with LOD values of 0.22 and 0.52 microg/L, were obtained for Cd and Ni, respectively. The proposed method was applied satisfactorily for the determination of both elements in drinking and wastewater samples.

  7. Rational approach to solvent system selection for liquid-liquid extraction-assisted sample pretreatment in counter-current chromatography.

    Science.gov (United States)

    Wang, Jiajia; Gu, Dongyu; Wang, Miao; Guo, Xinfeng; Li, Haoquan; Dong, Yue; Guo, Hong; Wang, Yi; Fan, Mengqi; Yang, Yi

    2017-05-15

    A rational liquid-liquid extraction approach was established to pre-treat samples for high-speed counter-current chromatography (HSCCC). n-Hexane-ethyl acetate-methanol-water (4:5:4:5, v/v) and (1:5:1:5, v/v) were selected as solvent systems for liquid-liquid extraction by systematically screening K of target compounds to remove low- and high-polarity impurities in the sample, respectively. After liquid-liquid extraction was performed, 1.4g of crude sample II was obtained from 18.5g of crude sample I which was extracted from the flowers of Robinia pseudoacacia L., and then separated with HSCCC by using a solvent system composed of n-hexane-ethyl acetate-methanol-water (1:2:1:2, v/v). As a result, 31mg of robinin and 37mg of kaempferol 7-O-α-l-rhamnopyranoside were isolated from 200mg of crude sample II in a single run of HSCCC. A scale-up separation was also performed, and 160mg of robinin with 95% purity and 188mg of kaempferol 7-O-α-l-rhamnopyranoside with 97% purity were produced from 1.2g of crude sample II. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Quantitative trace analysis of polyfluorinated alkyl substances (PFAS) in ambient air samples from Mace Head (Ireland): A method intercomparison

    Science.gov (United States)

    Jahnke, Annika; Barber, Jonathan L.; Jones, Kevin C.; Temme, Christian

    A method intercomparison study of analytical methods for the determination of neutral, volatile polyfluorinated alkyl substances (PFAS) was carried out in March, 2006. Environmental air samples were collected in triplicate at the European background site Mace Head on the west coast of Ireland, a site dominated by 'clean' westerly winds coming across the Atlantic. Extraction and analysis were performed at two laboratories active in PFAS research using their in-house methods. Airborne polyfluorinated telomer alcohols (FTOHs), fluorooctane sulfonamides and sulfonamidoethanols (FOSAs/FOSEs) as well as additional polyfluorinated compounds were investigated. Different native and isotope-labelled internal standards (IS) were applied at various steps in the analytical procedure to evaluate the different quantification strategies. Field blanks revealed no major blank problems. European background concentrations observed at Mace Head were found to be in a similar range to Arctic data reported in the literature. Due to trace-levels at the remote site, only FTOH data sets were complete and could therefore be compared between the laboratories. Additionally, FOSEs could partly be included. Data comparison revealed that despite the challenges inherent in analysis of airborne PFAS and the low concentrations, all methods applied in this study obtained similar results. However, application of isotope-labelled IS early in the analytical procedure leads to more precise results and is therefore recommended.

  9. Extractive Sampling and Optical Remote Sensing of F-100 Aircraft Engine Emissions (PREPRINT)

    National Research Council Canada - National Science Library

    Cowen, Kenneth; Goodwin, Bradley; Satola, Jan; Kagann, Robert; Hashmonay, Ram; Spicer, Chester; Holdren, Michael; Mayfield, Howard T

    2008-01-01

    ... from military aircraft, in order to meet increasingly stringent regulatory requirements. This paper describes the results of a recent field study using extractive and optical remote sensing (ORS...

  10. Mixed functional monomers-based monolithic adsorbent for the effective extraction of sulfonylurea herbicides in water and soil samples.

    Science.gov (United States)

    Pei, Miao; Zhu, Xiangyu; Huang, Xiaojia

    2018-01-05

    Effective extraction is a key step in the determination of sulfonylurea herbicides (SUHs) in complicated samples. According to the chemical properties of SUHs, a new monolithic adsorbent utilizing acrylamidophenylboronic acid and vinylimidazole as mixed functional monomers was synthesized. The new adsorbent was employed as the extraction phase of multiple monolithic fiber solid-phase microextraction (MMF-SPME) of SUHs, and the extracted SUHs were determined by high-performance liquid chromatography with diode array detection (HPLC-DAD). Results well evidence that the prepared adsorbent could extract SUHs in environmental waters and soil effectively through multiply interactions such as boronate affinity, dipole-dipole and π-π interactions. Under the optimized extraction conditions, the limits of detection for target SUHs in environmental water and soil samples were 0.018-0.17μg/L and 0.14-1.23μg/kg, respectively. At the same time, the developed method also displayed some analytical merits including wide linear dynamic ranges, good method reproducibility, satisfactory sensitivity and low consume of organic solvent. Finally, the developed were successfully applied to monitor trace SUHs in environmental water and soil samples. The recoveries at three fortified concentrations were in the range of 70.6-119% with RSD below 11% in all cases. The obtained results well demonstrate the excellent practical applicability of the developed MMF-SPME-HPLC-DAD method for the monitoring of SUHs in water and soil samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Quantitative extraction of nucleotides from frozen muscle samples of Atlantic salmon ( Salmo salar ) and rainbow trout ( Oncorhynchus mykiss ) : Effects of time taken to sample and extraction method

    DEFF Research Database (Denmark)

    Thomas, P.M.; Bremner, Allan; Pankhurst, N.W.

    2000-01-01

    time taken to sample, method 2 resulted in higher adenylate and lower IMP concentration than method I. These results indicate that method 2 is most effective in obtaining realistic nucleotide concentrations from fish muscle because it maintains the tissue temperature below the critical freeze zone, (-0...

  12. Improved Methods of Carnivore Faecal Sample Preservation, DNA Extraction and Quantification for Accurate Genotyping of Wild Tigers

    Science.gov (United States)

    Harika, Katakam; Mahla, Ranjeet Singh; Shivaji, Sisinthy

    2012-01-01

    Background Non-invasively collected samples allow a variety of genetic studies on endangered and elusive species. However due to low amplification success and high genotyping error rates fewer samples can be identified up to the individual level. Number of PCRs needed to obtain reliable genotypes also noticeably increase. Methods We developed a quantitative PCR assay to measure and grade amplifiable nuclear DNA in feline faecal extracts. We determined DNA degradation in experimentally aged faecal samples and tested a suite of pre-PCR protocols to considerably improve DNA retrieval. Results Average DNA concentrations of Grade I, II and III extracts were 982pg/µl, 9.5pg/µl and 0.4pg/µl respectively. Nearly 10% of extracts had no amplifiable DNA. Microsatellite PCR success and allelic dropout rates were 92% and 1.5% in Grade I, 79% and 5% in Grade II, and 54% and 16% in Grade III respectively. Our results on experimentally aged faecal samples showed that ageing has a significant effect on quantity and quality of amplifiable DNA (pDNA degradation occurs within 3 days of exposure to direct sunlight. DNA concentrations of Day 1 samples stored by ethanol and silica methods for a month varied significantly from fresh Day 1 extracts (p0.05). DNA concentrations of fresh tiger and leopard faecal extracts without addition of carrier RNA were 816.5pg/µl (±115.5) and 690.1pg/µl (±207.1), while concentrations with addition of carrier RNA were 49414.5pg/µl (±9370.6) and 20982.7pg/µl (±6835.8) respectively. Conclusions Our results indicate that carnivore faecal samples should be collected as freshly as possible, are better preserved by two-step method and should be extracted with addition of carrier RNA. We recommend quantification of template DNA as this facilitates several downstream protocols. PMID:23071624

  13. Sources of present Chernobyl-derived caesium concentrations in surface air and deposition samples

    Energy Technology Data Exchange (ETDEWEB)

    Hoetzl, H.; Rosner, G.; Winkler, R. (Gesellschaft fuer Strahlen-und Umweltforschung Munich, Neuherberg (Germany). Forschungszentrum fuer Umwelt und Gesundheit Gesellschaft fuer Strahlen- und Umweltforschung mbH Muenchen, Neuherberg (Germany). Inst. fuer Strahlenschutz)

    1992-06-01

    The sources of Chernobyl-derived caesium concentrations in air and deposition samples collected from mid-1986 to end-1990 at Munich- Neuherberg, Germany, were investigated. Local resuspension has been found to be the main source. By comparison with deposition data from other locations it is estimated that within a range from 20 Bq m[sup -2] to 60 kBq m[sup -2] of initially deposited [sup 137]Cs activity [approx]2% is re-deposited by the process of local resuspension in Austria, Germany, Japan and United Kingdom, while significantly higher total resuspension is to be expected for Denmark and Finland. Stratospheric contribution to present concentrations is shown to be negligible. This is confirmed by cross correlation analysis between the time series of [sup 137]Cs in air and precipitation before and after the Chernobyl accident and the respective time series of cosmogenic [sup 7]Be, which is an indicator of stratospheric input. Seasonal variations of caesium concentrations with maxima in winter were observed. (author). 32 refs.; 5 figs.; 1 tab.

  14. Sources of present Chernobyl-derived caesium concentrations in surface air and deposition samples

    International Nuclear Information System (INIS)

    Hoetzl, H.; Rosner, G.; Winkler, R.; Gesellschaft fuer Strahlen- und Umweltforschung mbH Muenchen, Neuherberg

    1992-01-01

    The sources of Chernobyl-derived caesium concentrations in air and deposition samples collected from mid-1986 to end-1990 at Munich- Neuherberg, Germany, were investigated. Local resuspension has been found to be the main source. By comparison with deposition data from other locations it is estimated that within a range from 20 Bq m -2 to 60 kBq m -2 of initially deposited 137 Cs activity ∼2% is re-deposited by the process of local resuspension in Austria, Germany, Japan and United Kingdom, while significantly higher total resuspension is to be expected for Denmark and Finland. Stratospheric contribution to present concentrations is shown to be negligible. This is confirmed by cross correlation analysis between the time series of 137 Cs in air and precipitation before and after the Chernobyl accident and the respective time series of cosmogenic 7 Be, which is an indicator of stratospheric input. Seasonal variations of caesium concentrations with maxima in winter were observed. (author). 32 refs.; 5 figs.; 1 tab

  15. Modelling and Evaluating Air Quality with Fuzzy Logic Algorithm-Ankara-Cebeci Sample

    OpenAIRE

    Atacak, Ismail; Arici, Nursal; Guner, Dilem

    2017-01-01

    Air is one of the most important life sources for all living things. Gases that are present and absent in the composition of clean air also considered as pollutants in the atmosphere. If the pollutants rise above a certain concentration level, air pollution occurs. Air pollution damages all living things, especially human health. Accurate estimation of pollutant concentrations through air pollution modeling has an important effect in reducing the adverse effects of pollution and taking necess...

  16. Air-deployable oil spill sampling devices review phase 2 testing. Volume 1

    International Nuclear Information System (INIS)

    Hawke, L.; Dumouchel, A.; Fingas, M.; Brown, C.E.

    2007-01-01

    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

  17. Impact of preferential sampling on exposure prediction and health effect inference in the context of air pollution epidemiology.

    Science.gov (United States)

    Lee, A; Szpiro, A; Kim, S Y; Sheppard, L

    2015-06-01

    Preferential sampling has been defined in the context of geostatistical modeling as the dependence between the sampling locations and the process that describes the spatial structure of the data. It can occur when networks are designed to find high values. For example, in networks based on the U.S. Clean Air Act monitors are sited to determine whether air quality standards are exceeded. We study the impact of the design of monitor networks in the context of air pollution epidemiology studies. The effect of preferential sampling has been illustrated in the literature by highlighting its impact on spatial predictions. In this paper, we use these predictions as input in a second stage analysis, and we assess how they affect health effect inference. Our work is motivated by data from two United States regulatory networks and health data from the Multi-Ethnic Study of Atherosclerosis and Air Pollution. The two networks were designed to monitor air pollution in urban and rural areas respectively, and we found that the health analysis results based on the two networks can lead to different scientific conclusions. We use preferential sampling to gain insight into these differences. We designed a simulation study, and found that the validity and reliability of the health effect estimate can be greatly affected by how we sample the monitor locations. To better understand its effect on second stage inference, we identify two components of preferential sampling that shed light on how preferential sampling alters the properties of the health effect estimate.

  18. Impact of preferential sampling on exposure prediction and health effect inference in the context of air pollution epidemiology

    Science.gov (United States)

    Lee, A.; Szpiro, A.; Kim, S.Y.; Sheppard, L.

    2018-01-01

    Summary Preferential sampling has been defined in the context of geostatistical modeling as the dependence between the sampling locations and the process that describes the spatial structure of the data. It can occur when networks are designed to find high values. For example, in networks based on the U.S. Clean Air Act monitors are sited to determine whether air quality standards are exceeded. We study the impact of the design of monitor networks in the context of air pollution epidemiology studies. The effect of preferential sampling has been illustrated in the literature by highlighting its impact on spatial predictions. In this paper, we use these predictions as input in a second stage analysis, and we assess how they affect health effect inference. Our work is motivated by data from two United States regulatory networks and health data from the Multi-Ethnic Study of Atherosclerosis and Air Pollution. The two networks were designed to monitor air pollution in urban and rural areas respectively, and we found that the health analysis results based on the two networks can lead to different scientific conclusions. We use preferential sampling to gain insight into these differences. We designed a simulation study, and found that the validity and reliability of the health effect estimate can be greatly affected by how we sample the monitor locations. To better understand its effect on second stage inference, we identify two components of preferential sampling that shed light on how preferential sampling alters the properties of the health effect estimate. PMID:29576734

  19. Improved detection of multiple environmental antibiotics through an optimized sample extraction strategy in liquid chromatography-mass spectrometry analysis.

    Science.gov (United States)

    Yi, Xinzhu; Bayen, Stéphane; Kelly, Barry C; Li, Xu; Zhou, Zhi

    2015-12-01

    A solid-phase extraction/liquid chromatography/electrospray ionization/multi-stage mass spectrometry (SPE-LC-ESI-MS/MS) method was optimized in this study for sensitive and simultaneous detection of multiple antibiotics in urban surface waters and soils. Among the seven classes of tested antibiotics, extraction efficiencies of macrolides, lincosamide, chloramphenicol, and polyether antibiotics were significantly improved under optimized sample extraction pH. Instead of only using acidic extraction in many existing studies, the results indicated that antibiotics with low pK a values (antibiotics with high pK a values (>7) were extracted more efficiently under neutral conditions. The effects of pH were more obvious on polar compounds than those on non-polar compounds. Optimization of extraction pH resulted in significantly improved sample recovery and better detection limits. Compared with reported values in the literature, the average reduction of minimal detection limits obtained in this study was 87.6% in surface waters (0.06-2.28 ng/L) and 67.1% in soils (0.01-18.16 ng/g dry wt). This method was subsequently applied to detect antibiotics in environmental samples in a heavily populated urban city, and macrolides, sulfonamides, and lincomycin were frequently detected. Antibiotics with highest detected concentrations were sulfamethazine (82.5 ng/L) in surface waters and erythromycin (6.6 ng/g dry wt) in soils. The optimized sample extraction strategy can be used to improve the detection of a variety of antibiotics in environmental surface waters and soils.

  20. 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)

    Kanekar, A.S.; Pathak, P.N.; Mohapatra, P.K.

    2014-01-01

    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 137 Cs from synthetic soil, cellulose (tissue paper), and plant samples by supercritical fluid extraction (SFE) route. CEs showed poor extraction of 137 Cs from soil matrix. SFE experiments using 1 × 10 -3 M solutions of CMC, CBC and CNC in acetonitrile at 3 M HNO 3 as modifiers displayed better extraction of 137 Cs, viz. 21(±2) % (CMC), 16.5(±3) % (CBC), and 4(±1) % (CNC). It was not possible to recover 137 Cs quantitatively from soil matrix. The inefficient extraction of 137 Cs from soil matrix was attributed to its incorporation into the interstitial sites. Experiments on tissue papers using CMC showed near quantitative 137 Cs recovery. On the other hand, recovery from plant samples varied between 50(±5) % (for stems) and 75(±5) % (for leaves). (author)

  1. 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.

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

    Science.gov (United States)

    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 ...

  3. The use of supercritical fluid extraction as a sample preparation technique for soils

    International Nuclear Information System (INIS)

    Levy, J.M.; Dolata, L.A.; Rosselli, A.C.; Ravey, R.M.

    1994-01-01

    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

  4. Rapid sampling of BTEX in air by SPME in the city of Nice and at the Nice-Cote d'Azur airport

    International Nuclear Information System (INIS)

    Tumbiolo, S.; Gal, J.F.; Maria, P.Ch.; Laborde, P.; Teton, S.

    2006-01-01

    This article presents the results of a tentative application of Solid Phase Micro Extraction (SPME) to the analysis of BTEX (benzene, toluene, ethyl-benzene and xylenes) at the μg/m 3 level in indoor and outdoor air. The salient features of the method validation are reported. Sampling by QUALITAIR using Radiello passive samplers, was carried out from 2001 to 2004 in the city of Nice and its airport. Urban traffic impact was proved, but a link between BTX concentrations and the variations of airport activities was not clearly established. During the same period, several samplings were performed using SPME. Taking into account the short (30 minutes) sampling time, rapid changes of BTEX concentrations were evidenced, as for example the start of airplane engines. As field studies have shown, SPME technique appears as a method of choice for fast qualitative analysis and quantitative determination of Volatile Organic Compounds (VOC). The small dimensions of the SPME sampling system and the short sampling time let envisage its utilisation for the rapid diagnostic and the monitoring of indoor air quality. (author)

  5. 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.

  6. 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. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Sample preparation for avian and porcine influenza virus cDNA amplification simplified: Boilign vs. conventional RNA extraction

    International Nuclear Information System (INIS)

    Fereidouni, S.R.; Starick, E.; Ziller, M.; Harder, T.C.; Unger, H.; Hamilton, K.; Globig, A.

    2016-01-01

    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)

  8. Optimization of microwave-assisted extraction with saponification (MAES) for the determination of polybrominated flame retardants in aquaculture samples.

    Science.gov (United States)

    Fajar, N M; Carro, A M; Lorenzo, R A; Fernandez, F; Cela, R

    2008-08-01

    The efficiency of microwave-assisted extraction with saponification (MAES) for the determination of seven polybrominated flame retardants (polybrominated biphenyls, PBBs; and polybrominated diphenyl ethers, PBDEs) in aquaculture samples is described and compared with microwave-assisted extraction (MAE). Chemometric techniques based on experimental designs and desirability functions were used for simultaneous optimization of the operational parameters used in both MAES and MAE processes. Application of MAES to this group of contaminants in aquaculture samples, which had not been previously applied to this type of analytes, was shown to be superior to MAE in terms of extraction efficiency, extraction time and lipid content extracted from complex matrices (0.7% as against 18.0% for MAE extracts). PBBs and PBDEs were determined by gas chromatography with micro-electron capture detection (GC-muECD). The quantification limits for the analytes were 40-750 pg g(-1) (except for BB-15, which was 1.43 ng g(-1)). Precision for MAES-GC-muECD (%RSD < 11%) was significantly better than for MAE-GC-muECD (%RSD < 20%). The accuracy of both optimized methods was satisfactorily demonstrated by analysis of appropriate certified reference material (CRM), WMF-01.

  9. A system for high-quality CO2 isotope analyses of air samples collected by the CARIBIC Airbus A340-600.

    Science.gov (United States)

    Assonov, S; Taylor, P; Brenninkmeijer, C A M

    2009-05-01

    In 2007, JRC-IRMM began a series of atmospheric CO2 isotope measurements, with the focus on understanding instrumental effects, corrections as well as metrological aspects. The calibration approach at JRC-IRMM is based on use of a plain CO2 sample (working reference CO2) as a calibration carrier and CO2-air mixtures (in high-pressure cylinders) to determine the method-related correction under actual analytical conditions (another calibration carrier, in the same form as the samples). Although this approach differs from that in other laboratories, it does give a direct link to the primary reference NBS-19-CO2. It also helps to investigate the magnitude and nature for each of the instrumental corrections and allows for the quantification of the uncertainty introduced. Critical tests were focused on the instrumental corrections. It was confirmed that the use of non-symmetrical capillary crimping (an approach used here to deal with small samples) systematically modifies delta13C(CO2) and delta18O(CO2), with a clear dependence on the amount of extracted CO2. However, the calibration of CO2-air mixtures required the use of the symmetrical dual-inlet mode. As a proof of our approach, we found that delta13C(CO2) on extracts from mixtures agreed (within 0.010 per thousand) with values obtained from the 'mother' CO2 used for the mixtures. It was further found that very low levels of hydrocarbons in the pumping systems and the isotope ratio mass spectrometry (IRMS) instrument itself were critical. The m/z 46 values (consequently the calculated delta18O(CO2) values) are affected by several other effects with traces of air co-trapped with frozen CO2 being the most critical. A careful cryo-distillation of the extracted CO2 is recommended. After extensive testing, optimisation, and routine automated use, the system was found to give precise data on air samples that can be traced with confidence to the primary standards. The typical total combined uncertainty in delta13C(CO2) and

  10. 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.

  11. Chemosorption sampling and analysis of formaldehyde in air. Influence on recovery during the simultaneous sampling of formaldehyde, phenol, furfural and furfuryl alcohol

    Energy Technology Data Exchange (ETDEWEB)

    Andersson, K.; Hallgren, C.; Levin, J.O.; Nilsson, C.A.

    1981-12-01

    A method based on trapping formaldehyde on a 2,4-dinitrodinitrophenylhydrazine-coated porous polymer (Amberlite XAD-2) was evaluated for air sampling in occupational environments. The aldehyde is converted to its 2,4-dinitrophenylhydrazone on the adsorbent. The influence of some organic compounds which often occur together with formaldehyde-furfural, phenol and furfuryl alcohol--was studied. The results show that the method allows the sampling of formaldehyde in the range 0.01--1.0 mg/m3 of air, based on a 3-1 (15 min) sample and a coating of 1%. Furfural, phenol, and furfuryl alcohol do not interfere and may be conveniently sampled at the same time. Formaldehyde and furfural hydrazones were analyzed by high-performance liquid chromatography, phenol and furfuryl alcohol by gas chromatography.

  12. Nanostructured conducting molecularly imprinted polymer for selective extraction of salicylate from urine and serum samples by electrochemically controlled solid-phase micro-extraction

    International Nuclear Information System (INIS)

    Ameli, Akram; Alizadeh, Naader

    2011-01-01

    Highlights: ► Overoxidized polypyrrole templated with salicylate has been utilized as conducting molecular imprinted polymer for EC-SPME. ► This first study reported on conducting molecular imprinted polymer was used to EC-SPME of salicylate. ► 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 × 10 −8 to 5 × 10 −4 and 1.2 × 10 −6 to 5 × 10 −4 mol mL −1 and the detection limit was 4 × 10 −8 mol L −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.

  13. Validation of a One-Step Method for Extracting Fatty Acids from Salmon, Chicken and Beef Samples.

    Science.gov (United States)

    Zhang, Zhichao; Richardson, Christine E; Hennebelle, Marie; Taha, Ameer Y

    2017-10-01

    Fatty acid extraction methods are time-consuming and expensive because they involve multiple steps and copious amounts of extraction solvents. In an effort to streamline the fatty acid extraction process, this study compared the standard Folch lipid extraction method to a one-step method involving a column that selectively elutes the lipid phase. The methods were tested on raw beef, salmon, and chicken. Compared to the standard Folch method, the one-step extraction process generally yielded statistically insignificant differences in chicken and salmon fatty acid concentrations, percent composition and weight percent. Initial testing showed that beef stearic, oleic and total fatty acid concentrations were significantly lower by 9-11% with the one-step method as compared to the Folch method, but retesting on a different batch of samples showed a significant 4-8% increase in several omega-3 and omega-6 fatty acid concentrations with the one-step method relative to the Folch. Overall, the findings reflect the utility of a one-step extraction method for routine and rapid monitoring of fatty acids in chicken and salmon. Inconsistencies in beef concentrations, although minor (within 11%), may be due to matrix effects. A one-step fatty acid extraction method has broad applications for rapidly and routinely monitoring fatty acids in the food supply and formulating controlled dietary interventions. © 2017 Institute of Food Technologists®.

  14. [Hygienic assessment of a recirculatory combined air-conditioning extract-and-input system in office building].

    Science.gov (United States)

    Malysheva, A G; Abramov, E G

    2006-01-01

    The high concentrations of lead were reveled in the air and dust of some premises and on the filters of a combined air-conditioning extract-and-input system in the high-rise office buildings located in the ecologically lead favorable environment. The dust content of lead in some premises on the first floors dust was as high as 200 mg/kg, which was more than 6 times higher than that in the soil at the highway near the office buildings. The use of new technologies and devices for cleaning and optimizing the air in the premises requires analytical studies to assess the quality of the environment, by taking into account the optimal conditions of their operation.

  15. Sampling problems and the determination of mercury in surface water, seawater, and air

    International Nuclear Information System (INIS)

    Das, H.A.; van der Sloot, H.A.

    1976-01-01

    Analysis of surface water for mercury comprises the determination of both ionic and organically bound mercury in solution and that of the total mercury content of the suspended matter. Eventually, metallic mercury has to be determined too. Requirements for the sampling procedure are given. A method for the routine determination of mercury in surface water and seawater was developed and applied to Dutch surface waters. The total sample volume is 2500 ml. About 500 ml is used for the determination of the content of suspended matter and the total amount of mercury in the water. The sample is filtered through a bed of previously purified active charcoal at a low flow-rate. The main portion ca. 2000 ml) passes a flow-through centrifuge to separate the solid fraction. One liter is used to separate ''inorganic'' mercury by reduction, volatilization in an airstream and adsorption on active charcoal. The other liter is led through a column of active charcoal to collect all mercury. The procedures were checked with 197 Hg radiotracer both as an ion and incorporated in organic compounds. The mercury is determined by thermal neutron activation, followed by volatilization in a tube furnace and adsorption on a fresh carbon bed. The limit of determination is approximately equal to 1 ng 1 -1 . The rate of desorption from and adsorption on suspended material has been measured as a function of a pH of the solution for Hg +2 and various other ions. It can be concluded that only the procedure mentioned above does not disturb the equilibrium. The separation of mercury from air is obtained by suction of 1 m 3 through a 0.22 μm filter and a charcoal bed. The determination is then performed as in the case of the water samples

  16. 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. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Extraction of nucleic acids from yeast cells and plant tissues using ethanol as medium for sample preservation and cell disruption.

    Science.gov (United States)

    Linke, Bettina; Schröder, Kersten; Arter, Juliane; Gasperazzo, Tatiana; Woehlecke, Holger; Ehwald, Rudolf

    2010-09-01

    Here we report that dehydrated ethanol is an excellent medium for both in situ preservation of nucleic acids and cell disruption of plant and yeast cells. Cell disruption was strongly facilitated by prior dehydration of the ethanol using dehydrated zeolite. Following removal of ethanol, nucleic acids were extracted from the homogenate pellet using denaturing buffers. The method provided DNA and RNA of high yield and integrity. Whereas cell wall disruption was essential for extraction of DNA and large RNA molecules, smaller molecules such as tRNAs could be selectively extracted from undisrupted, ethanol-treated yeast cells. Our results demonstrate the utility of absolute ethanol for sample fixation, cell membrane and cell wall disruption, as well as preservation of nucleic acids during sample storage.

  18. Application of the CaF2(Eu) scintillator to 85Kr monitoring in atmospheric air samples

    International Nuclear Information System (INIS)

    Wilhelmova, Ludmila; Dvorak, Zdenek; Tomasek, Milan; Stukheil, Karel

    1986-01-01

    A detection system with a CaF 2 (Eu) scintillator has been developed for monitoring β-radiation of 85 Kr in atmospheric air samples. The geometry of the detector chamber was optimized to achieve maximum detection efficiency. The design of the detector is described and values of the detection efficiency are presented for various compositions and pressures of the gaseous samples. The conditions for calibration of the detector used for monitoring of 85 Kr in enriched air samples have been established. (author)

  19. Air sampling to assess potential generation of aerosolized viable bacteria during flow cytometric analysis of unfixed bacterial suspensions

    Science.gov (United States)

    Carson, Christine F; Inglis, Timothy JJ

    2018-01-01

    This study investigated aerosolized viable bacteria in a university research laboratory during operation of an acoustic-assisted flow cytometer for antimicrobial susceptibility testing by sampling room air before, during and after flow cytometer use. The aim was to assess the risk associated with use of an acoustic-assisted flow cytometer analyzing unfixed bacterial suspensions. Air sampling in a nearby clinical laboratory was conducted during the same period to provide context for the existing background of microorganisms that would be detected in the air. The three species of bacteria undergoing analysis by flow cytometer in the research laboratory were Klebsiella pneumoniae, Burkholderia thailandensis and Streptococcus pneumoniae. None of these was detected from multiple 1000 L air samples acquired in the research laboratory environment. The main cultured bacteria in both locations were skin commensal and environmental bacteria, presumed to have been disturbed or dispersed in laboratory air by personnel movements during routine laboratory activities. The concentrations of bacteria detected in research laboratory air samples were reduced after interventional cleaning measures were introduced and were lower than those in the diagnostic clinical microbiology laboratory. We conclude that our flow cytometric analyses of unfixed suspensions of K. pneumoniae, B. thailandensis and S. pneumoniae do not pose a risk to cytometer operators or other personnel in the laboratory but caution against extrapolation of our results to other bacteria and/or different flow cytometric experimental procedures. PMID:29608197

  20. Magnetic solid-phase extraction of tetracyclines using ferrous oxide coated magnetic silica microspheres from water samples.

    Science.gov (United States)

    Lian, Lili; Lv, Jinyi; Wang, Xiyue; Lou, Dawei

    2018-01-26

    A novel magnetic solid-phase extraction approach was proposed for extraction of potential residues of tetracyclines (TCs) in tap and river water samples, based on Fe 3 O 4 @SiO 2 @FeO magnetic nanocomposite. Characterized results showed that the received Fe 3 O 4 @SiO 2 @FeO had distinguished magnetism and core-shell structure. Modified FeO nanoparticles with an ∼5 nm size distribution were homogeneously dispersed on the surface of the silica shell. Owing to the strong surface affinity of Fe (II) toward TCs, the magnetic nanocomposite could be applied to efficiently extract three TCs antibiotics, namely, oxytetracycline, tetracycline and chlortetracycline from water samples. Several factors, such as sorbent amount, pH condition, adsorption and desorption time, desorption solvent, selectivity and sample volume, influencing the extraction performance of TCs were investigated and optimized. The developed method showed excellent linearity (R > 0.9992) in the range of 0.133-333 μg L -1 , under optimized conditions. The limits of detection were between 0.027 and 0.107 μg L -1 for oxytetracycline, tetracycline and chlortetracycline, respectively. The feasibility of this method was evaluated by analysis of tap and river water samples. The recoveries at the spiked concentration levels ranged from 91.0% to 104.6% with favorable reproducibility (RSD < 4%). Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Recovery of Picloram and 2,4-Dichlorophenoxyacetic Acid from Aqueous Samples by Reversed-Phase Solid-Phase Extraction

    Science.gov (United States)

    Martha J.M. Wells; Jerry L. Michael

    1987-01-01

    Extensive preparation of samples before chromatographic analysis is usually the most time-consuming process in the determination of many organic compounds in environmental matrices. In the past, removal of some organic from aqueous solution was commonly done by liquid/liquid extraction. However, the introduction of stable, covalently bonded reversed-phase sorbents now...

  2. 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

    2012-03-05

    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).

  3. Sample preservation, transport and processing strategies for honeybee RNA extraction: Influence on RNA yield, quality, target quantification and data normalization.

    Science.gov (United States)

    Forsgren, Eva; Locke, Barbara; Semberg, Emilia; Laugen, Ane T; Miranda, Joachim R de

    2017-08-01

    Viral infections in managed honey bees are numerous, and most of them are caused by viruses with an RNA genome. Since RNA degrades rapidly, appropriate sample management and RNA extraction methods are imperative to get high quality RNA for downstream assays. This study evaluated the effect of various sampling-transport scenarios (combinations of temperature, RNA stabilizers, and duration) of transport on six RNA quality parameters; yield, purity, integrity, cDNA synthesis efficiency, target detection and quantification. The use of water and extraction buffer were also compared for a primary bee tissue homogenate prior to RNA extraction. The strategy least affected by time was preservation of samples at -80°C. All other regimens turned out to be poor alternatives unless the samples were frozen or processed within 24h. Chemical stabilizers have the greatest impact on RNA quality and adding an extra homogenization step (a QIAshredder™ homogenizer) to the extraction protocol significantly improves the RNA yield and chemical purity. This study confirms that RIN values (RNA Integrity Number), should be used cautiously with bee RNA. Using water for the primary homogenate has no negative effect on RNA quality as long as this step is no longer than 15min. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Iron oxide functionalized graphene nano-composite for dispersive solid phase extraction of chemical warfare agents from aqueous samples.

    Science.gov (United States)

    Chinthakindi, Sridhar; Purohit, Ajay; Singh, Varoon; Tak, Vijay; Goud, D Raghavender; Dubey, D K; Pardasani, Deepak

    2015-05-15

    Present study deals with the preparation and evaluation of graphene based magnetic nano-composite for dispersive solid phase extraction of Chemical Weapons Convention (CWC) relevant chemicals from aqueous samples. Nano-composite, Fe3O4@SiO2-G was synthesized by covalently bonding silica coated Fe3O4 onto the graphene sheets. Nerve agents (NA), Sulfur mustard (SM) and their non-toxic environmental markers were the target analytes. Extraction parameters like amount of sorbent, extraction time and desorption conditions were optimized. Dispersion of 20 milligram of sorbent in 200mL of water sample for 20min. followed by methanol/chloroform extraction produced average to good recoveries (27-94%) of targeted analytes. Recoveries of real agents exhibited great dependency upon sample pH and ionic strength. Sarin produced maximum recovery under mild acidic conditions (56% at pH 5) while VX demanded alkaline media (83% at pH 9). Salts presence in the aqueous samples was found to be advantageous, raising the recoveries to as high as 94% for SM. Excellent limits of detection (LOD) for sulphur mustard and VX (0.11ngmL(-1) and 0.19ngmL(-1) respectively) proved the utility of the developed method for the off-site analysis of CWC relevant chemicals. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. 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.

  6. Remote control air sampling and fast chemical analysis of the composition

    Energy Technology Data Exchange (ETDEWEB)

    Kukuczka, A; Golisz, T

    1981-01-01

    In 1979 the Central mine rescue station in Bytom (Poland) developed and introduced into use a new method of remote control air and gas (from fires) sampling and swift chemical analysis of the samples' composition. The device in this method includes: a probe (situated beyond the fire detector directly in the control zone), thick-walled elastic hose, direr, piston pump, rotameter, chromatograph and minicomputer. The basic technical data included in the set: the capacity of the pump 8 1/min, 2.5 kg mass. run on 12 V current (built at the Main Mining Affairs Inst. in Poland); the chromatograph is VARIAN 1420-10 (USA produced),the working gas is helium (balloon volume 40 1), feed--alternating 220V, capacity--1.5 kW, time for measuring gas from fires-- 15 to 20 min (as apposed to the 1.5h spent before when the SRC device was being used) at an accuracy of /sup + -/ 0.05% (volume); the chromatograph works with a mini-computer (model CDS-111C) with a 20 kg mass.and a size of 16 x 46 x 56 cm. As tests in Moszczenica coal mines, where a fire in 504/2 occurred, showed (the chromatograph was located 750m from the probe for burning gases), the method proved to be a good one although the VARIAN 1420-10 was insufficiently reliable and the VARIAN-1400-AEROGRAF proved to be better.

  7. Forecasting Urban Air Quality via a Back-Propagation Neural Network and a Selection Sample Rule

    Directory of Open Access Journals (Sweden)

    Yonghong Liu

    2015-07-01

    Full Text Available In this paper, based on a sample selection rule and a Back Propagation (BP neural network, a new model of forecasting daily SO2, NO2, and PM10 concentration in seven sites of Guangzhou was developed using data from January 2006 to April 2012. A meteorological similarity principle was applied in the development of the sample selection rule. The key meteorological factors influencing SO2, NO2, and PM10 daily concentrations as well as weight matrices and threshold matrices were determined. A basic model was then developed based on the improved BP neural network. Improving the basic model, identification of the factor variation consistency was added in the rule, and seven sets of sensitivity experiments in one of the seven sites were conducted to obtain the selected model. A comparison of the basic model from May 2011 to April 2012 in one site showed that the selected model for PM10 displayed better forecasting performance, with Mean Absolute Percentage Error (MAPE values decreasing by 4% and R2 values increasing from 0.53 to 0.68. Evaluations conducted at the six other sites revealed a similar performance. On the whole, the analysis showed that the models presented here could provide local authorities with reliable and precise predictions and alarms about air quality if used at an operational scale.

  8. 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.

  9. Contributions from the data samples in NOC technique on the extracting of the Sq variation

    Science.gov (United States)

    Wu, Yingyan; Xu, Wenyao

    2015-04-01

    The solar quiet daily variation, Sq, a rather regular variation is usually observed at mid-low latitudes on magnetic quiet days or less-disturbed days. It is mainly resulted from the dynamo currents in the ionospheric E region, which are driven by the atmospheric tidal wind and different processes and flow as two current whorls in each of the northern and southern hemispheres[1]. The Sq exhibits a conspicuous day-to-day (DTD) variability in daily range (or strength), shape (or phase) and its current focus. This variability is mainly attributed to changes in the ionospheric conductivity and tidal winds, varying with solar radiation and ionospheric conditions. Furthermore, it presents a seasonal variation and solar cycle variation[2-4]. In generally, Sq is expressed with the average value of the five international magnetic quiet days. Using data from global magnetic stations, equivalent current system of daily variation can be constructed to reveal characteristics of the currents[5]. In addition, using the differences of H component at two stations on north and south side of the Sq currents of focus, Sq is extracted much better[6]. Recently, the method of Natural Orthoganal Components (NOC) is used to decompose the magnetic daily variation and express it as the summation of eigenmodes, and indicate the first NOC eigenmode as the solar quiet daily variation, the second as the disturbance daily variation[7-9]. As we know, the NOC technique can help reveal simpler patterns within a complex set of variables, without designed basic-functions such as FFT technique. But the physical explanation of the NOC eigenmodes is greatly depends on the number of data samples and data regular-quality. Using the NOC method, we focus our present study on the analysis of the hourly means of the H component at BMT observatory in China from 2001 to 2008. The contributions of the number and the regular-quality of the data samples on which eigenmode corresponds to the Sq are analyzed, by

  10. 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.

  11. Simple extraction methods that prevent the artifactual conversion of chlorophyll to chlorophyllide during pigment isolation from leaf samples.

    Science.gov (United States)

    Hu, Xueyun; Tanaka, Ayumi; Tanaka, Ryouichi

    2013-06-19

    thick. However, it may convert a small fraction of chlorophyll a into pheophytin a. Although extraction at sub-zero temperatures is suitable for all plant species examined in this study, this method might be complicated for a large number of samples and it requires liquid nitrogen and equipment for leaf grinding. Using DMF as an extractant is simple and suitable with Arabidopsis samples. However, this solvent cannot completely block the formation of chlorophyllide in thicker leaves.

  12. 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.

  13. Automated on-line liquid–liquid extraction system for temporal mass spectrometric analysis of dynamic samples

    Energy Technology Data Exchange (ETDEWEB)

    Hsieh, Kai-Ta; Liu, Pei-Han [Department of Applied Chemistry, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China); Urban, Pawel L. [Department of Applied Chemistry, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China); Institute of Molecular Science, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China)

    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{sup −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. - Highlights: • Mass spectrometric analysis normally requires sample preparation. • Liquid–liquid extraction can isolate analytes from complex matrices. • The proposed system automates

  14. Automated on-line liquid–liquid extraction system for temporal mass spectrometric analysis of dynamic samples

    International Nuclear Information System (INIS)

    Hsieh, Kai-Ta; Liu, Pei-Han; Urban, Pawel L.

    2015-01-01

    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. - Highlights: • Mass spectrometric analysis normally requires sample preparation. • Liquid–liquid extraction can isolate analytes from complex matrices. • The proposed system automates the

  15. Early Detection of Foot-And-Mouth Disease Virus from Infected Cattle Using A Dry Filter Air Sampling System.

    Science.gov (United States)

    Pacheco, J M; Brito, B; Hartwig, E; Smoliga, G R; Perez, A; Arzt, J; Rodriguez, L L

    2017-04-01

    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 the aerogenous nature of the virus. In the current study, air from rooms housing individual (n = 17) or two groups (n = 4) of cattle experimentally infected with FDMV A24 Cruzeiro of different virulence levels was sampled to assess the feasibility of applying air sampling as a non-invasive, screening tool to identify sources of FMDV infection. Detection of FMDV RNA in air was compared with first detection of clinical signs and FMDV RNA levels in serum and oral fluid. FMDV RNA was detected in room air samples 1-3 days prior (seven animals) or on the same day (four animals) as the appearance of clinical signs in 11 of 12 individually housed cattle. Only in one case clinical signs preceded detection in air samples by one day. Overall, viral RNA in oral fluid or serum preceded detection in air samples by 1-2 days. Six individually housed animals inoculated with attenuated strains did not show clinical signs, but virus was detected in air in one of these cases 3 days prior to first detection in oral fluid. In groups of four cattle housed together, air detection always preceded appearance of clinical signs by 1-2 days and coincided more often with viral shedding in oral fluid than virus in blood. These data confirm that air sampling is an effective non-invasive screening method for detecting FMDV infection in confined to enclosed spaces (e.g. auction barns, milking parlours). This technology could be a useful tool as part of a surveillance strategy during FMD prevention, control or eradication efforts. Published 2015. This article is a U.S. Government work and is in the public domain in the USA.

  16. 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

    2016-09-02

    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. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Rapid fingerprinting and classification of extra virgin olive oil by microjet sampling and extractive electrospray ionization mass spectrometry.

    Science.gov (United States)

    Law, Wai Siang; Chen, Huan Wen; Balabin, Roman; Berchtold, Christian; Meier, Lukas; Zenobi, Renato

    2010-04-01

    Microjet sampling in combination with extractive electrospray ionization (EESI) mass spectrometry (MS) was applied to the rapid characterization and classification of extra virgin olive oil (EVOO) without any sample pretreatment. When modifying the composition of the primary ESI spray solvent, mass spectra of an identical EVOO sample showed differences. This demonstrates the capability of this technique to extract molecules with varying polarities, hence generating rich molecular information of the EVOO. Moreover, with the aid of microjet sampling, compounds of different volatilities (e.g.E-2-hexenal, trans-trans-2,4-heptadienal, tyrosol and caffeic acid) could be sampled simultaneously. EVOO data was also compared with that of other edible oils. Principal Component Analysis (PCA) was performed to discriminate EVOO and EVOO adulterated with edible oils. Microjet sampling EESI-MS was found to be a simple, rapid (less than 2 min analysis time per sample) and powerful method to obtain MS fingerprints of EVOO without requiring any complicated sample pretreatment steps.

  18. Air-assisted dispersive liquid-liquid microextraction based on a new hydrophobic deep eutectic solvent for the preconcentration of benzophenone-type UV filters from aqueous samples.

    Science.gov (United States)

    Ge, Dandan; Zhang, Yi; Dai, Yixiu; Yang, Shumin

    2018-04-01

    Deep eutectic solvents are considered as new and green solvents that can be widely used in analytical chemistry such as microextraction. In the present work, a new dl-menthol-based hydrophobic deep eutectic solvent was synthesized and used as extraction solvents in an air-assisted dispersive liquid-liquid microextraction method for preconcentration and extraction of benzophenone-type UV filters from aqueous samples followed by high-performance liquid chromatography with diode array detection. In an experiment, the deep eutectic solvent formed by dl-menthol and decanoic acid was added to an aqueous solution containing the UV filters, and then the mixture was sucked up and injected five times by using a glass syringe, and a cloudy state was achieved. After extraction, the solution was centrifuged and the upper phase was subjected to high-performance liquid chromatography for analysis. Various parameters such as the type and volume of the deep eutectic solvent, number of pulling, and pushing cycles, solution pH and salt concentration were investigated and optimized. Under the optimum conditions, the developed method exhibited low limits of detection and limits of quantitation, good linearity, and precision. Finally, the proposed method was successfully applied to determine the benzophenone-type filters in environmental water samples with relative recoveries of 88.8-105.9%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. As, Cd, Cr, Ni and Pb pressurized liquid extraction with acetic acid from marine sediment and soil samples

    International Nuclear Information System (INIS)

    Moreda-Pineiro, Jorge; Alonso-Rodriguez, Elia; Lopez-Mahia, Purificacion; Muniategui-Lorenzo, Soledad; Prada-Rodriguez, Dario; Moreda-Pineiro, Antonio; Bermejo-Barrera, Adela; Bermejo-Barrera, Pilar

    2006-01-01

    Rapid leaching procedures by Pressurized Liquid Extraction (PLE) have been developed for As, Cd, Cr, Ni and Pb leaching from environmental matrices (marine sediment and soil samples). The Pressurized Liquid Extraction is completed after 16 min. The released elements by acetic acid Pressurized Liquid Extraction have been evaluated by inductively coupled plasma-optical emission spectrometry. The optimum multi-element leaching conditions when using 5.0 ml stainless steel extraction cells, were: acetic acid concentration 8.0 M, extraction temperature 100 deg. C, pressure 1500 psi, static time 5 min, flush solvent 60%, two extraction steps and 0.50 g of diatomaceous earth as dispersing agent (diatomaceous earth mass/sample mass ratio of 2). Results have showed that high acetic acid concentrations and high extraction temperatures increase the metal leaching efficiency. Limits of detection (between 0.12 and 0.5 μg g -1 ) and repeatability of the over-all procedure (around 6.0%) were assessed. Finally, accuracy was studied by analyzing PACS-2 (marine sediment), GBW-07409 (soil), IRANT-12-1-07 (cambisol soil) and IRANT-12-1-08 (luvisol soil) certified reference materials (CRMs). These certified reference materials offer certified concentrations ranges between 2.9 and 26.2 μg g -1 for As, from 0.068 to 2.85 μg g -1 for Cd, between 26.4 and 90.7 μg g -1 for Cr, from 9.3 to 40.0 μg g -1 for Ni and between 16.3 and 183.0 μg g -1 for Pb. Recoveries after analysis were between 95.7 and 105.1% for As, 96.2% for Cd, 95.2 and 100.6% for Cr, 95.7 and 103% for Ni and 94.2 and 105.5% for Pb

  20. Molecularly Imprinted Polymers (MIP for Selective Solid Phase Extraction of Celecoxib in Urine Samples Followed by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Saeedeh Ansari

    2017-09-01

    Full Text Available In this study, for the analysis of human urine samples, a novel method explained for the determination of celecoxib, a nonsteroidal anti-inflammatory drug (NSAID, using molecularly imprinted solid-phase extraction (MISPE coupled with high-performance liquid chromatography (HPLC. The synthesis of the MIP was performed by precipitation polymerization in methacrylic acid (MAA, ethylene glycol dimethacrylate (EGDMA, chloroform, 2,2′-azobisisobutyronitrile (AIBN and celecoxib as the functional monomer, cross-linker monomer, solvent, initiator and target drug, respectively. The celecoxib imprinted polymer was utilized as a specific sorbent for the solid phase extraction (SPE of celecoxib from samples. The molecularly imprinted polymer (MIP performance was compared with the synthesized non-molecularly imprinted polymer (NIP. Scanning electron microscopy (SEM, FT-IR spectroscopy, UV-VIS spectrophotometry and thermogravimetric analysis (TGA/DTG were used for characterizing the synthesized polymers. Moreover, the MISPE procedure parameters such as pH, eluent solvent flow rate, eluent volume and sorbent mass that probably influence the extraction process have been optimized to achieve the highest celecoxib extraction efficiency. The relative standard deviation (RSD %, recovery percent, limit of detection (LOD and limit of quantification (LOQ of this proposed method were 1.12%, 96%, 8 µg L-1 and 26.7 µg L-1, respectively. The proposed MISPE-HPLC-UV method can be used for the separation and enrichment of trace amounts of celecoxib in human urine and biological samples.

  1. Surfactant assisted pulsed two-phase electromembrane extraction followed by GC analysis for quantification of basic drugs in biological samples.

    Science.gov (United States)

    Zahedi, Pegah; Davarani, Saied Saeed Hosseiny; Moazami, Hamid Reza; Nojavan, Saeed

    2016-01-05

    In this work, a simple and efficient surfactant assisted pulsed two-phase electromembrane extraction (SA-PEME) procedure combined with gas chromatography (GC) has been developed for the determination of alfentanil, sufentanil and methadone in various samples. It has been found that the addition of anionic surfactant causes the accumulation of the cationic analytes at the SLM/solution interface resulting in an easier transfer of the analytes into the organic phase. The method was accomplished with 1-octanol as the acceptor phase and supported liquid membrane (SLM) by means of an 80 V pulsed electrical driving force and the extraction time of 20 min. The model analytes were extracted from 3.0 mL sample solution (pH 4.0) containing 0.02% w/v surfactant (sodium dodecyl sulfate). The duty cycle of 92% and frequency of 0.357 Hz gave the best performance. Extraction recoveries in the range of 70.5-95.2% and satisfactory repeatability (7.6samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. The contents of fifteen essential, trace and toxic elements in some green tea samples and in their aqueous extracts

    International Nuclear Information System (INIS)

    Memon, A.N.; Kazi, T.G.

    2002-01-01

    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)

  3. Extraction methods for determination of Pu and Am contents in soil samples from the Chernobyl' NPP 30-km zone

    International Nuclear Information System (INIS)

    Shvetsov, I.K.; Yakovlev, N.G.; Kalinichenko, B.S.; Kulakov, V.M.; Kulazhko, V.G.; Vlasov, M.M.; Shubko, V.M.; Pchelkin, V.A.; Rodionov, Yu.F.; Lisin, S.K.

    1989-01-01

    The possibilities for decreasing the time of soil sample analysis for Pu, Am, Cm isotope concentrations with simultaneous increasing the sensitivity and analysis representativity are demonstrated. It is achieved due to changing the total sample break-down by oxidizing leaching, and the procedure of ion-exchange separation by single extraction using trioctylamine. Experience in the method applications for analysis of soil samples in the Chernobyl' NPP 30-km zone aimed at determination of correlation coefficients for Pu/Ce-144 and Pu/Am-241 is generalized. 4 refs.; 4 figs.; 1 tab

  4. Sequential extraction procedure for determination of uranium, thorium, radium, lead and polonium radionuclides by alpha spectrometry in environmental samples

    Science.gov (United States)

    Oliveira, J. M.; Carvalho, F. P.

    2006-01-01

    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® 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).

  5. Potential contamination of shipboard air samples by diffusive emissions of PCBs and other organic pollutants: implications and solutions.

    Science.gov (United States)

    Lohmann, Rainer; Jaward, Foday M; Durham, Louise; Barber, Jonathan L; Ockenden, Wendy; Jones, Kevin C; Bruhn, Regina; Lakaschus, Soenke; Dachs, Jordi; Booij, Kees

    2004-07-15

    Air samples were taken onboard the RRS Bransfield on an Atlantic cruise from the United Kingdom to Halley, Antarctica, from October to December 1998, with the aim of establishing PCB oceanic background air concentrations and assessing their latitudinal distribution. Great care was taken to minimize pre- and post-collection contamination of the samples, which was validated through stringent QA/QC procedures. However, there is evidence that onboard contamination of the air samples occurred,following insidious, diffusive emissions on the ship. Other data (for PCBs and other persistent organic pollutants (POPs)) and examples of shipboard contamination are presented. The implications of these findings for past and future studies of global POPs distribution are discussed. Recommendations are made to help critically appraise and minimize the problems of insidious/diffusive shipboard contamination.

  6. 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 ......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 sensitivity of detection of Campylobacter in air is comparable to that in other sample materials. Profiling of airborne particles in six poultry houses revealed that the aerodynamic conditions were dependent on the age of the chickens and very comparable among different poultry houses, with low proportions...

  7. Work Plan for the Evaluation of Soil Vapor Extraction Using Internal Combustion Engine Technology at Site SS-42 Luke Air Force Base, Arizona

    National Research Council Canada - National Science Library

    1996-01-01

    ...). Luke AFB is one of several Air Force installations identified as prospective test sites to demonstrate the ICE system with advanced emission controls as part of a low-cost soil vapor extraction (SVE...

  8. Noninvasive genetic sampling of endangered muriqui (Primates, Atelidae: efficiency of fecal DNA extraction

    Directory of Open Access Journals (Sweden)

    Paulo B. Chaves

    2006-01-01

    Full Text Available The muriqui (Brachyteles is one of the most endangered primates in the world, however little is known about the viability of the remaining populations. We evaluated the technique of extracting DNA from wild muriqui feces for PCR applications. In order to determine the effect of the DNA in subsequent amplifications, we analyzed five different extracts. The importance of the recommended BSA and the HotStarTaq DNA polymerase was tested. The minimal conditions to successfully amplify highly degraded fecal DNA were determined, showing that the recommended reagents are not required. We envision that this method may be useful in further conservation management studies.

  9. Air sampling procedures to evaluate microbial contamination: a comparison between active and passive methods in operating theatres.

    Science.gov (United States)

    Napoli, Christian; Marcotrigiano, Vincenzo; Montagna, Maria Teresa

    2012-08-02

    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. 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). 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. 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.

  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. 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.

  12. Analysis of water extracts from airborne dust samples by capillary isotachophoresis

    Czech Academy of Sciences Publication Activity Database

    Sázelová, Petra; Kašička, Václav; Koval, Dušan; Kilár, F.; Knopp, D.; Peltre, G.

    2003-01-01

    Roč. 990, - (2003), s. 303-309 ISSN 0021-9673 R&D Projects: GA MŠk OK 382 Grant - others:INCO-Copernicus(XE) ERB-IC15-CT98-0322 Institutional research plan: CEZ:AV0Z4055905 Keywords : isotachophoresis * dust * air analysis Subject RIV: CC - Organic Chemistry Impact factor: 2.922, year: 2003

  13. Comparison of halocarbon measurements in an atmospheric dry whole air sample.

    Science.gov (United States)

    Rhoderick, George C; Hall, Bradley D; Harth, Christina M; Kim, Jin Seog; Lee, Jeongsoon; Montzka, Stephen A; Mühle, Jens; Reimann, Stefan; Vollmer, Martin K; Weiss, Ray