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Sample records for additional sample clean-up

  1. Glufosinate ammonium clean-up procedure from water samples using SPE

    NASA Astrophysics Data System (ADS)

    Tayeb M., A.; Ismail B., S.; Mardiana-Jansar, K.; Ta, Goh Choo; Agustar, Hani Kartini

    2015-09-01

    For the determination of glufosinate ammonium residue in soil and water samples, different solid phase extraction (SPE) sorbent efficiency was studied. Four different SPE sorbents i.e.: CROMABOND PS-H+, CROMABOND PS-OH-, ISOLUTE ENV+, Water Sep-Pak and OASIS HLB were used. Sample clean-up performance was evaluated using high performance liquid chromatography (Agilent 1220 infinity LC) with fluorescence detector. Detection of FMO-derivatives was done at λ ex = 260 nm and λ em= 310 nm. OASIS HLB column was the most suitable for the clean-up in view of the overall feasibility of the analysis.

  2. Determination of amphetamines in hair by integrating sample disruption, clean-up and solid phase derivatization.

    PubMed

    Argente-García, A; Moliner-Martínez, Y; Campíns-Falcó, P; Verdú-Andrés, J; Herráez-Hernández, R

    2016-05-20

    The utility of matrix solid phase dispersion (MSPD) for the direct analysis of amphetamines in hair samples has been evaluated, using liquid chromatography (LC) with fluorescence detection and precolumn derivatization. The proposed approach is based on the employment of MSPD for matrix disruption and clean-up, followed by the derivatization of the analytes onto the dispersant-sample blend. The fluorogenic reagent 9-fluorenylmethyl chloroformate (FMOC) has been used for derivatization. Different conditions for MSPD, analyte purification and solid phase derivatization have been tested, using amphetamine (AMP), methamphetamine (MET), ephedrine (EPE) and 3,4-methylenedioxymethamphetamine (MDMA) as model compounds. The results have been compared with those achieved by using ultrasound-assisted alkaline digestion and by MSPD combined with conventional solution derivatization. On the basis of the results obtained, a methodology is proposed for the analysis of amphetamines in hair which integrates sample disruption, clean-up and derivatization using a C18 phase. Improved sensitivity is achieved with respect to that obtained by the alkaline digestion or by the MSPD followed by solution derivatization methods. The method can be used for the quantification of the tested amphetamines within the 2.0-20.0ng/mg concentration interval, with limits of detection (LODs) of 0.25-0.75ng/mg. The methodology is very simple and rapid (the preparation of the sample takes less than 15min).

  3. Comparison of solid-phase extraction sorbents for sample clean-up in the analysis of organic explosives.

    PubMed

    Tachon, Romain; Pichon, Valérie; Barbe Le Borgne, Martine; Minet, Jean-Jacques

    2008-03-21

    A solid-phase extraction procedure was developed for the clean-up of forensic samples collected at bombing scenes. Recoveries of common organic explosives from methanolic extracts diluted with water were studied on different hydrophobic sorbents. Polymeric sorbents retained explosive compounds better than octadecyl-bonded silica-based materials. Clean-up efficiency was evaluated with simulated samples prepared from commercial motor oil. Polymeric sorbent with the smallest specific surface area was found to limit the coextraction of matrix components. Performance of the method was confirmed by a reduction of ion suppression in LC/MS analysis.

  4. A Membrane-Based Electro-Separation Method (MBES) for Sample Clean-Up and Norovirus Concentration

    PubMed Central

    Kang, Wei; Cannon, Jennifer L.

    2015-01-01

    Noroviruses are the leading cause of acute gastroenteritis and foodborne illnesses in the United States. Enhanced methods for detecting noroviruses in food matrices are needed as current methods are complex, labor intensive and insensitive, often resulting in inhibition of downstream molecular detection and inefficient recovery. Membrane-based electro-separation (MBES) is a technique to exchange charged particles through a size-specific dialysis membrane from one solution to another using electric current as the driving force. Norovirus has a net negative surface charge in a neutrally buffered environment, so when placed in an electric field, it moves towards the anode. It can then be separated from the cathodic compartment where the sample is placed and then collected in the anodic compartment for downstream detection. In this study, a MBES-based system was designed, developed and evaluated for concentrating and recovering murine norovirus (MNV-1) from phosphate buffer. As high as 30.8% MNV-1 migrated from the 3.5 ml sample chamber to the 1.5 ml collection chamber across a 1 μm separation membrane when 20 V was applied for 30 min using 20 mM sodium phosphate with 0.01% SDS (pH 7.5) as the electrolyte. In optimization of the method, weak applied voltage (20 V), moderate duration (30 min), and low ionic strength electrolytes with SDS addition were needed to increase virus movement efficacy. The electric field strength of the system was the key factor to enhance virus movement, which could only be improved by shortening the electrodes distance, instead of increasing system applied voltage because of virus stability. This study successfully demonstrated the norovirus mobility in an electric field and migration across a size-specific membrane barrier in sodium phosphate electrolyte. With further modification and validation in food matrixes, a novel, quick, and cost-effective sample clean-up technique might be developed to separate norovirus particles from food

  5. Compliance Sampling Applications in MEC Clean-Up at Military Training Sites

    SciTech Connect

    Hathaway, J.; Gilbert, Richard O.; Wilson, John E.; Pulsipher, Brent A.

    2008-01-31

    Millions of acres of Department of Defense (DoD) closed, transferred and transferring ranges may contain munitions and explosives of concern (MEC) (General Accounting Office, 2001). It is usually necessary to conduct geophysical surveys to search for MEC at these ranges before they can be released from DoD control for other uses. The process of searching for and removing MEC should be carefully planned to follow a quality control process to achieve cleanup goals. After detected MEC have been removed, a confirmation survey of the cleaned areas may be conducted to increase confidence in the cleanup process. These confirmation surveys are the focus of this paper. One possible statistically-based approach for conducting a confirmation survey is to use “accept-on-zero” attribute compliance sampling (AOZ ACS) (Schilling 1978, 1982; Squeglia, 1994). This approach involves conducting an inspection or sampling of a random selection of n “units” from among the total number of units (N) for a site. For example, the site may be divided into N non-overlapping 200ft x 200ft land areas (grids), n of which are randomly selected and inspected for MEC (n < N). The number n is statistically determined by specifying N and the confidence required that no more than Y% of the 200ft x 200ft units contain MEC. An example is provided by Williams (2003) for a site near Denver, Colorado. He describes the use of process quality control and AOZ ACS as it is laid out in Military-Standard-1916 (DoD 1996, 1999). The purpose of this paper is to (i) provide the mathematical foundation of AOZ ACS and an equation that can be used to compute n, (ii) discuss the pros and cons of AOZ ACS when units are defined to be either individual transects or anomalies, and (iii) present the results of simulation studies conducted to investigate the performance of AOZ ACS when individual transects are not randomly selected and there is a non-random spatial pattern of MEC. Goals (ii) and (iii) are of

  6. Water compatible stir-bar devices imprinted with underivatised glyphosate for selective sample clean-up.

    PubMed

    Gomez-Caballero, Alberto; Diaz-Diaz, Goretti; Bengoetxea, Olatz; Quintela, Amaia; Unceta, Nora; Goicolea, M Aranzazu; Barrio, Ramón J

    2016-06-17

    This paper reports the development of stir bars with a new MIP based coating, for the selective sorptive extraction of the herbicide glyphosate (GLYP). Molecular imprinting of the polymer has directly been carried out employing underivatised GLYP as the template molecule. Due to the poor solubility of the target compound in organic solvents, the MIP methodology has been optimised for rebinding in aqueous media, being the synthesis and the rebinding steps carried out in water:methanol mixtures and pure aqueous media. The coating has been developed by radical polymerisation initiated by UV energy, using N-allylthiourea and 2-dimethyl aminoethyl methacrylate as functional monomers and ethylene glycol dimethacrylate as the cross-linker. Mechanical stability of the coating has been improved using 1,3-divinyltetramethyldisiloxane in the polymerisation mixture. Under the optimised conditions, the MIP has demonstrated excellent selectivity for the target compound in the presence of structural analogues, including its major metabolites. The applicability of the proposed method to real matrices has also been assessed using river water and soil samples. Registered mean recoveries ranged from 90.6 to 97.3% and RSD values were below 5% in all cases, what confirmed the suitability of the described methodology for the selective extraction and quantification of GLYP.

  7. Determination of carbendazim, thiabendazole, and o-phenylphenol residues in lemons by HPLC following sample clean-up by ion-pairing.

    PubMed

    Prousalis, Konstantinos P; Polygenis, Dimitris A; Syrokou, Alexandra; Lamari, Fotini N; Tsegenidis, Theodore

    2004-06-01

    An efficient analytical method is presented involving effective sample clean-up with solid-phase extraction and HPLC-UV analysis for the simultaneous determination of carbendazim, thiabendazole, and o-phenylphenol residues in lemons. Sample preparation involves extraction with acetonitrile acidified with trifluoroacetic acid and an ethyl acetate/petroleum ether mixture. Purification of the crude extract was carried out with liquid-liquid partitioning after addition of an aqueous ammonia solution. Final clean-up was performed on polymeric reversed-phase cartridges pretreated with sodium dodecyl sulfate. Chromatographic analysis was performed on a reversed-phase HPLC column isocratically eluted with an acetonitrile/water/ammonia mixture and UV detection at 254 nm. The chromatographic method is repeatable, reproducible, and sensitive. Fungicide recoveries from lemon samples fortified at levels of 5 and 1 mg kg(-1) were 81-85% for carbendazim, 96-98% for thiabendazole, and 81-106% for o-phenylphenol with coefficients of variation of 2.5-7.4%. Detection limits for carbendazim, thiabendazole, and o-phenylphenol in lemons were 0.21, 0.27, and 0.51 mg kg(-1), respectively.

  8. Improved sample extraction and clean-up for the GC-MS determination of BADGE and BFDGE in vegetable oil.

    PubMed

    Brede, C; Skjevrak, I; Herikstad, H; Anensen, E; Austvoll, R; Hemmingsen, T

    2002-05-01

    A straightforward method was established for the determination of migration contaminants in olive oil with a special focus on the two can-coating migration compounds bisphenol A diglycidyl ether (BADGE) and bisphenol F diglycidyl ether (BFDGE). The preferred sample preparation was a single liquid-liquid extraction of compounds from the oil into 20% (v/v) methanol in acetonitrile, followed by clean-up with solid-phase extraction on aminopropyl bonded to silica. This purification procedure selectively removed all free fatty acids from the extracts without removing phenolic compounds of interest. The solid-phase extraction columns were used many times by implementing a procedure of washing out the strongly retained fatty acids with 2% acetic acid in methanol. Gas chromatography coupled with full scan (m/z 33-700) electron ionization mass spectrometry was used for the determination of several model compounds in olive oil samples. BADGE and BFDGE could be determined in the 0.05-2 mg kg(-1) range in oil samples with a relative SD of <6% (six replicates). The method was used in an enforcement campaign for the Norwegian Food Control Authority to analyse vegetable oil samples from canned fish-in-oil.

  9. Efficient sample clean-up and online preconcentration for sensitive determination of melamine in milk samples by capillary electrophoresis with contactless conductivity detection.

    PubMed

    Ji, Yan-ling; Chen, Xiao-wei; Zhang, Zhu-bao; Li, Jing; Xie, Tian-yao

    2014-10-01

    Based on an efficient sample clean-up and field-amplified sample injection online preconcentration technique in capillary electrophoresis with contactless conductivity detection, a new analytical method for the sensitive determination of melamine in milk samples was established. In order to remove the complex matrix interference, which resulted in a serious problem during field-amplified sample injection, liquid-liquid extraction was utilized. As a result, liquid-liquid extraction provides excellent sample clean-up efficiency when ethyl acetate was used as organic extraction by adjusting the pH of the sample solution to 9.5. Both inorganic salts and biological macromolecules are effectively removed by liquid-liquid extraction. The sample clean-up procedure, capillary electrophoresis separation parameters and field-amplified sample injection conditions are discussed in detail. The capillary electrophoresis separation was achieved within 5 min under the following conditions: an uncoated fused-silica capillary, 12 mM HAc + 10 mM NaAc (pH = 4.6) as running buffer, separation voltage of +13 kV, electrokinetic injection of +12 kV × 10 s. Preliminary validation of the method performance with spiked melamine provided recoveries >90%, with limits of detection and quantification of 0.015 and 0.050 mg/kg, respectively. The relative standard deviations of intra- and inter-day were below 6%. This newly developed method is sensitive and cost effective, therefore, suitable for screening of melamine contamination in milk products.

  10. A LC/UV/Vis method for determination of cyanocobalamin in multivitamin dietary supplements with on-line sample clean-up

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A HPLC-UV method using a two-column strategy with a switching valve for on-line sample clean-up was developed for the determination of cyanocobalamin (CN-CBL-vitamin B12, in dietary supplements. The method uses two columns, an Agilent Zorbax C8 (150 mm x 4.6 mm, 5 um particle) reversed-phase column...

  11. Cloud point sample clean-up and capillary zone electrophoresis with field enhanced sample injection and micelle to solvent stacking for the analysis of herbicides in milk.

    PubMed

    Kukusamude, Chunyapuk; Srijaranai, Supalax; Kato, Masaru; Quirino, Joselito P

    2014-07-18

    Sample clean-up by cloud point phase separation and analysis by capillary electrophoresis with stacking was developed for quaternary ammonium herbicides (i.e., paraquat and diquat) in milk. For sample clean-up, a mixture of 845μL of milk sample, 5μL of 100mM phosphoric acid, and 150μL of Triton X-114 was heated (60°C for 2min) and centrifugated (3000rpm for 2min) in 2-mL Eppendorf tube. The upper phase was directly analysed by capillary electrophoresis via electrokinetic injection at 10kV for 150s. The separation electrolyte was 100mM phosphate buffer with 20% acetonitrile at pH 2.5. Before sample injection, a micellar solution (10mM SDS in 80mM phosphate buffer at pH 2.5) and an organic solvent rich solution (30% ACN) was hydrodynamically introduced into the capillary. These solutions provided the necessary conditions for stacking the cationic herbicides via the combination of field enhanced sample injection and micelle to solvent stacking. The LODs (S/N=3) obtained from the entire strategy for paraquat and diquat in milk was 0.004 and 0.018μg/mL, respectively. This is 1.5 to >2 orders of magnitude better than the corresponding LODs obtained from the electrophoretic analysis of herbicide standards prepared in the separation electrolyte. The strategy was also successfully applied to 5 milk samples available in the market.

  12. Determination of deoxynivalenol and deoxynivalenol-3-glucoside in wheat and barley using liquid chromatography coupled to mass spectrometry: on-line clean-up versus conventional sample preparation techniques.

    PubMed

    Nathanail, Alexis V; Sarikaya, Ebru; Jestoi, Marika; Godula, Michal; Peltonen, Kimmo

    2014-12-29

    In this study, we compared the performance of conventional sample preparation techniques used in mycotoxin analyses against automated on-line sample clean-up for the determination of deoxynivalenol (DON) and its conjugated derivative, deoxynivalenol-3-β-d-glucoside (D3G), in cereal grains. Blank wheat and barley samples were spiked with DON and D3G, extracted with a mixture of acetonitrile:water (84:16, v/v) and processed by one of the following: extract and shoot, MycoSep(®) 227 clean-up columns, MycoSep 227 with an additional acetonitrile elution step and centrifugal filtration, followed by analysis with liquid chromatography tandem mass spectrometry. Based on method performance characteristics and poor recoveries (<30%) obtained for the polar D3G with some techniques, the extract and shoot approach was chosen for the inter-laboratory method comparison study. Thus, the same spiked samples were analysed in parallel by another laboratory with an in-house validated on-line sample clean-up method, utilising TurboFlow™ chromatography coupled to high resolution mass spectrometry. Method validation was performed by determination of specificity, linearity, recovery, intra-day precision and the limits of detection and quantification. Matrix-matched linearity (R(2)>0.985) was established in the range of 100-1600 and 20-320μg/kg for DON and D3G, respectively. Average recoveries (%RSD) were acceptable with both methods for wheat and barley, ranging between 73% and 102% (3-12%) for DON and 72% and 98% (1-10%) for D3G. The benefit of using automated sample clean-up in comparison to extract and shoot is the ability to inject directly pure extracts into the mass spectrometer, offering faster analyses and improved sensitivity with minimum system maintenance.

  13. In-house validation of an improved sample extraction and clean-up method for GC determination of isomers of nervonic acid in meat products.

    PubMed

    Agazzi, Marie-Elisabeth; Bau, Andrea; Barcarolo, Robertino; Luecker, Ernst; Barrero-Moreno, Josefa; Anklam, Elke

    2003-06-01

    An improved extraction and clean-up method for determination of brain-specific fatty acids, in particular lignoceric acid (C24:0) and the cis/ trans isomers of nervonic acid (15 c-t C24:1), in meat products has been developed. The method is based on isolation of the polar lipids of interest from the bulk lipids by solid-phase extraction. The fatty acids, derivatised to their fatty acid methyl esters, are quantified by GC in a DB5 column. Fresh meat samples were extracted by using a mixture of n-butanol:hexane (1:9) as solvent. The extract was loaded in a silica gel cartridge column previously equilibrated with hexane. The first fraction containing the major part of the fat was eluted with hexane while acetone and methanol allowed the elution of fatty acids bound to polar moieties such as nervonic and lignoceric acids. This second fraction containing the analyte was methylated and injected into the GC for quantification after addition octacosane (C(28)) as internal standard.

  14. Ion Mobility Mass Spectrometry for Ion Recovery and Clean-Up of MS and MS/MS Spectra Obtained from Low Abundance Viral Samples

    NASA Astrophysics Data System (ADS)

    Harvey, David J.; Crispin, Max; Bonomelli, Camille; Scrivens, Jim H.

    2015-07-01

    Many samples of complex mixtures of N-glycans released from small amounts of material, such as glycoproteins from viruses, present problems for mass spectrometric analysis because of the presence of contaminating material that is difficult to remove by conventional methods without involving sample loss. This study describes the use of ion mobility for extraction of glycan profiles from such samples and for obtaining clean CID spectra when targeted m/z values capture additional ions from those of the target compound. N-glycans were released enzymatically from within SDS-PAGE gels, from the representative recombinant glycoprotein, gp120 of the human immunodeficiency virus, and examined by direct infusion electrospray in negative mode followed by ion mobility with a Waters Synapt G2 mass spectrometer (Waters MS-Technologies, Manchester, UK). Clean profiles of singly, doubly, and triply charged N-glycans were obtained from samples in cases where the raw electrospray spectra displayed only a few glycan ions as the result of low sample concentration or the presence of contamination. Ion mobility also enabled uncontaminated CID spectra to be obtained from glycans when their molecular ions displayed coincidence with ions from fragments or multiply charged ions with similar m/z values. This technique proved to be invaluable for removing extraneous ions from many CID spectra. The presence of such ions often produces spectra that are difficult to interpret. Most CID spectra, even those from abundant glycan constituents, benefited from such clean-up, showing that the extra dimension provided by ion mobility was invaluable for studies of this type.

  15. Coupling of acetonitrile deproteinization and salting-out extraction with acetonitrile stacking for biological sample clean-up and the enrichment of hydrophobic compounds (porphyrins) in capillary electrophoresis.

    PubMed

    Li, Qi; Huie, Carmen W

    2006-11-01

    A new sample pretreatment approach in CE was developed for concurrent biological sample clean-up and the concentration of hydrophobic compounds based on the combination of ACN deproteinization with salting-out extraction. Further enhancement in concentration detection sensitivity was achieved by coupling (offline) salting-out extraction with an online CE sample enrichment technique known as "ACN stacking". By optimizing the pH of salting-out extraction, a number of model compounds (hydrophobic porphyrins with clinical significances), i.e. zinc-protoporphyrin, protoporphyrin, and coproporphyrin (CP) III and I, can be efficiently extracted from the aqueous sample into a smaller volume organic solvent (ACN) phase and an enrichment factor of ca. 100 can be obtained. The pressure injection of the enriched ACN phase (containing ca.1% NaCl) into the CE capillary at 10% capillary volume resulted in additional concentration of the various hydrophobic porphyrins, allowing for a combined enrichment factor of ca.1000 to be obtained. Calibration curves obtained for the determination of a pair of positional isomers with significant diagnostic value, urinary CPIII and CPI, were found to be linear between 10-300 ng/mL (with R2 = 0.999), and LODs (absorbance detection at 400 nm) were ca. 0.8 ng/mL (1.1 nmol/L of CPIII or CPI). Based on a single salting-out extraction, intraday precisions (nine consecutive injections) for both CPIII and CPI (at spiked concentrations of 10-300 ng/mL into urine) in terms of migration time and peak area were found to be within the range of 0.2-0.5 and 0.8-2.9%, respectively.

  16. Development of sample preparation method for auxin analysis in plants by vacuum microwave-assisted extraction combined with molecularly imprinted clean-up procedure.

    PubMed

    Hu, Yuling; Li, Yuanwen; Zhang, Yi; Li, Gongke; Chen, Yueqin

    2011-04-01

    A novel sample preparation method for auxin analysis in plant samples was developed by vacuum microwave-assisted extraction (VMAE) followed by molecularly imprinted clean-up procedure. The method was based on two steps. In the first one, conventional solvent extraction was replaced by VMAE for extraction of auxins from plant tissues. This step provided efficient extraction of 3-indole acetic acid (IAA) from plant with dramatically decreased extraction time, furthermore prevented auxins from degradation by creating a reduced oxygen environment under vacuum condition. In the second step, the raw extract of VMAE was further subjected to a clean-up procedure by magnetic molecularly imprinted polymer (MIP) beads. Owing to the high molecular recognition ability of the magnetic MIP beads for IAA and 3-indole-butyric acid (IBA), the two target auxins in plants can be selectively enriched and the interfering substance can be eliminated by dealing with a magnetic separation procedure. Both the VMAE and the molecularly imprinted clean-up conditions were investigated. The proposed sample preparation method was coupled with high-performance liquid chromatogram and fluorescence detection for determination of IAA and IBA in peas and rice. The detection limits obtained for IAA and IBA were 0.47 and 1.6 ng/mL and the relative standard deviation were 2.3% and 2.1%, respectively. The IAA contents in pea seeds, pea embryo, pea roots and rice seeds were determined. The recoveries were ranged from 70.0% to 85.6%. The proposed method was also applied to investigate the developmental profiles of IAA concentration in pea seeds and rice seeds during seed germination.

  17. Determination of triazine herbicides in seaweeds: development of a sample preparation method based on Matrix Solid Phase Dispersion and Solid Phase Extraction Clean-up.

    PubMed

    Rodríguez-González, N; González-Castro, M J; Beceiro-González, E; Muniategui-Lorenzo, S; Prada-Rodríguez, D

    2014-04-01

    A method using dual process columns of Matrix Solid Phase Dispersion (MSPD) and Solid Phase Extraction (SPE) has been developed for extracting and cleaning-up of nine triazine herbicides (ametryn, atrazine, cyanazine, prometryn, propazine, simazine, simetryn, terbuthylazine and terbutryn) in seaweed samples. Under optimized conditions, samples were blended with 2g of octasilyl-derivatized silica (C8) and transferred into an SPE cartridge containing ENVI-Carb II/PSA (0.5/0.5 g) as a clean up co-sorbent. Then the dispersed sample was washed with 10 mL of n-hexane and triazines were eluted with 20 mL ethyl acetate and 5 mL acetonitrile. Finally the extract was concentrated to dryness, re-constituted with 1 mL methanol:water (1:1) and injected into the HPLC-DAD system. The linearity of the calibration curves was excellent in matrix matched standards, and yielded the coefficients of determination>0.995 for all the target analytes. The recoveries ranged from 75% to 100% with relative standard deviations lower than 7%. The achieved LOQs (<10 µg kg(-1)) for all triazines under study permits to ensure proper determination at the maximum allowed residue levels set in the European Union Legislation. Samples of three seaweeds were subjected to the procedure proving the suitability of MSPD method for the analysis of triazines in different seaweeds samples.

  18. Sample clean-up by sol-gel immunoaffinity chromatography for the determination of bisphenol A in food and urine.

    PubMed

    Cichna-Markl, Margit

    2012-02-01

    Bisphenol A (2,2-bis(4-hydroxyphenyl)propane, BPA) is an industrial chemical mainly used as a monomer in the synthesis of polycarbonates and epoxy resins. BPA has been shown to elicit estrogenic effects via binding to the nuclear estrogen receptors α and β. Food is considered as the major source of BPA exposure for the general human population. When incorporated into the body, BPA is metabolised in the liver, mainly to BPA glucuronide, and excreted via the urine. The present paper presents analytical methods for the determination of BPA concentrations in foodstuffs and the determination of free and total (free plus conjugated) BPA in urine samples. The paper provides protocols for the preparation and operation of sol-gel immunoaffinity columns and their application to remove interfering matrix compounds and to enrich BPA. In addition, the paper points out major sources of systematic errors in BPA analysis and describes how they can be avoided.

  19. Multicriteria optimisation of a simultaneous supercritical fluid extraction and clean-up procedure for the determination of persistent organohalogenated pollutants in aquaculture samples.

    PubMed

    Rodil, R; Carro, A M; Lorenzo, R A; Cela, R

    2007-04-01

    A useful tool based on a single-step extraction and clean-up procedure for the determination of 15 organohalogenated pollutants (including brominated flame retardants) in aquaculture samples, using aluminium oxide basic and acidic silica gel in the supercritical extraction cell followed by gas chromatography with electron capture detection or mass spectrometry has been developed. This effective clean-up step ensures a minimum of chromatographic difficulties related to complex matrix components such as aquaculture feed. The extraction procedure has been screened by a fractional factorial design for the preliminary statistically significant parameters. The factors selected were extraction temperature, pressure, static extraction time, dynamic extraction time and carbon dioxide flow rate. The Doehlert design, followed by a multicriteria decision-making strategy, was then performed in order to determine the optimum conditions for the two most significant factors: pressure (165 bar) and dynamic extraction time (27 min). Under optimal conditions, the procedure developed with GC-MS/MS provides an excellent linearity, detection (0.01-0.2 ng g(-1)) and quantification limits (0.05-0.8 ng g(-1)) for most of the analytes investigated. The feasibility of the proposed supercritical fluid extraction method was validated by analysing two reference materials and fish feed and shellfish samples with satisfactory results.

  20. Semi-covalent imprinted polymer using propazine methacrylate as template molecule for the clean-up of triazines in soil and vegetable samples.

    PubMed

    Cacho, C; Turiel, E; Martín-Esteban, A; Ayala, D; Pérez-Conde, C

    2006-05-12

    A semi-covalent imprinted polymer was prepared by precipitation polymerisation using propazine methacrylate as template molecule, ethylene glycol dimethacrylate as cross-linker and toluene as porogen. After removal of propazine by basic hydrolysis of the covalent bond, the optimum loading, washing and elution conditions for the solid-phase extraction of the selected triazines were established. The binding sites present in the polymeric matrix were characterised by fitting the experimental results of several rebinding studies to the Langmuir-Freundlich isotherm. Subsequently, an analytical methodology based on molecularly imprinted solid-phase extraction (MISPE) was developed for the determination of several triazinic herbicides in soil and vegetable samples. Following this procedure, a good degree of clean-up of the sample extracts was easily achieved, allowing the HPLC-UV determination of selected triazines in complex samples at low concentration levels.

  1. One-step selective electrokinetic removal of inorganic anions from small volumes and its application as sample clean-up for mass spectrometric techniques.

    PubMed

    Tubaon, Ria Marni; Haddad, Paul R; Quirino, Joselito P

    2017-03-10

    The presence of inorganic anions in a sample interferes with mass spectrometric (MS) analysis. Here, a simple method to remove these ions from a liquid sample in one-step is described. The inorganic anions present in a 50μL sample were extracted into a low pH solution inside a 200μm i.d.×33cm long capillary by the use of an electric field. The selective removal of unwanted anions and retention of target analytes was accomplished by control of the apparent electrophoretic velocities of anions and analytes at a boundary that separated the sample and extraction solution. No physical barrier (e.g., membrane) was required and with the boundary situated at the tip of the capillary, efficient removal of inorganic anions (e.g., >80% removal) and good recovery of target analytes (e.g., >80% recovery) were achieved. The time required for removal of the inorganic anions was found to depend on their initial concentrations. The removal process was investigated using different concentrations of bromide and nitrate (as potassium salts) and negatively chargeable drugs as target analytes. This micro-sample clean-up technique used no organic solvents and little consumables and was studied to the determination of 0.6μg/L arsenic and 8.3μg/L vanadium in 500mg/L sodium chloride using inductively coupled plasma MS and 50μM angiotensin I in 1000mg/L sodium chloride using electrospray ionisation MS. Micro-sample clean-up was performed for 45min at 3kV in both demonstrations. The calculated recoveries for the metals at trace levels were 110-130%, and for the peptide was 103.8%.

  2. Novel technique for the combined recovery, extraction and clean-up of forensic organic and inorganic trace explosives samples.

    PubMed

    Warren, D; Hiley, R W; Phillips, S A; Ritchie, K

    1999-01-01

    This paper describes a simple processing and analysis scheme for explosives trace swab samples which deals both with organic and inorganic materials. Swabs, wetted with ethanol or ethanol/water mixture, were extracted with ethanol/water mixture. The extract was passed directly through a simple column containing an acrylonitrile/styrene copolymer adsorbent. The adsorbent retained common organic explosives, which were recovered with an efficiency of 30-50% as a relatively clean ethyl acetate solution. The concentrated ethyl acetate eluate was analysed using gas chromatography with chemiluminescence or mass spectrometric detection. The unretained inorganic ions and sugars, which were recovered with generally high efficiency as an ethanol/water solution, could be directly analysed using ion chromatography and/or capillary electrophoresis. Minor difficulties encountered in the analysis of sugars, fluoride and phosphate were examined.

  3. Simultaneous analysis of organochlorinated pesticides (OCPs) and polychlorinated biphenyls (PCBs) from marine samples using automated pressurized liquid extraction (PLE) and Power Prep™ clean-up.

    PubMed

    Helaleh, Murad I H; Al-Rashdan, Amal; Ibtisam, A

    2012-05-30

    An automated pressurized liquid extraction (PLE) method followed by Power Prep™ clean-up was developed for organochlorinated pesticide (OCP) and polychlorinated biphenyl (PCB) analysis in environmental marine samples of fish, squid, bivalves, shells, octopus and shrimp. OCPs and PCBs were simultaneously determined in a single chromatographic run using gas chromatography-mass spectrometry-negative chemical ionization (GC-MS-NCI). About 5 g of each biological marine sample was mixed with anhydrous sodium sulphate and placed in the extraction cell of the PLE system. PLE is controlled by means of a PC using DMS 6000 software. Purification of the extract was accomplished using automated Power Prep™ clean-up with a pre-packed disposable silica column (6 g) supplied by Fluid Management Systems (FMS). All OCPs and PCBs were eluted from the silica column using two types of solvent: 80 mL of hexane and a 50 mL mixture of hexane and dichloromethane (1:1). A wide variety of fish and shellfish were collected from the fish market and analyzed using this method. The total PCB concentrations were 2.53, 0.25, 0.24, 0.24, 0.17 and 1.38 ng g(-1) (w/w) for fish, squid, bivalves, shells, octopus and shrimp, respectively, and the corresponding total OCP concentrations were 30.47, 2.86, 0.92, 10.72, 5.13 and 18.39 ng g(-1) (w/w). Lipids were removed using an SX-3 Bio-Beads gel permeation chromatography (GPC) column. Analytical criteria such as recovery, reproducibility and repeatability were evaluated through a range of biological matrices.

  4. Trivalent copper chelate-luminol chemiluminescence system for highly sensitive CE detection of dopamine in biological sample after clean-up using SPE.

    PubMed

    Wang, Lin; Liu, Ying; Xie, Haoyue; Fu, Zhifeng

    2012-06-01

    A transition metal chelate unstable at a high oxidation state, diperiodatocuprate (III) (K₅[Cu(HIO₆)₂], DPC), was synthesized and applied in the luminol-based chemiluminescence (CL) system for highly sensitive CE end-column detection of dopamine (DA). This method was based on the fact that DA enhanced the CL emission resulting from the reaction between luminol and DPC in alkaline medium. The DPC-luminol-DA CL system showed very intensive emission and very fast kinetic characteristics, thus resulting in a high sensitivity in flow-through detection mode for CE. Under optimal conditions, the linear range was 1.0 × 10⁻⁸-5.0 × 10⁻⁵ g/mL (R² = 0.9984) with a limit of detection of 6.0 × 10⁻⁹ g/mL (S/N = 3). The RSDs of the peak height and the migration time were about 4.2 and 2.4% for a standard sample at 3.0 × 10⁻⁶ g/mL (n = 5), respectively. The presented method has been successfully used for the determination of DA in commercial preparation and human urine samples after clean-up using SPE.

  5. HPLC-based method using sample pre-column clean-up for the determination of methanethiol and ethanethiol in parenteral amino acid solutions.

    PubMed

    do Nascimento, P C; Bohrer, D; Rohlfes, A L; de Carvalho, L M; Ramirez, A

    2001-05-01

    A method has been developed for the chromatographic determination of methanethiol (MT) and ethanethiol (ET) as contaminants in amino acid parenteral nutrition (PN) solutions. The clean-up of the samples before chromatographic analysis was investigated by solid-phase extraction (SPE) on pre-columns filled with polyethylene powder (PE), aluminium oxide (AlOx), silica (SiOx), or polyurethane foam (PUF) as adsorbents. The thiols were more efficiently separated from the matrices by SPE on PUF pre-columns. Simultaneous derivatization and elution with DTNB (5,5'-dithiobis(2-nitrobenzoic acid)) enabled further discrimination between MT and ET by reversed-phase HPLC with spectrophotometric detection. The retention times for the derivatized MT and ET species were 12.5 and 23.0 min, respectively. Recoveries from spiked PN samples were calculated to be approximately 90%, and the MT and ET content of commercial PN solutions was determined using the methodology described. Detection limits of 15 and 10 microg L(-1) were calculated for MT and ET, respectively.

  6. Selective extraction of antimycotic drugs from sludge samples using matrix solid-phase dispersion followed by on-line clean-up.

    PubMed

    Casado, Jorge; Castro, Gabriela; Rodríguez, Isaac; Ramil, María; Cela, Rafael

    2015-01-01

    An effective and selective, modular sample preparation method for the extraction of eight antimycotic drugs, belonging to three different chemical classes, from digested sludge samples is proposed. To this end, matrix solid-phase dispersion (MSPD) was on-line connected with a cationic exchanger solid-phase extraction (SPE) cartridge. Analytes were extracted from the MSPD syringe, which contained the freeze-dried sludge sample dispersed with C18 plus a clean-up layer of primary and secondary amine (PSA) sorbent, with 10 mL of methanol. This extract flowed also through the SPE cartridge, where target compounds remained trapped while neutral interferences are released. After discarding the MSPD syringe, analytes were recovered with 10 mL of methanol (0.5% in NH3) before LC-MS/MS determination using a hybrid quadrupole time-of-flight (QTOF) mass spectrometer furnished with an electrospray ionization (ESI) source. In comparison with previously published sample preparation methodologies, the developed approach greatly simplifies sample handling and reduces attenuation of ESI ionization for sample extracts when compared to standard solutions. The obtained absolute recoveries ranged between 70 and 118%, and the limits of quantification (LOQs) of the method varied between 5 and 8 ng g(-1). Four antimycotic drugs were ubiquitous in urban sludge samples, with maximum average concentrations (above 400 ng g(-1)) corresponding to clotrimazole (CTZ). The screening capabilities of the LC-QTOF-MS system demonstrated that the developed modular extraction and purification methodology might be useful for the selective extraction of other basic drugs (e.g., sertraline, amitryptiline, and amiodarone) from sludge.

  7. TRACKING CLEAN UP AT HANFORD

    SciTech Connect

    CONNELL, C.W.

    2005-05-27

    The Hanford Federal Facility Agreement and Consent Order, known as the ''Tri-Party Agreement'' (TPA), is a legally binding agreement among the US Department of Energy (DOE), The Washington State Department of Ecology, and the US Environmental Protection Agency (EPA) for cleaning up the Hanford Site. Established in the 1940s to produce material for nuclear weapons as part of the Manhattan Project, Hanford is often referred to as the world's large environmental cleanup project. The Site covers more than 580 square miles in a relatively remote region of southeastern Washington state in the US. The production of nuclear materials at Hanford has left a legacy of tremendous proportions in terms of hazardous and radioactive waste. From a waste-management point of view, the task is enormous: 1700 waste sites; 450 billion gallons of liquid waste; 70 billion gallons of contaminated groundwater; 53 million gallons of tank waste; 9 reactors; 5 million cubic yards of contaminated soil; 22 thousand drums of mixed waste; 2.3 tons of spent nuclear fuel; and 17.8 metric tons of plutonium-bearing material and this is just a partial listing. The agreement requires that DOE provide the results of analytical laboratory and non-laboratory tests/readings to the lead regulatory agency to help guide then in making decisions. The agreement also calls for each signatory to preserve--for at least ten years after the Agreement has ended--all of the records in it, or its contractors, possession related to sampling, analysis, investigations, and monitoring conducted. The Action Plan that supports the TPA requires that Ecology and EPA have access to all data that is relevant to work performed, or to be performed, under the Agreement. Further, the Action Plan specifies two additional requirements: (1) that EPA, Ecology and their respective contractor staffs have access to all the information electronically, and (2) that the databases are accessible to, and used by, all personnel doing TPA

  8. New method for the determination of parabens and bisphenol A in human milk samples using ultrasound-assisted extraction and clean-up with dispersive sorbents prior to UHPLC-MS/MS analysis.

    PubMed

    Rodríguez-Gómez, R; Dorival-García, N; Zafra-Gómez, A; Camino-Sánchez, F J; Ballesteros, O; Navalón, A

    2015-06-15

    A sensitive and accurate analytical method for the determination of methyl-, ethyl-, propyl- and butylparaben and bisphenol A in human milk samples has been developed and validated. The combination of ultrasound-assisted extraction (UAE) and a simplified and rapid clean-up technique that uses sorbent materials has been successfully applied for the preparation of samples prior to ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis. The analytes were extracted from freeze-dried human milk samples using acetonitrile and ultrasonic radiation (three 15-min cycles at 70% amplitude), and further cleaned-up with C18 sorbents. The most influential parameters affecting the UAE method and the clean-up steps were optimized using design of experiments. Negative electrospray ionization (ESI) in the selected reaction monitoring (SRM) mode was used for MS detection. The use of two reactions for each compound allowed simultaneous quantification and identification in one run. The analytes were separated in less than 10min. Deuterium-labeled ethylparaben-d5 (EPB-d5) and deuterium-labeled bisphenol A-d16 (BPA-d16) were used as surrogates. The limits of quantification ranged from 0.4 to 0.7ngmL(-1), while inter- and intra-day variability was under 11.1% in all cases. In the absence of certified reference materials, recovery assays with spiked samples using matrix-matched calibration were used to validate the method. Recovery rates ranged from 93.8% to 112.2%. The proposed method was satisfactorily applied for the determination of four selected parabens and bisphenol A in human milk samples obtained from nursing mothers living in the province of Granada (Spain).

  9. Cleaning Up Our Drinking Water

    SciTech Connect

    Manke, Kristin L.

    2007-08-01

    Imagine drinking water that you wring out of the sponge you’ve just used to wash your car. This is what is happening around the world. Rain and snow pass through soil polluted with pesticides, poisonous metals and radionuclides into the underground lakes and streams that supply our drinking water. “We need to understand this natural system better to protect our groundwater and, by extension, our drinking water,” said Pacific Northwest National Laboratory’s Applied Geology and Geochemistry Group Manager, Wayne Martin. Biologists, statisticians, hydrologists, geochemists, geologists and computer scientists at PNNL work together to clean up contaminated soils and groundwater. The teams begin by looking at the complexities of the whole environment, not just the soil or just the groundwater. PNNL researchers also perform work for private industries under a unique use agreement between the Department of Energy and Battelle, which operates the laboratory for DOE. This research leads to new remediation methods and technologies to tackle problems ranging from arsenic at old fertilizer plants to uranium at former nuclear sites. Our results help regulators, policy makers and the public make critical decisions on complex environmental issues.

  10. Exhaust gas clean up process

    DOEpatents

    Walker, R.J.

    1988-06-16

    A method of cleaning an exhaust gas containing particulates, SO/sub 2/ and NO/sub x/ is described. The method involves prescrubbing with water to remove HCl and most of the particulates, scrubbing with an aqueous absorbent containing a metal chelate and dissolved sulfite salt to remove NO/sub x/ and SO/sub 2/, and regenerating the absorbent solution by controlled heating, electrodialysis and carbonate salt addition. The NO/sub x/ is removed as N/sub 2/ gas or nitrogen sulfonate ions and the oxides of sulfur are removed as a valuable sulfate salt. 4 figs.

  11. Exhaust gas clean up process

    DOEpatents

    Walker, Richard J.

    1989-01-01

    A method of cleaning an exhaust gas containing particulates, SO.sub.2 and NO.sub.x includes prescrubbing with water to remove HCl and most of the particulates, scrubbing with an aqueous absorbent containing a metal chelate and dissolved sulfite salt to remove NO.sub.x and SO.sub.2, and regenerating the absorbent solution by controlled heating, electrodialysis and carbonate salt addition. The NO.sub.x is removed as N.sub.2 or nitrogen-sulfonate ions and the oxides of sulfur are removed as a vaulable sulfate salt.

  12. Validated quantitation of angiotensin II receptor antagonists (ARA-II) in human plasma by liquid-chromatography-tandem mass spectrometry using minimum sample clean-up and investigation of ion suppression.

    PubMed

    Ferreirós, Nerea; Dresen, Sebastian; Alonso, Rosa María; Weinmann, Wolfgang

    2007-12-01

    For the quantitation of angiotensin II receptor antagonists (ARA-II) in human plasma, a method using liquid-chromatography (LC)-electrospray ionization tandem mass spectrometry (MS/MS) has been developed with respect to simple sample clean-up and investigation of ion suppression effects. For sample preparation, protein precipitation using zinc sulphate and methanol showed advantages in speed, recovery, and reproducibility over solid-phase extraction. A triple quadrupole mass spectrometer (Sciex API 365) with turbo ionspray source was used for detection of compounds with multireaction monitoring (MRM) of two transitions per compound. Suppression effects caused by endogenous matrix compounds were investigated by post-column infusion of analytes and LC analysis of precipitates of blank plasma samples and could be excluded. A validation was performed for the ARA-II drugs (valsartan, irbesartan, losartan and its active metabolite EXP 3174, eprosartan, candesartan, and telmisartan). The developed method showed good intra- and interday precision (<12% relative standard deviation) and accuracy (<11.5% bias) at different concentrations for all the studied compounds. The calculated lower limits of quantitation were between 7 and 13 ng/mL, and the compounds were stable during the analytical process. These rather expensive drugs against hypertension are prescribed with increasing numbers in Europe and the industrialized nations. Complications might arise from overdosage or metabolic disorders. However, drug monitoring is not usually performed. Because the therapeutic concentrations range from a few nanograms to hundreds of nanograms per milliliter for the different drugs, and they are not amenable to gas chromatography/MS analysis because of their high molecular weight and polarity, the LC-MS/MS method is the golden standard for therapeutic drug monitoring and for clinical and forensic toxicology of ARA-II drugs.

  13. Myelodysplastic syndromes in Chernobyl clean-up workers.

    PubMed

    Gluzman, Daniil F; Sklyarenko, Lilia M; Koval, Stella V; Rodionova, Nataliia K; Zavelevich, Michael P; Ivanivskaya, Tetiana S; Poludnenko, Liudmyla Yu; Ukrainskaya, Nataliia I

    2015-10-01

    The studies of the recent decades posed the question of the association between radiation exposure and myelodysplastic syndromes (MDS). This association has been proved in secondary MDS originating upon exposure to chemotherapeutics and/or radiation therapy. The long-term study in Japanese atomic (A)-bomb survivors demonstrated the significant linear dose-response for MDS confirming the link between radiation exposure and this form of hematopoietic malignancies. All these findings provide the strong basis for studying MDS in the persons exposed to radiation following the Chernobyl disaster, especially those in the cohort of Chernobyl clean-up workers of 1986-1987. The data on MDS among Chernobyl clean-up workers (1986-1987) diagnosed in 1996-2012 at the reference laboratory of RE Kavetsky Institute of Experimental Pathology, Oncology and Radiobiology are summarized. MDS cases were diagnosed in 23 persons (21 males and 2 females) having been exposed to radiation as clean-up workers of 1986-1987. Refractory anemia (RA) has been detected in 13, refractory anemia with ring sideroblasts (RARS)-in 2, and refractory anemia with excess blasts (RAEB)-in 8 patients. The median age of those MDS patients was 62.0 years. In addition, 5 cases of chronic myelomonocytic leukemia (CMML) were recorded in the group of Chernobyl clean-up workers with the median time of 14.8 years from 1986-1987 to diagnosis. The association between radiation exposure and MDS is discussed. The suggested life-long risk for myelodysplastic syndromes among A-bomb survivors in Japan highlights the importance of the continuing follow-up studies in the affected populations in the post-Chernobyl period.

  14. Rodent Control: Seal Up! Trap Up! Clean Up!

    MedlinePlus

    ... rodent food sources and nesting sites... Diseases from rodents Diseases directly transmitted by rodents Diseases indirectly transmitted by rodents Cleaning up after rodents Take precautions before and during clean up of ...

  15. 40 CFR 263.31 - Discharge clean up.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 26 2014-07-01 2014-07-01 false Discharge clean up. 263.31 Section 263...) STANDARDS APPLICABLE TO TRANSPORTERS OF HAZARDOUS WASTE Hazardous Waste Discharges § 263.31 Discharge clean up. A transporter must clean up any hazardous waste discharge that occurs during transportation...

  16. 40 CFR 263.31 - Discharge clean up.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 26 2011-07-01 2011-07-01 false Discharge clean up. 263.31 Section 263...) STANDARDS APPLICABLE TO TRANSPORTERS OF HAZARDOUS WASTE Hazardous Waste Discharges § 263.31 Discharge clean up. A transporter must clean up any hazardous waste discharge that occurs during transportation...

  17. 40 CFR 263.31 - Discharge clean up.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 27 2013-07-01 2013-07-01 false Discharge clean up. 263.31 Section 263...) STANDARDS APPLICABLE TO TRANSPORTERS OF HAZARDOUS WASTE Hazardous Waste Discharges § 263.31 Discharge clean up. A transporter must clean up any hazardous waste discharge that occurs during transportation...

  18. 40 CFR 263.31 - Discharge clean up.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 27 2012-07-01 2012-07-01 false Discharge clean up. 263.31 Section 263...) STANDARDS APPLICABLE TO TRANSPORTERS OF HAZARDOUS WASTE Hazardous Waste Discharges § 263.31 Discharge clean up. A transporter must clean up any hazardous waste discharge that occurs during transportation...

  19. Matrix solid phase dispersion-Soxhlet simultaneous extraction clean-up for determination of organochlorine pesticide residues in tobacco.

    PubMed

    Cai, Jibao; Gao, Yun; Zhu, Xiaolan; Su, Qingde

    2005-11-01

    A novel method combining matrix solid phase dispersion (MSPD) with Soxhlet simultaneous extraction clean-up (SSEC) was developed. Being a single-step extraction and clean-up procedure, it could be used instead of multistep solvent extraction and Florisol column clean-up. It not only reduces sample contamination during the procedure, but it also decreases the amount of organic solvent needed. The retention times of standards were used to qualitatively assess the method, and the external standard method was used to quantitatively assess it. Residues of organochlorine pesticides (OCP) in tobaccos were determined by gas chromatography-electron capture detection (GC-ECD), and their identities were confirmed by the standard addition method (SAM). The performance of the method was evaluated and validated: the detection limit was 0.01-0.02 microg g(-1), relative standard deviations were 5-26%, and recoveries were 72-99% at fortification levels of 0.10, 1.00 and 10.0 microg g(-1). The analytical characteristics of MSPD-SSEC compared very favorably with the results from the classical multistep solvent extraction and Florisol column clean-up method.

  20. Helping nature clean up oil spills

    SciTech Connect

    Paddock, A.

    1996-11-01

    Oil spills are nothing new. In fact, for millions of years crude oil has been seeping up to the Earth`s surface, and for all that time Mother Nature has been on the job with microbes, or bacteria, to harmlessly convert the oil to water and carbon dioxide gas. Not all bacteria are bad. True, some can make us sick, however, the good ones help us bake bread, brew beer, and even clean up oil spills by a process known as biodegradation. Oil and bacteria don`t easily get together because oil and water don`t mix and bacteria prefer to stay in water. After some oil tankers spills in the English Channel 25 years ago, major oil companies (Arco, BP, Exxon, and others) developed oil dispersant products-specialized chemicals that make oils and sea water mix. The simplest examples of similar wetting agents are soaps and detergents. Now, thanks to dispersants, the natural bacteria at sea can easily get to the oil and the normally slow biodegradation process goes rather quickly.

  1. Cockroaches probably cleaned up after dinosaurs.

    PubMed

    Vršanský, Peter; van de Kamp, Thomas; Azar, Dany; Prokin, Alexander; Vidlička, L'ubomír; Vagovič, Patrik

    2013-01-01

    Dinosaurs undoubtedly produced huge quantities of excrements. But who cleaned up after them? Dung beetles and flies with rapid development were rare during most of the Mesozoic. Candidates for these duties are extinct cockroaches (Blattulidae), whose temporal range is associated with herbivorous dinosaurs. An opportunity to test this hypothesis arises from coprolites to some extent extruded from an immature cockroach preserved in the amber of Lebanon, studied using synchrotron X-ray microtomography. 1.06% of their volume is filled by particles of wood with smooth edges, in which size distribution directly supports their external pre-digestion. Because fungal pre-processing can be excluded based on the presence of large particles (combined with small total amount of wood) and absence of damages on wood, the likely source of wood are herbivore feces. Smaller particles were broken down biochemically in the cockroach hind gut, which indicates that the recent lignin-decomposing termite and cockroach endosymbionts might have been transferred to the cockroach gut upon feeding on dinosaur feces.

  2. Site clean up of coal gasification residues

    SciTech Connect

    Wilson, J.W.; Ding, Y.

    1995-12-31

    The coal gasification plant residues tested in this research consists of various particle sizes of rock, gravel, tar-sand agglomerates, fine sand and soil. Most of the soils particles were tar free. One of the fractions examined contained over 3000 ppM polyaromatic hydrocarbons (PAHs). The residues were subjected to high pressure water jet washing, float and sink tests, and soil washing. Subsequent PAH analyses found less than 1 ppM PAHs in the water jet washing water. Soils washed with pure water lowered PAH concentrations to 276 ppM; the use of surfactants decreased PAHs to 47, 200, and 240 ppM for different test conditions. In the 47 ppM test, the surfactant temperature had been increased to 80 C, suggesting that surfactant washing efficiency can be greatly improved by increasing the solution temperature. The coal tar particles were not extracted by the surfactants used. Coke and tar-sand agglomerates collected from the float and sink gravimetric separation were tested for heating value. The tar exhibited a very high heating value, while the coke had a heating value close to that of bituminous coal. These processes are believed to have the potential to clean up coal gasification plant residues at a fairly low cost, pending pilot-scale testing and a feasibility study.

  3. Cockroaches Probably Cleaned Up after Dinosaurs

    PubMed Central

    Vršanský, Peter; van de Kamp, Thomas; Azar, Dany; Prokin, Alexander; Vidlička, L'ubomír; Vagovič, Patrik

    2013-01-01

    Dinosaurs undoubtedly produced huge quantities of excrements. But who cleaned up after them? Dung beetles and flies with rapid development were rare during most of the Mesozoic. Candidates for these duties are extinct cockroaches (Blattulidae), whose temporal range is associated with herbivorous dinosaurs. An opportunity to test this hypothesis arises from coprolites to some extent extruded from an immature cockroach preserved in the amber of Lebanon, studied using synchrotron X-ray microtomography. 1.06% of their volume is filled by particles of wood with smooth edges, in which size distribution directly supports their external pre-digestion. Because fungal pre-processing can be excluded based on the presence of large particles (combined with small total amount of wood) and absence of damages on wood, the likely source of wood are herbivore feces. Smaller particles were broken down biochemically in the cockroach hind gut, which indicates that the recent lignin-decomposing termite and cockroach endosymbionts might have been transferred to the cockroach gut upon feeding on dinosaur feces. PMID:24324610

  4. ROSEE cleans up after the Cold War

    SciTech Connect

    Valenti, M.

    1994-07-01

    This article describes a robot named ROSEE, designed by engineers at the DOE's Hanford site to minimize the risk of radiation exposure to workers cleaning up to residue left by America's manufacture of nuclear weapons. ROSEE is the acronym for Remotely Operated Sediment Extraction Equipment, a robot designed to vacuum sediment and debris from a nuclear fuels storage pool at the Department of Energy's Hanford nuclear waste storage site in Richland, Wash. The task facing ROSEE involves cleaning out the N basin at Hanford. Work is schedules to begin before the fall. The basin houses nuclear fuel refined during 24 years of the Cold War era. This water-filled structure is 24 feet deep, 87 feet long, and 56 feet wide, approximately three times larger than an Olympic-size swimming pool. Nuclear fuel was contained in honeycomb cells mounted 1 inch from the bottom of the pool. The cells rise 10 feet from the bottom of the basin, and each cell is 21 inches deep and 14 inches wide. The cells now hold radioactive residues that must be removed for final safe disposal.

  5. Tidd hot gas clean up program. Final report

    SciTech Connect

    1995-10-01

    This Final Report on the Tidd Hot Gas Clean Up Program covers the period from initial Proof-of-Concept testing in August, 1990, through final equipment inspections in May, 1995. The Tidd Hot Gas Clean Up (HGCU) system was installed in the Tidd Pressurized Fluidized Bed Combustion (PFBC) Demonstration Plant, which is the first utility-scale PFBC plant in the United States. Detailed design work on the project began in July, 1990, and site construction began in December, 1991. Initial operation of the system occurred in May, 1992, and the hot gas filter was commissioned in October, 1992. The test program ended in March, 1995, when the Tidd Plant was shut down following its four-year test program. Section 1.0 of this report is an executive summary of the project covering the project background, system description, test results and conclusions. Section 2.0 is an introduction covering the program objectives and schedule. Section 3.0 provides detailed descriptions of the system and its major components. Section 4.0 provides detailed results of all testing including observations and posttest inspection results. Sections 5.0 and 6.0 list the program conclusions and recommendations, respectively. Appendix I is a report prepared by Southern Research Institute on the properties of Tidd PFBC ash sampled during the test program. Appendix II is a report prepared by Westinghouse STC on the performance of candle filter fail-safe regenerator devices.

  6. CE IGCC repowering project hot gas clean up system

    SciTech Connect

    Not Available

    1993-09-01

    With sponsorship from the Department of Energy (DOE), and the state of Illinois, Combustion Engineering, Inc. is currently developing a design for a 60 Mw IGCC (Integrated Coal Gasification Combined Cycle) for City Water, Light & Power (CWL&P) in Springfield, Illinois. In addition, to DOE and the state of Illinois, Combustion Engineering, Inc. and CWL&P are contributing to the project. In order to obtain a high thermal efficiency, a hot gas cleanup system has been incorporated for product gas clean up. The cleanup system currently incorporated in the system design is one that is being developed by General Electric Environmental Services, Inc. (GEESI). This is a moving bed process which includes the regeneration of the sorbent material. Testing of the system is currently underway in GEESI`s pilot plant in Schenectady, New York. The hot gas clean up system will use a moving-bed of zinc titanate as an absorbent material to capture gaseous sulfur species in the gas. The cleanup system will be required to operate in a range of 850--1150{degree}F (454--621{degree}C) and under a pressure of 20 atmospheres. Results of the tests indicate that overall sulfur efficiency exceeds 95%, the zinc titanate can be regenerated, and produces an SO{sub 2}-rich tail gas suitable for conversion to sulfuric acid, elemental sulfur or disposable waste.

  7. 40 CFR 263.31 - Discharge clean up.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ....31 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES (CONTINUED) STANDARDS APPLICABLE TO TRANSPORTERS OF HAZARDOUS WASTE Hazardous Waste Discharges § 263.31 Discharge clean up. A transporter must clean up any hazardous waste discharge that occurs during transportation...

  8. 36. HISTORIC PHOTOGRAPH SHOWING BILL KEYS CLEANING UP AFTER THE ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    36. HISTORIC PHOTOGRAPH SHOWING BILL KEYS CLEANING UP AFTER THE MILL RUN (NOTE SCREEN FROM MORTAR SETTING ON TABLE, STAMPS ARE HUNG UP). - Wall Street Gold Mill, Twentynine Palms, San Bernardino County, CA

  9. Organophosphorous Pesticide Detection in Olive Oil by Using a Miniaturized, Easy-to-Use, and Cost-Effective Biosensor Combined with QuEChERS for Sample Clean-Up

    PubMed Central

    Arduini, Fabiana; Forchielli, Matteo; Scognamiglio, Viviana; Nikolaevna, Kozitsina Alisa; Moscone, Danila

    2016-01-01

    Herein, we report a portable electrochemical biosensor based on butyrylcholinesterase (BChE) immobilized on carbon black (CB)-modified screen-printed electrodes (SPEs) for the detection of organophosphorous pesticides in olive oil. The BChE/CB-SPE biosensor was developed to detect paraoxon in standard solutions as well as in olive oil samples previously treated with the QuEChERS method to extract pesticides from the whole fatty matrix. The biosensor shows a linear concentration range of between 20 and 100 ppb for paraoxon both in standard solutions (phosphate buffer 0.05 M) and in olive oil extracts, with a detection limit of 6 ppb in olive oil extract, corresponding to 10% of inhibition. The accuracy of this biosensor in olive oil samples was assessed with olive oil spiked with paraoxon, obtaining satisfactory recovery values. PMID:28029127

  10. Determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline by inductively coupled plasma mass spectrometry after sample clean up with hollow fiber solid phase microextraction system

    NASA Astrophysics Data System (ADS)

    Nomngongo, Philiswa N.; Ngila, J. Catherine

    2014-08-01

    This study reports a simple and efficient method for the determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline samples by inductively coupled plasma mass spectrometry after matrix removal and analyte pre-concentration using hollow fiber-solid phase microextraction (HF-SPME). The optimization of HF-SPME procedure was carried out using two-level full factorial and central composite designs. Four factors (variables), that are, sample solution pH, acceptor phase amount, extraction time and eluent concentration were optimized. Under the optimized experimental conditions, the precision was ≤ 3% (C = 10 μg L- 1, n = 15), limits of detection and quantification ranged from 0.1 to 0.3 μg L- 1 and 0.3-0.9 μg L- 1, respectively, and the maximum preconcentration factor was 30. The HF-SPME method was applied for the determination of trace metals in real gasoline and diesel samples.

  11. PRP: The Proven Solution for Cleaning Up Oil Spills

    NASA Technical Reports Server (NTRS)

    2006-01-01

    The basic technology behind PRP is thousands of microcapsules, tiny balls of beeswax with hollow centers. Water cannot penetrate the microcapsule s cell, but oil is absorbed right into the beeswax spheres as they float on the water s surface. This way, the contaminants, chemical compounds that originally come from crude oil such as fuels, motor oils, or petroleum hydrocarbons, are caught before they settle. PRP works well as a loose powder for cleaning up contaminants in lakes and other ecologically fragile areas. The powder can be spread over a contaminated body of water or soil, and it will absorb contaminants, contain them in isolation, and dispose of them safely. In water, it is important that PRP floats and keeps the oil on the surface, because, even if oil exposure is not immediately lethal, it can cause long-term harm if allowed to settle. Bottom-dwelling fish exposed to compounds released after oil spills may develop liver disease, in addition to reproductive and growth problems. This use of PRP is especially effective for environmental cleanup in sensitive areas like coral reefs and mangroves.

  12. Capillary-Channeled Polymer (C-CP) Fibers as a Stationary Phase for Sample Clean-Up of Protein Solutions for Matrix-Assisted Laser/Desorption Ionization Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Manard, Benjamin T.; Marcus, R. Kenneth

    2012-08-01

    Capillary-channeled polymer (C-CP) fibers are employed in a micropipette tip format to affect a stationary phase for the solid phase extraction (SPE) of proteins from buffer solutions prior to MALDI-MS analysis. Proteins readily adsorb to the polypropylene (PP) C-CP fibers while buffer species are easily washed off the tips using DI-H2O. Elution of the solutes is achieved with an aliquot of 50:50 ACN:H2O, which is compatible with the subsequent spotting on the MALDI target with the matrix solution. Lysozyme and cytochrome c are used as test species, with a primary buffer composition of 100 mM Tris-HCl. In this case, direct MALDI-MS produces no discernible protein signals. SPE on the C-CP fibers yields high fidelity mass spectra for 1 μL sample volumes. Limits of detection for cytochrome c in 100 mM Tris-HCl are on the order of 40 nM. Extraction of cytochrome c from buffer concentrations of up to 1 M Tris-HCl, provides signal recoveries that are suppressed by only ~50 % versus neat protein solutions. Finally, extraction of 3.1 μM cytochrome c from a synthetic urine matrix exhibits excellent recovery.

  13. Hebei Spirit Oil Spill Exposure and Subjective Symptoms in Residents Participating in Clean-Up Activities

    PubMed Central

    Cheong, Hae-Kwan; Lee, Jong Seong; Kwon, Hojang; Ha, Eun-Hee; Hong, Yun-Chul; Choi, Yeyong; Jeong, Woo-Chul; Hur, Jongil; Lee, Seung-Min; Kim, Eun-Jung; Im, Hosub

    2011-01-01

    Objectives This study was conducted to examine the relationship between crude oil exposure and physical symptoms among residents participating in clean-up work associated with the Hebei Spirit oil spill, 2007 in Korea. Methods A total of 288 residents responded to a questionnaire regarding subjective physical symptoms, sociodemographic characteristics and clean-up activities that occurred between two and eight weeks after the accident. Additionally, the urine of 154 of the respondents was analyzed for metabolites of volatile organic compounds (VOCs) and polycyclic aromatic hydrocarbons (PAHs) and heavy metals. To compare the urinary levels of exposure biomarkers, the urine of 39 inland residents who were not directly exposed to the oil spill were analyzed. Results Residents exposed to oil remnants through clean-up work showed associations between physical symptoms and the exposure levels defined in various ways, including days of work, degree of skin contamination, and levels of some urinary exposure biomarkers of VOCs, metabolites and metals, although no major abnormalities in urinary exposure biomarkers were observed. Conclusions This study provides evidence of a relationship between crude oil exposure and acute human health effects and suggests the need for follow-up to evaluate the exposure status and long-term health effects of clean-up participants. PMID:22125768

  14. Mt. Dioxin: "Clean Up" Action Threatens Florida Community.

    ERIC Educational Resources Information Center

    Gibbs, Lois

    1995-01-01

    Addresses citizen action taken by African American communities in Pensacola, Florida located in close proximity to a Superfund site. Discusses how the community is organizing to stop site clean-up efforts that residents claim have unjustly increased their already high exposure to toxins such as dioxin. (LZ)

  15. Marine Debris Clean-Ups as Meaningful Science Learning

    ERIC Educational Resources Information Center

    Stepath, Carl M.; Bacon, Joseph Scott

    2010-01-01

    This seven to eight week hands-on Marine Debris Clean-up Project used a service project to provide an introduction of marine science ecology, watershed interrelationships, the scientific method, and environmental stewardship to 8th grade middle school students. It utilized inquiry based learning to introduce marine debris sources and impacts to…

  16. Coupling detergent lysis/clean-up methodology with intact protein fractionation for enhanced proteome characterization

    SciTech Connect

    Sharma, Ritin; Dill, Brian; Chourey, Karuna; Shah, Manesh B; Verberkmoes, Nathan C; Hettich, Robert {Bob} L

    2012-01-01

    The expanding use of surfactants for proteome sample preparations has prompted the need to systematically optimize the application and removal of these MS-deleterious agents prior to proteome measurements. Here we compare four different detergent clean-up methods (Trichloroacetic acid (TCA) precipitation, Chloroform/Methanol/Water (CMW) extraction, commercial detergent removal spin column method (DRS) and filter-aided sample preparation(FASP)) with respect to varying amounts of protein biomass in the samples, and provide efficiency benchmarks with respect to protein, peptide, and spectral identifications for each method. Our results show that for protein limited samples, FASP outperforms the other three clean-up methods, while at high protein amount all the methods are comparable. This information was used in a dual strategy of comparing molecular weight based fractionated and unfractionated lysates from three increasingly complex samples (Escherichia coli, a five microbial isolate mixture, and a natural microbial community groundwater sample), which were all lysed with SDS and cleaned up using FASP. The two approaches complemented each other by enhancing the number of protein identifications by 8%-25% across the three samples and provided broad pathway coverage.

  17. Evaluation of a soil contaminated site and clean-up criteria: A geostatistical approach

    SciTech Connect

    Leonte, D.; Schofield, N.

    1996-12-31

    A case study of soil contamination assessment and clean-up in a site proposed for residential development is presented in this paper. The contamination consists mainly of heavy metals of which lead is the most important contaminant. The site has been sampled on an approximately 25 x 25 square meter grid to between 1 and 3 meters depth to evaluate the extent of the contamination. Three hotspots were identified based on eyeballing the lead sample values and a crude contouring. A geostatistical approach is proposed to map the lead contamination and provide an alternate evaluation. The results suggest a significantly different evaluation of the area for clean-up based on the probability of the lead concentration exceeding allowable levels.

  18. The Total Costs of Cleaning Up Nonfederal Superfund Sites

    DTIC Science & Technology

    1994-01-01

    NONFEDERAL SUPERFUND SITES Accesion For NTIS CRA&I DTIC TAB El Uc;anroun~ced [j Justification ................................ The Congress of the United...Preface T he federal Superfund program to clean up the nation’s worst hazardous waste sites has been controversial since its creation in 1980. As...the Congress begins to consider reauthorizing Superfund , which is due to expire on September 30, 1994, it is giving increased scrutiny to several

  19. Clean-up of Nuclear Licensed Facility 57

    SciTech Connect

    Jeanjacques, Michel; Bremond, Marie Pierre; Marchand, Carole; Poyau, Cecile; Viallefont, Cecile; Gautier, Laurent; Masure, Frederic

    2007-07-01

    Available in abstract form only. Full text of publication follows: In the early sixties a radiochemistry laboratory dedicated to Research and Development was built at the French Atomic Energy Commission's centre at Fontenay aux Roses (CEA-FAR); it was named Building 18. More buildings were added during the decade: Building 54, storehouses and offices and Building 91, a hall and laboratories for chemical engineering research into natural and depleted uranium. These three buildings together constitute NLF57. Construction work took place between 1959 and 1962 and the buildings entered operation in 1961. The research and development programs performed in NLF57 involved spent fuel reprocessing studies, waste treatment processes and studies and production of transuranic elements with the related analytical methods development. The research and development program ended on 30 June 1995. The NLF57 clean-up program was launched to reduce the nuclear and conventional hazards and minimise HLW and MLW production during the dismantling work. The clean-up work was divided into categories by type to facilitate its organisation: treatment and removal of nuclear material, removal of radioactive sources, treatment and removal of organic and aqueous effluents, treatment and removal of solid waste, pumping out of the PETRUS tank, flushing and decontamination of the tanks and clean-up of buildings. (authors)

  20. Analysis of fusaric acid in maize using molecularly imprinted solid phase extraction (MISPE) clean-up and ion-pair LC with diode array UV detection

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Fusaric acid is a phytotoxin and mycotoxin occasionally found in maize contaminated with Fusarium fungi. A selective sample clean-up procedure was developed to detect fusaric acid in maize using molecularly imprinted solid phase extraction (MISPE) clean-up coupled with ion-pair liquid chromatography...

  1. Comparison of Clean-Up Methods for Ochratoxin A on Wine, Beer, Roasted Coffee and Chili Commercialized in Italy

    PubMed Central

    Prelle, Ambra; Spadaro, Davide; Denca, Aleksandra; Garibaldi, Angelo; Gullino, Maria Lodovica

    2013-01-01

    The most common technique used to detect ochratoxin A (OTA) in food matrices is based on extraction, clean-up, and chromatography detection. Different clean-up cartridges, such as immunoaffinity columns (IAC), molecular imprinting polymers (MIP), Mycosep™ 229, Mycospin™, and Oasis® HLB (Hydrophilic Lipophilic balance) as solid phase extraction were tested to optimize the purification for red wine, beer, roasted coffee and chili. Recovery, reproducibility, reproducibility, limit of detection (LOD) and limit of quantification (LOQ) were calculated for each clean-up method. IAC demonstrated to be suitable for OTA analysis in wine and beer with recovery rate >90%, as well as Mycosep™ for wine and chili. On the contrary, MIP columns were the most appropriate to clean up coffee. A total of 120 samples (30 wines, 30 beers, 30 roasted coffee, 30 chili) marketed in Italy were analyzed, by applying the developed clean-up methods. Twenty-seven out of 120 samples analyzed (22.7%: two wines, five beers, eight coffees, and 12 chili) resulted positive to OTA. A higher incidence of OTA was found in chili (40.0%) more than wine (6.6%), beers (16.6%) and coffee (26.6%). Moreover, OTA concentration in chili was the highest detected, reaching 47.8 µg/kg. Furthermore, three samples (2.5%), two wines and one chili, exceeded the European threshold. PMID:24152987

  2. Comparison of clean-up methods for ochratoxin A on wine, beer, roasted coffee and chili commercialized in Italy.

    PubMed

    Prelle, Ambra; Spadaro, Davide; Denca, Aleksandra; Garibaldi, Angelo; Gullino, Maria Lodovica

    2013-10-22

    The most common technique used to detect ochratoxin A (OTA) in food matrices is based on extraction, clean-up, and chromatography detection. Different clean-up cartridges, such as immunoaffinity columns (IAC), molecular imprinting polymers (MIP), Mycosep™ 229, Mycospin™, and Oasis® HLB (Hydrophilic Lipophilic balance) as solid phase extraction were tested to optimize the purification for red wine, beer, roasted coffee and chili. Recovery, reproducibility, reproducibility, limit of detection (LOD) and limit of quantification (LOQ) were calculated for each clean-up method. IAC demonstrated to be suitable for OTA analysis in wine and beer with recovery rate >90%, as well as Mycosep™ for wine and chili. On the contrary, MIP columns were the most appropriate to clean up coffee. A total of 120 samples (30 wines, 30 beers, 30 roasted coffee, 30 chili) marketed in Italy were analyzed, by applying the developed clean-up methods. Twenty-seven out of 120 samples analyzed (22.7%: two wines, five beers, eight coffees, and 12 chili) resulted positive to OTA. A higher incidence of OTA was found in chili (40.0%) more than wine (6.6%), beers (16.6%) and coffee (26.6%). Moreover, OTA concentration in chili was the highest detected, reaching 47.8 µg/kg. Furthermore, three samples (2.5%), two wines and one chili, exceeded the European threshold.

  3. An alternative clean-up column for the determination of polychlorinated biphenyls in solid matrices.

    PubMed

    Ndunda, Elizabeth N; Madadi, Vincent O; Mizaikoff, Boris

    2015-12-01

    The need for continuous monitoring of polychlorinated biphenyls (PCBs) has necessitated the development of analytical techniques that are sensitive and selective with minimal reagent requirement. In light of this, we developed a column for clean-up of soil and sediment extracts, which is less demanding in terms of the amount of solvent and sorbent. The dual-layer column consists of acidified silica gel and molecularly imprinted polymers (MIPs). MIPs were synthesized via aqueous suspension polymerization using PCB 15 as the dummy template, 4-vinylpyridine as the functional monomer and ethylene glycol dimethacrylate as the cross-linker and the obtained particles characterized via SEM, BET, and batch rebinding assays. Pre-concentration of the spiked real-world water sample using MISPE gave recoveries between 85.2 and 104.4% (RSD < 8.69). On the other hand, the specific dual-layer column designed for clean-up of extracts from complex matrices provided recoveries of 91.6-102.5% (RSD < 4%) for spiked soil, which was comparable to clean-up using acidified silica (70.4-90.5%; RSD < 3.72%) and sulfoxide modified silica (89.7-103.0%; RSD < 13.0%). However, the polymers were reusable maintaining recoveries of 79.8-111.8% after 30 cycles of regeneration and re-use, thereby availing a cost-effective clean-up procedure for continuous monitoring of PCBs. Method detection limits were 0.01-0.08 ng g(-1) and 0.002-0.01 ng mL(-1) for solid matrices and water, respectively.

  4. Determination of pesticide residues in fish tissues by modified QuEChERS method and dual-d-SPE clean-up coupled to gas chromatography-mass spectrometry.

    PubMed

    Molina-Ruiz, Juan Manuel; Cieslik, Ewa; Cieslik, Iwona; Walkowska, Izabela

    2015-01-01

    The aim of this research was to modify the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method for the determination of organochlorine and organophosphate pesticides in fatty animal matrices such as fish muscle tissues of carp and sturgeon collected from Carp Valley, Lesser Poland. Pesticides extraction effectiveness was evaluated at 0.030 mg kg(-1) spiking level and efficiency of the dispersive-solid-phase extraction (d-SPE) clean-up step was evaluated by comparison testing two different d-SPE clean-up stages, first the addition of the d-SPE sorbent combination (PSA + SAX + NH2), and secondly the addition of C18 after extracts enrichment with the d-SPE sorbent combination (PSA + SAX + NH2), introducing a novel concept of clean-up named dual-d-SPE clean-up. Analysis of pesticide residues was performed by Gas Chromatography Quadrupole Mass Spectrometry (GC/Q-MS) working in selected-ion monitoring (SIM) mode. Linear relation was observed from 0 to 200 ng mL(-1) and determination coefficient R(2) > 0.997 in all instances for all target analytes. Better recoveries and cleanliness of extracts in both samples, carp and sturgeon tissues, were obtained after C18 addition during the dual-d-SPE clean-up step. Recoveries were in the range 70-120%, with relative standard deviation lower than 10% at 0.030 mg kg(-1) spiking level for most pesticides. LODs ranged 0.001-0.003 mg kg(-1), while LOQs ranged 0.004-0.009 mg kg(-1). The proposed method was successfully applied analyzing pesticide residues in real carp and sturgeon muscle samples; detectable pesticide residues were observed, but in all of the cases contamination level was lower than the default maximum residue levels (MRLs) set by the European Union (EU), Regulation (EC) N 396/2005.

  5. Evaluation of alternative PCB clean-up strategies using an individual-based population model of mink.

    PubMed

    Salice, Christopher J; Sample, Bradley E; Miller Neilan, Rachael; Rose, Kenneth A; Sable, Shaye

    2011-12-01

    Population models can be used to place observed toxic effects into an assessment of the impacts on population-level endpoints, which are generally considered to provide greater ecological insight and relevance. We used an individual-based model of mink to evaluate the population-level effects of exposure to polychlorinated biphenyls (PCBs) and the impact that different remediation strategies had on mink population endpoints (population size and extinction risk). Our simulations indicated that the initial population size had a strong impact on mink population dynamics. In addition, mink populations were extremely responsive to clean-up scenarios that were initiated soon after the contamination event. In fact, the rate of PCB clean-up did not have as strong a positive effect on mink as did the initiation of clean-up (start time). We show that population-level approaches can be used to understand adverse effects of contamination and to also explore the potential benefits of various remediation strategies.

  6. Hudson River PCB clean-up to begin

    NASA Astrophysics Data System (ADS)

    Showstack, Randy

    U.S. Environmental Protection Agency Administrator Christie Whitman signed the Record of Decision on 1 February to clean up a stretch of the Hudson River that has been contaminated by polychlorinated biphenyls (PCBs). The decision calls for dredging 2 million cubic meters of PCB-contaminated sediment from a 64-kilometer stretch of the upper Hudson to remove about 68,000 kilograms of PCBs.The plan follows years of scientific study about whether the PCBs were safely encased in the sediment or posed a continuing hazard, and concern over whether the PCBs can be safely removed without stirring up a larger pollution problem along the river. The EPA found that PCBs in the sediment are not safely buried because erosion and river flows can redistribute river sediment. The agency also found that although PCBs break down naturally over time, this degradation does not render them harmless.

  7. Impact of soil heterogeneity on measuring the attainment of PCB clean-up standards

    SciTech Connect

    Phillips, I.M.; Ghirardi, J.K.; Morin, J.O.

    1996-12-31

    The sources of variance in the results of samples collected during a pilot-scale remediation treatability testing for PCBs were evaluated using basic statistical methods. The relative contributions of soil heterogeneity and chemical testing methods were estimated. The sources of variance were estimated using both inter- and intralaboratory testing and the determination of the total variance of each sample set. It was found that 67 to 94 percent of the variance in the results was contributed by the sample heterogeneity which can not be readily controlled. The results of treated samples from the pilot-scale treatability testing showed a mean concentration of PCBs of 13.6 ppm with a standard deviation of 10.1. The range of the distribution of concentrations was 1.3 to 35 ppm. Based on these findings, it is inappropriate to use an absolute clean-up standard to evaluate whether the clean-up has been achieved. The use of the mean is more appropriate as it takes into account the variance in the results caused by sample heterogeneity.

  8. Monitoring the clean-up operation of agricultural fields flooded with red mud in Hungary.

    PubMed

    Uzinger, Nikolett; Rékási, Márk; Anton, Áron D; Koós, Sándor; László, Péter; Anton, Attila

    2016-12-01

    In the course of the clean-up operation after the red mud inundation in 2010, red mud was removed from the soil surface in places where the layer was more than 5 cm deep. Before its removal, the red mud seeped into the soil. In 2012, soil samples were taken from depths of 0 to 20 and 20 to 40 cm on some of the affected areas. The parameters investigated were pH, organic matter, salt%, and the total and mobile fractions of various elements. The values recorded in 2012 were compared with those measured immediately after the removal of the red mud in 2010 and with the background and clean-up target concentrations. The pH values remained below the designated limit, while the salt content only exhibited values in the weakly salty range on areas at the greatest distance from the dam. In the central part of the inundated area, total Na contents above the 900 mg/kg target value were observed, but the Na content in the 0-20-cm layer generally exhibited a decrease due to leaching. The pH and As concentration also showed a decline on several areas compared with the values recorded in 2010. Total As and Co contents in excess of the target values were recorded on the lowest-lying part of the flooded area, probably because the finest red mud particles were deposited the furthest from the dam, where they seeped into the soil. Nevertheless, the mobility and plant availability of both elements remained moderate. The total contents of both Co and Mo, however, exhibited a significant rise compared with both the background value and the 2010 data. The monitoring of the cleaned-up areas showed that after a 2-year period element concentrations that exceeded the target values and could be attributed to the red mud pollution were only detectable on the lowest-lying areas.

  9. Next steps in the development of ecological soil clean-up values for metals.

    PubMed

    Wentsel, Randall; Fairbrother, Anne

    2014-07-01

    This special series in Integrated Environmental Assessment Management presents the results from 6 workgroups that were formed at the workshop on Ecological Soil Levels-Next Steps in the Development of Metal Clean-Up Values (17-21 September 2012, Sundance, Utah). This introductory article presents an overview of the issues assessors face when conducting risk assessments for metals in soils, key US Environmental Protection Agency (USEPA) documents on metals risk assessment, and discusses the importance of leveraging from recent major terrestrial research projects, primarily to address Registration, Evaluation, Authorization and Restriction of Chemical Substances (REACH) requirements in Europe, that have significantly advanced our understanding of the behavior and toxicity of metals in soils. These projects developed large data sets that are useful for the risk assessment of metals in soil environments. The workshop attendees met to work toward developing a process for establishing ecological soil clean-up values (Eco-SCVs). The goal of the workshop was to progress from ecological soil screening values (Eco-SSLs) to final clean-up values by providing regulators with the methods and processes to incorporate bioavailability, normalize toxicity thresholds, address food-web issues, and incorporate background concentrations. The REACH data sets were used by workshop participants as case studies in the development of the ecological standards for soils. The workshop attendees discussed scientific advancements in bioavailability, soil biota and wildlife case studies, soil processes, and food-chain modeling. In addition, one of the workgroups discussed the processes needed to frame the topics to gain regulatory acceptance as a directive or guidance by Canada, the USEPA, or the United States.

  10. Development of hot gas clean-up system for IGCC

    SciTech Connect

    Hori, Tetsuya

    1999-07-01

    The syngas generated at the gasifier in the Integrated Gasification Combined Cycle (IGCC) is reductive gas, so the sulfur in the fuel is reduced to H{sub 2}S and COS. Many wet types of gas clear up systems using liquid solvents are commercially available. However, the authors have been developing the higher performance and efficient system using oxide metals sorbent, that they call Hot Gas Clean Up system (HGCU system) with fluidized bed reactors. Therefore, the authors have participated, in Yubari and Nakoso pilot plant projects as the national project to develop and establish the HGCU system and it's technology to realize lower environmental emission and high thermal efficiency. The test results of those pilot plants had a very good performance and the authors have confirmed that the HGCU system is applicable to IGCC plant. Those pilot plants have used the iron oxide (crashed iron ore) as the desulfurization sorbent. However, the iron oxide sorbent cannot get high desulfurization performance for the gas containing high moisture (about 10 vol% and over) and cannot reach environmental requirements of the near future. Thus, the authors have developed the HGCU system using zinc oxide sorbent that is expected to have higher desulfurization performance. They have carried out many tests at the Coal Gasification Test facility (CGT test plant). They achieved 20 ppmV total HGCU system has high performance and reliability.

  11. Using Phytoremediation to Clean Up Contamination at Military Installations

    SciTech Connect

    Zellmer, S.D.; Hinchman, R.R.; Negri, M.C.; Schneider, J.F.; Gatliff, E.G.

    1997-07-01

    During and following World War II, wastes from the production of munitions and other military materials were disposed of using the best available practices acceptable at that time. However, these disposal methods often contaminated soil and groundwater with organic compounds and metals that require cleanup under current regulations. An emerging technology for cleaning contaminated soils and shallow groundwater is phytoremediation, an environmentally friendly, low- cost, and low-tech process. Phytoremediation encompasses all plant- influenced biological, chemical, and physical processes that aid in the uptake, degradation, and metabolism of contaminants by either plants or free-living organisms in the plant`s rhizosphere. A phytoremediation system can be viewed as a biological, solar-driven, pump-and-treat system with an extensive, self-extending uptake network (the root system) that enhances the soil and below-ground ecosystem for subsequent productive use. Argonne National Laboratory (ANL) has been conducting basic and applied research in phytoremediation since 1990. Initial greenhouse studies evaluated salt-tolerant wetland plants to clean UP and reduce the volume of salty `produced water` from petroleum wells. Results of these studies were used to design a bioreactor for processing produced water that is being demonstrated at a natural gas well in Oklahoma; this system can reduce produced water volume by about 75% in less than eight days, representing substantial savings in waste disposal cost. During 1994, ANL conducted a TNT plant uptake and in situ remediation study in a ridge-and-furrow area used for the disposal of pink water at the Joliet Army Ammunition Plant.

  12. Comparison of solid phase extraction, saponification and gel permeation chromatography for the clean-up of microwave-assisted biological extracts in the analysis of polycyclic aromatic hydrocarbons.

    PubMed

    Navarro, P; Cortazar, E; Bartolomé, L; Deusto, M; Raposo, J C; Zuloaga, O; Arana, G; Etxebarria, N

    2006-09-22

    The feasibility of different clean-up procedures was studied for the determination of polycyclic aromatic hydrocarbons (PAHs) in biota samples such as oysters, mussels and fish liver. In this sense, once the samples were extracted--essentially with acetone and in a microwave system--and before they could be analysed by gas chromatography-mass spectrometry (GC-MS), three different approaches were studied for the clean-up step: solid phase extraction (SPE), microwave-assisted saponification (MAS) and gel permeation chromatography (GPC). The main aim of this work was to maximise the recoveries of PAHs and to minimise the presence of interfering compounds in the last extract. In the case of SPE, Florisil cartridges of 1, 2 and 5 g, and silica cartridges of 5 g were studied. In that case, and with oysters and mussels, microwave-assisted extraction and 5 g Florisil cartridges provided good results. In addition, the concentrations obtained for Standard Reference Material (SRM) NIST 2977 (mussel tissue) were in good agreement with the certified values. In the case of microwave-assisted saponification, the extracts were not as clean as those obtained with 5 g Florisil and this fact lead to overestimate the concentration of the heaviest PAHs. Finally, the cleanest extracts were obtained by GPC. The method was successfully applied to mussels, oysters and hake liver, and the results obtained for NIST 2977 (mussel tissue) were within the confidence interval of the certified reference material for most of the certified analytes.

  13. [Determination of indicator polychlorinated biphenyls in vegetable oils by double clean-up-gas chromatography].

    PubMed

    Ding, Liping; Cai, Chunping; Wang, Danhong

    2014-11-01

    To investigate the residues of seven indicator polychlorinated biphenyls (PCBs) in vegetable oils, a method was established for the determination of trace PCBs in vegetable oils by double clean-up coupled with gas chromatography (GC). After extracted with acetonitrile, the sample extract was concentrated to dryness followed by re-dissolving with hexane. And the solution was pretreated by adding concentrated sulfuric acid followed cleaned-up with silica gel in dispersive solid-phase extraction protocol, then analyzed by GC with external standard meth- od. Under the optimized chromatographic conditions, the analysis was carried out with a capillary column (HP-5, 30 m x 0.32 mm x 0.25 μm) at a flow rate of 0.8 mL/min, and the sample volume was 1.00 μL. Monitoring with an electron-capture detector, all the target analytes were separated by temperature-programming of the column. Good linearities were obtained in the range of 10-500 μg/L for the seven indicator PCBs with the correlation coefficients greater than 0. 999. For different matrices, the limits of detection (S/N = 3) and limits of quantitation (S/N = 10) were in the range of 1.8-8.9 pg/kg and 5.9-29.8 μg/kg, respectively. At three spiked levels of 10, 20 and 100 μg/kg of the seven indicator PCBs in olive oil, palm oil and peanut oil blank samples, the average recoveries ranged from 71.0% to 105.5% with the RSDs of 4.0%-11.3%. The method is simple, rapid and accurate, and can be used for the routine analysis of the indicator PCBs in vegetable oils.

  14. CE-ECL detection of gatifloxacin in biological fluid after clean-up using SPE.

    PubMed

    Fu, Zhifeng; Wang, Lin; Li, Cuifang; Liu, Ying; Zhou, Xueting; Wei, Wei

    2009-11-01

    A simple, rapid and sensitive CE method has been proposed for the determination of gatifloxacin in biological fluid. This method is based on the ECL reaction of gatifloxacin and tris(2,2'-bipyridyl)ruthenium(II) occurred in the end-column detection cell. Under the optimal conditions, gatifloxacin can be assayed within 10 min over the concentration range of 5.0x10(-8)-5.0x10(-6) g/mL with the theoretical plate numbers of 18,000. The intra-day and inter-day precision of the signal intensity and the migration time shows acceptable reproducibility for the analysis of gatifloxacin. The presented method has been successfully applied to determine the concentrations of gatifloxacin in urine and blood samples after clean-up using C(18) SPE column.

  15. 25 CFR 170.906 - Who cleans up radioactive and hazardous material spills?

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 25 Indians 1 2013-04-01 2013-04-01 false Who cleans up radioactive and hazardous material spills? 170.906 Section 170.906 Indians BUREAU OF INDIAN AFFAIRS, DEPARTMENT OF THE INTERIOR LAND AND WATER... § 170.906 Who cleans up radioactive and hazardous material spills? The carrier is typically...

  16. 25 CFR 170.906 - Who cleans up radioactive and hazardous material spills?

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 25 Indians 1 2010-04-01 2010-04-01 false Who cleans up radioactive and hazardous material spills? 170.906 Section 170.906 Indians BUREAU OF INDIAN AFFAIRS, DEPARTMENT OF THE INTERIOR LAND AND WATER... § 170.906 Who cleans up radioactive and hazardous material spills? The carrier is typically...

  17. 25 CFR 170.906 - Who cleans up radioactive and hazardous material spills?

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 25 Indians 1 2012-04-01 2011-04-01 true Who cleans up radioactive and hazardous material spills? 170.906 Section 170.906 Indians BUREAU OF INDIAN AFFAIRS, DEPARTMENT OF THE INTERIOR LAND AND WATER... § 170.906 Who cleans up radioactive and hazardous material spills? The carrier is typically...

  18. 25 CFR 170.906 - Who cleans up radioactive and hazardous material spills?

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 25 Indians 1 2011-04-01 2011-04-01 false Who cleans up radioactive and hazardous material spills? 170.906 Section 170.906 Indians BUREAU OF INDIAN AFFAIRS, DEPARTMENT OF THE INTERIOR LAND AND WATER... § 170.906 Who cleans up radioactive and hazardous material spills? The carrier is typically...

  19. The use of the Karl sub-scale laser for Raman beam clean-up experiments

    NASA Astrophysics Data System (ADS)

    Dudas, Alan J.; Burris, Harris R.

    1987-03-01

    The two X-ray preionized discharge pumped front end lasers for the Raman Beam Clean-up Experiment (LARBC) have been examined both optically and electrically in an effort to increase the optical and temporal quality of the injection locked beam produced. The KARL subscale has been successfully injection locked by the front end lasers and preliminary studies of the stability of the injection locking begun. An isolator system has been designed and constructed to prevent damage to system optics from energy moving the wrong way in the system. A gas processing system was tested to remove contaminants in the laser gas. Additional units have been purchased for use on all lasers in the system. Diagnostics for the experiment will be coordinated through the WP3202 digitizing system.

  20. Planar solid phase extraction clean-up and microliter-flow injection analysis-time-of-flight mass spectrometry for multi-residue screening of pesticides in food.

    PubMed

    Oellig, Claudia; Schwack, Wolfgang

    2014-07-18

    For multi-residue analysis of pesticides in food, a sufficient clean-up is essential for avoiding matrix effects in liquid and gas chromatography (LC and GC) analysis coupled to mass spectrometry (MS). In the last two years, high-throughput planar solid phase extraction (HTpSPE) was established as a new clean-up concept for pesticide residue analysis in fruits and vegetables (C. Oellig, W. Schwack, 2011) and tea (C. Oellig, W. Schwack, 2012). HTpSPE results in matrix-free extracts almost free of interferences and matrix effects. In this study, a time-of-flight mass spectrometer (TOFMS) was applied to directly analyze HTpSPE extracts for pesticide residues. This HTpSPE-microliter-flow injection analysis (μL-FIA)-TOFMS approach detects all pesticides at once in a single mass spectrum, without a liquid chromatographic separation step. Complete sample information was obtained after the injection of the cleaned extract within a single peak. Recovery studies for seven representative pesticides in four different matrices (apples, red grapes, cucumbers, tomatoes) provided mean recoveries of 86-116% with relative standard deviations of 1.3-10% (n=5) using the mass signal intensities under the entire sample peak. Comparing the mass spectra of sample peaks from spiked extracts and solvent standards indicated the efficiency of HTpSPE clean-up. A pesticide database search detected all spiked pesticides with a low incidence of false-positives. HTpSPE of one sample required a few minutes, and numerous samples could be cleaned in parallel at minimal cost with low sample and solvent consumption. The μL-FIA-TOFMS screening then needed an additional 6min per sample. The novel screening approach was successfully applied to QuEChERS extracts of several real samples, and the pesticides identified by HTpSPE-μL-FIA-TOFMS were identical to the pesticides detected by common target LC-MS/MS analyses. The high degree of concordantly identified pesticides by the new developed HTp

  1. EPA Report: Diesel Engine Clean-up Program Nets Major Air, Public Health Benefits

    EPA Pesticide Factsheets

    Atlanta, GA - Clean diesel grants aimed at cleaning up old diesel engines have greatly improved public health by cutting harmful pollution that causes premature deaths, asthma attacks, and missed school and workdays, according to a new report by the

  2. EVALUATION OF PERSONAL COOLING DEVICES FOR A DIOXIN CLEAN-UP OPERATION

    EPA Science Inventory

    The study investigated the use of personal coolers to increase worker productivity and safety while working at elevated, ambient temperatures cleaning up dioxin contaminated soil.^The study included laboratory tests to measure the thermal characteristics of the chemical protectiv...

  3. EPA Reaches $55 Million Settlement for Soil Clean-up at South-Bay Superfund Site

    EPA Pesticide Factsheets

    These funds are key to advancing our cleanup actions at this site, said Jared Blumenfeld, EPA's Regional Administrator for the Pacific Southwest. EPA looks forward to working with local residents as we clean up and revitalize their neighborhood, which h

  4. Palm Beach County to Receive $300,000 to Clean up and Redevelop Contaminated Brownfields Sites

    EPA Pesticide Factsheets

    ATLANTA - Today the U.S. Environmental Protection Agency (EPA) announced that Palm Beach County will receive $300,000 to clean up and redevelop contaminated brownfields sites in Florida. Nationally, approximately $13.2 million in supplemental

  5. Dunbar Asphalt to Clean up 29-Acre Portion of Sharon Steel Superfund Site, Hermitage, Pa.

    EPA Pesticide Factsheets

    PHILADELPHIA (Sept. 14, 2015) The U.S. Environmental Protection Agency today announced a proposed settlement the government has reached with Dunbar Asphalt Products, Inc., to clean up a 29-acre portion of the Sharon Steel Corporation Superfund Site

  6. Development of a molecularly imprinted polymer for prometryne clean-up in the environment.

    PubMed

    Guo, Li Juan; Qu, Jin Rong; Miao, Shan Shan; Geng, Hao Ran; Yang, Hong

    2013-12-01

    Molecularly imprinted polymers (MIPs) are prepared on the surface of modified silica gel using prometryne as a template, methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as a crosslinker, and 2,2-azobisisobutyronitrile as an initiator. The structure of the MIPs was characterized using SEM and FTIR spectroscopy. The selectivity of the MIPs for the template molecule prometryne was proven by adsorption experiments. Highly selective SPE cartridges of MIP particles were developed and an optimized prometryne procedure was developed for the enrichment and clean-up of prometryne residues in water, soil, and wheat samples. The concentrations of prometryne in the samples were analyzed by HPLC. The average recoveries of prometryne spiked for water at 0.05∼0.8 mg/L were 101.47-106.65% and the RSD was 2.63-4.71%. The average recoveries of prometryne spiked for soil at 0.05∼0.8 mg/L were 87.34-94.91% with the RSD being 2.77-8.41%. The average recoveries of prometryne spiked for wheat plant at 0.2∼2.0 mg/kg were 91.04-97.76% with the RSD being 6.53-10.69%. The method developed here can be regenerated and repeatedly used more than two dozen times.

  7. Separation and determination of citrinin in corn using HPLC fluorescence detection assisted by molecularly imprinted solid phase extraction clean-up

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A liquid chromatography based method to detect citrinin in corn was developed using molecularly imprinted solid phase extraction (MISPE) sample clean-up. Molecularly imprinted polymers were synthesized using 1,4-dihydroxy-2-naphthoic acid as the template and an amine functional monomer. Density func...

  8. 7 CFR 27.25 - Additional samples of cotton; drawing.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... 7 Agriculture 2 2014-01-01 2014-01-01 false Additional samples of cotton; drawing. 27.25 Section... CONTAINER REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.25 Additional samples of cotton; drawing. In addition to the samples hereinbefore...

  9. 7 CFR 27.25 - Additional samples of cotton; drawing.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... 7 Agriculture 2 2012-01-01 2012-01-01 false Additional samples of cotton; drawing. 27.25 Section... CONTAINER REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.25 Additional samples of cotton; drawing. In addition to the samples hereinbefore...

  10. 7 CFR 27.25 - Additional samples of cotton; drawing.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 7 Agriculture 2 2011-01-01 2011-01-01 false Additional samples of cotton; drawing. 27.25 Section... CONTAINER REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.25 Additional samples of cotton; drawing. In addition to the samples hereinbefore...

  11. 7 CFR 27.25 - Additional samples of cotton; drawing.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 7 Agriculture 2 2010-01-01 2010-01-01 false Additional samples of cotton; drawing. 27.25 Section... CONTAINER REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.25 Additional samples of cotton; drawing. In addition to the samples hereinbefore...

  12. 7 CFR 27.25 - Additional samples of cotton; drawing.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... 7 Agriculture 2 2013-01-01 2013-01-01 false Additional samples of cotton; drawing. 27.25 Section... CONTAINER REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.25 Additional samples of cotton; drawing. In addition to the samples hereinbefore...

  13. Detection of THCCOOH in hair by MSD-NCI after HPLC clean-up.

    PubMed

    Sachs, H; Dressler, U

    2000-01-10

    Regular consumption of cannabis can easily be detected by examination of hair for tetrahydrocannabinol, cannabinol, and cannabidiol. Although several studies have demonstrated that after contamination with smoke or treatment with THC containing shampoos THC is not detectable, or only in small traces, the detection of 11-nor-9-carboxy-delta 9-tetrahydrocannabinol (THCCOOH) should be offered to prove the consumption and metabolisation of THC. Up to now this confirmation was only available using tandem MS techniques combined with negative chemical ionisation. A new method using a normal quadrupole GC/MS is described. The lack of expensive instruments has to be paid for by a costly and time consuming extraction and clean-up. After the sample has been digested by 2 M NaOH at 95 degrees C and the neutralised liquid has been extracted with a mixture of n-hexane and ethyl acetate the dried residue is reconstituted in acetonitrile-methanol-0.01 M sulfuric acid (49:21:30, v/v/v) and the cannabinoids separated by HPLC. Each fraction is collected over 1 min. Another extraction with n-hexane-ethyl acetate is followed by evaporation, derivatisation, and GC/MS determination. The calibration with THCCOOH spiked hair led to a LOD of 0.3 pg/mg and a LOQ of 1.1 pg/mg.

  14. Salt clean-up procedure for the determination of domoic acid by HPLC.

    PubMed

    Hatfield, C L; Wekell, J C; Gauglitz, E J; Barnett, H J

    1994-01-01

    Domoic acid (DA) was first reported in mussels from Prince Edward Island, Canada, in 1987. It reappeared in anchovies and pelicans from Monterey Bay, California, in 1991. Later that year, domoic acid was found in razor clams and Dungeness crabs along the Washington and Oregon coasts. Since the initial outbreak, a variety of analytical methods for the detection of this neurotoxin have been developed. Here, we describe a modification to the solid phase extraction (SPE) clean-up step in Quilliam's HPLC-UV method (1991: NRCC No. 33001). The standard 10% acetonitrile (MeCN) wash and 0.5M ammonium citrate buffer (ACB) in 10% MeCN (pH = 4.5) eluting solution have been replaced with a 0.1M sodium chloride (NaCl) in 10% MeCN wash and a 0.5M NaCl in 10% MeCN eluting solution. This modification allows the analysis to work equally well on both clam and crab viscera and meat. Chromatograms of visceral samples no longer contain interfering or late eluting peaks; and all chromatograms are free of the large solvent peak tailing associated with the ACB eluent. The newly modified method allows for an improved and more versatile domoic acid analysis.

  15. Cleaning Up.

    ERIC Educational Resources Information Center

    Walker, John

    2002-01-01

    Offers strategies to make schools' cleaning operations run more smoothly. Discusses how to estimate the amount of space that needs cleaning and how long it should take, the benefits of team cleaning versus zone cleaning, and the importance of monitoring complaints and overtime to ensure staff is performing efficiently. (EV)

  16. Cleaning up

    SciTech Connect

    Perry, T.S.

    1993-02-01

    This article reports on the electronics manufacturer's response to findings that chemicals used in manufacturing integrated circuits induced miscarriages in plant workers and other environmental problems such as ozone depletion and the use of heavy metals and toxic gases in manufacturing. The topics of the article include the finding that a photoresist is at fault, the phase-out of ethylene glycol ethers, alternatives to ethylene glycol ethers, ozone-eating CFCs, use of citrus derived substitutes for CFCs, alternative manufacturing processes, substitutes for other ozone depleting chemicals, and the use of heavy metals in electronics manufacturing.

  17. Multiplug filtration clean-up with multiwalled carbon nanotubes in the analysis of pesticide residues using LC-ESI-MS/MS.

    PubMed

    Zhao, Pengyue; Fan, Sufang; Yu, Chuanshan; Zhang, Junyan; Pan, Canping

    2013-10-01

    A novel design for a rapid clean-up method was developed for the analysis of pesticide residues in fruit and vegetables followed by LC-ESI-MS/MS. The acetonitrile-based sample extraction technique was used to obtain the extracts, and further clean-up was carried out by applying the streamlined procedure on a multiplug filtration clean-up column coupled with a syringe. The sorbent used for clean-up in this research is multiwalled carbon nanotubes, which was mixed with anhydrous magnesium sulfate to remove water from the extracts. This method was validated on 40 representative pesticides and apple, cabbage, and potato sample matrices spiked at two concentration levels of 10 and 100 μg/kg. It exhibited recoveries between 71 and 117% for most pesticides with RSDs < 15%. Matrix-matched calibrations were performed with the coefficients of determination >0.995 for most studied pesticides between concentration levels of 10-500 μg/L. The LOQs for 40 pesticides ranged from 2 to 50 μg/kg. The developed method was successfully applied to the determination of pesticide residues in market fruit and vegetable samples.

  18. Application of single immunoaffinity clean-up for simultaneous determination of regulated mycotoxins in cereals and nuts.

    PubMed

    Vaclavikova, Marta; MacMahon, Shaun; Zhang, Kai; Begley, Timothy H

    2013-12-15

    A rapid and sensitive analytical strategy for the simultaneous determination of twelve mycotoxins (aflatoxins, fumonisins, zearalenon, deoxynivalenol, ochratoxin A, T-2 and HT-2 toxins) using ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was developed and validated. The method was validated for peanuts, barley and maize-breakfast cereals; selected as they represent the matrices most often contaminated by mycotoxins. The method is designed for fast and reliable analyses of mycotoxins in regulatory, industrial and private laboratories. Multi-target immunoaffinity columns containing antibodies for all mycotoxins studied herein were used for sample clean-up. Method optimization was predominantly focused on the simplification of extraction and clean-up procedure recommended by column producers. This newly developed and simplified procedure decreased both the sample preparation time and the solvent volumes used for their processing. The analysis of all regulated mycotoxins was conducted by a newly developed UHPLC-MS/MS method with a sample run time of only ten minutes. The method trueness was tested with analytical spikes and certified reference materials, with recoveries ranging from 71% to 112% for all of the examined mycotoxins.

  19. Analysis of sterigmatocystin in cereals, animal feed, seeds, beer and cheese by immunoaffinity column clean-up and HPLC and LC-MS/MS quantification.

    PubMed

    Marley, Elaine; Brown, Phyllis; Mackie, Jennifer; Donnelly, Carol; Wilcox, Joyce; Pietri, Amedeo; Macdonald, Susan

    2015-01-01

    A method is reported for the analysis of sterigmatocystin in various food and feed matrices using a commercial sterigmatocystin immunoaffinity column (IAC) for sample clean-up prior to HPLC analysis by UV with mass spectrometric detection (LC-MS/MS). Cereals (wheat, oats, rye, maize and rice), sunflower seeds and animal feed were spiked with sterigmatocystin at levels from 0.75 to 50 µg kg(-1) to establish method performance. Using acetonitrile/water extraction followed by IAC clean-up, and analysis by HPLC with detection at 325 nm, recoveries ranged from 68% to 106%, with repeatability from 4.2% to 17.5%. The limit of quantification with UV detection in these matrices was 1.5 µg kg(-1). For the analysis of beer and cheese the sample preparation prior to IAC clean-up was changed to accommodate the different properties of the matrix, prior to analysis by LC-MS/MS. For beer and cheese spiked at 5.0 µg kg(-1) the recoveries were 94% and 104%, and precision (RSDs) were 1.9% and 2.9% respectively. The limits of quantification by LC-MS/MS in beer and cheese were 0.02 and 0.6 µg kg(-1) respectively. The sterigmatocystin IAC was demonstrated to provide an efficient clean-up of various matrices to enable this mycotoxin to be determined by either HPLC with UV detection or LC-MS/MS.

  20. Validation data for HPLC/FLD determinations of ochratoxin A in red paprika and black pepper adopting a one-step clean-up procedure.

    PubMed

    Bononi, M; Gallone, F; Tateo, F

    2010-02-01

    Validation data for the determination of ochratoxin A (OTA) in two spice matrices, red paprika and black pepper, were obtained for samples prepared with a simplified single-step clean-up column. Extracts of finely ground samples of red paprika and black pepper were prepared and applied to a Mycosep 229 Ochra clean-up column. The purified extract was then subjected to HPLC/FLD analysis. The relative standard deviation for repeatability (RSDr) of the method was 11.8% for red paprika and 9.9% for black pepper. The limit of detection (LOD) value (three times the noise) was estimated as corresponding to the response of an extract derived from a blank matrix (previously washed) and spiked at 1.0 microg kg(-1). The limit of quantitation (LOQ) (three times LOD) was 3.0 microg kg(-1). The performance of the one-step column clean-up procedure appears to be a suitable alternative to commonly used clean-up techniques and allows the precise determination of OTA in two complex matrices.

  1. Dyscirculatory encephalopathy in Chernobyl disaster clean-up workers (a 20-year study).

    PubMed

    Podsonnaya, I V; Shumakher, G I; Golovin, V A

    2010-05-01

    Results obtained over 20-years of following 536 Chernobyl clean-up workers and 436 control subjects are presented. Dyscirculatory encephalopathy developed more frequently in persons exposed to radiation at age 30 years. As compared with the control group, workers were characterized by early onset of disease, faster progression, stable symptomatology for 5-6 years, and further progression of disease in the form of autonomic dysfunction, psycho-organic syndrome, and epilepsy. Major strokes were also more common in clean-up workers.

  2. EPA Report: Diesel Engine Clean-up Program Nets Major Air, Public Health Benefits

    EPA Pesticide Factsheets

    (New York, N.Y.) Clean diesel grants aimed at cleaning up old diesel engines have greatly improved public health by cutting harmful pollution that causes premature deaths, asthma attacks, and missed school and workdays, according to a new report by the U.S

  3. Clean Up, Rehabilitation, Resettlement of Enewetak Atoll -Marshall Islands. Volume III.

    DTIC Science & Technology

    The documentation is a summary of the Draft Environmental Impact Statement (DEIS) for a proposed project to clean up the Atoll of Enewetak and...resettle the Enewetak people on the Atoll . The summary has been prepared specifically for translation into the language of the Enewetak people.

  4. TECHNICAL APPROACHES TO CHARACTERIZING AND CLEANING UP BROWNFIELDS SITES: GUIDANCE DOCUMENT

    EPA Science Inventory

    NRMRL-CIN-1741 SAIC. Technical Approaches to Characterizing and Cleaning up Brownfields Sites. EPA/625/R/00/009 (NTIS PB2002-105021) , Available: 68-C7-0011. The guidance document gives assistance to communities, decision-makers, states and municipalities, academia, and the p...

  5. Case Study: Using Microbe Molecular Biology for Gulf Oil Spill Clean Up

    ERIC Educational Resources Information Center

    Jones, Daniel R.

    2011-01-01

    This case has the student actively investigate the regulation of expression of a novel bacterial gene in the context of attempts to solve a real world problem, clean up of the April 2010 Deep Water Horizon oil spill in the Gulf of Mexico. Although the case is fictitious, it is based on factual gene regulatory characteristics of oil-degrading…

  6. 25 CFR 170.906 - Who cleans up radioactive and hazardous material spills?

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 25 Indians 1 2014-04-01 2014-04-01 false Who cleans up radioactive and hazardous material spills? 170.906 Section 170.906 Indians BUREAU OF INDIAN AFFAIRS, DEPARTMENT OF THE INTERIOR LAND AND WATER... Federal agencies to address all cleanup issues, such as arranging or repackaging of the cargo,...

  7. 75 FR 26098 - Safety Zone; Under Water Clean Up of Copper Canyon, Lake Havasu, AZ

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-05-11

    ... SECURITY Coast Guard 33 CFR Part 165 RIN 1625-AA00 Safety Zone; Under Water Clean Up of Copper Canyon, Lake... establishing a temporary safety zone on the navigable waters of Lake Havasu in the Copper Canyon in support of the underwater cleanup of Copper Canyon. This temporary safety zone is necessary to provide for...

  8. EPA Orders CSX to Clean up Areas Impacted by West Virginia Train Derailment

    EPA Pesticide Factsheets

    PHILADELPHIA (Feb. 27, 2015 ) - Today, the U.S. Environmental Protection Agency ordered CSX to clean-up and restore the areas affected by the Feb. 16 train derailment in Mt. Carbon, W. Va. Twenty-seven cars derailed from the 109-car CSX train carryin

  9. Chromosome aberrations and rogue cells in lymphocytes of Chernobyl clean-up workers.

    PubMed

    Lazutka, J R

    1996-03-09

    A cytogenetic analysis was performed on peripheral blood lymphocytes from 183 Chernobyl clean-up workers and 27 control individuals. Increased frequencies of chromosome aberrations were associated with exposure to radiation at Chernobyl, alcohol abuse and a history of recent influenza infection. However, only approximately 20% of Chernobyl clean-up workers had an increased frequency of dicentric and ring chromosomes. At the same time, an increased frequency of acentric fragments in lymphocytes of clean-up workers was characteristic. The use of multivitamins as dietary supplement significantly decreased the frequency of chromosome aberrations, especially of chromatid breaks. Rogue cells were found in lymphocytes of 28 clean-up workers and 3 control individuals. The appearance of rogue cells was associated with a recent history of acute respiratory disease (presumably caused by adenoviral infection) and, probably, alcohol abuse. Dicentric chromosomes in rogue cells were distributed according to a negative binomial distribution. Occurrence of rogue cells due to a perturbation of cell cycle control and abnormal apoptosis is suggested.

  10. Determination of fusaric acid in maize using molecularly imprinted SPE clean-up

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A new liquid chromatography method to detect fusaric acid in maize is reported based on molecularly imprinted polymer solid phase extraction clean-up (MISPE) using mimic-templated molecularly-imprinted polymers. Picolinic acid was used as a toxin analog for imprinting polymers during a thermolytic s...

  11. Efficiency of different protocols for enamel clean-up after bracket debonding: an in vitro study

    PubMed Central

    Sigilião, Lara Carvalho Freitas; Marquezan, Mariana; Elias, Carlos Nelson; Ruellas, Antônio Carlos; Sant'Anna, Eduardo Franzotti

    2015-01-01

    Objective: This study aimed to assess the efficiency of six protocols for cleaning-up tooth enamel after bracket debonding. Methods: A total of 60 premolars were divided into six groups, according to the tools used for clean-up: 12-blade bur at low speed (G12L), 12-blade bur at high speed (G12H), 30-blade bur at low speed (G30L), DU10CO ORTHO polisher (GDU), Renew System (GR) and Diagloss polisher (GD). Mean roughness (Ra) and mean roughness depth (Rz) of enamel surface were analyzed with a profilometer. Paired t-test was used to assess Ra and Rz before and after enamel clean-up. ANOVA/Tukey tests were used for intergroup comparison. The duration of removal procedures was recorded. The association between time and variation in enamel roughness (∆Ra, ∆Rz) were evaluated by Pearson's correlation test. Enamel topography was assessed by scanning electron microscopy (SEM). Results: In Groups G12L and G12H, original enamel roughness did not change significantly. In Groups G30L, GDU, GR and GD, a smoother surface (p < 0.05) was found after clean-up. In Groups G30L and GD, the protocols used were more time-consuming than those used in the other groups. Negative and moderate correlation was observed between time and (∆Ra, ∆Rz); Ra and (∆Ra, ∆Rz); Rz (r = - 0.445, r = - 0.475, p < 0.01). Conclusion: All enamel clean-up protocols were efficient because they did not result in increased surface roughness. The longer the time spent performing the protocol, the lower the surface roughness. PMID:26560825

  12. Individual and workplace monitoring measurements made after a 240Pu incident and during the clean-up operations.

    PubMed

    Hochmann, R; Eisenwagner, H; Benesch, T; Hunt, J; Cruz-Suarez, R; Bulyha, S; Schmitzer, C

    2011-03-01

    On 3 August 2008, five glass vials containing around 7 GBq of (240)Pu in nitric acid solution burst in a laboratory operated by the IAEA in Seibersdorf, Austria. The vials were located in a fire-proof safe in the IAEA Safeguards Analytical Laboratory, and the release of the (240)Pu caused an air contamination in the room and in adjoining rooms. Immediate emergency work was carried out, which was then followed by a long period of clean-up operations. A large number of conventional individual and workplace monitoring measurements were carried out immediately after the incident and during the clean-up work. In addition, due to the fact that (240)Pu has a very low background presence in the environment, and that the IAEA laboratories operate an inductively coupled plasma mass spectrometry system capable of very low levels of detection of this radionuclide, a number of non-conventional measurements were made to detect (240)Pu on, for example, the photographic camera used to document the incident, on nasal swabs from the first responders, etc. Plastic beakers were left in the corridor of the controlled area to accumulate (240)Pu from precipitation to see whether it was possible to detect traces of the radionuclide. This paper presents the measurements obtained, and discusses their relevance to occupational radiation protection.

  13. OPERATION OF A TRITIUM GLOVEBOX CLEAN-UP SYSTEM USING ZIRCONIUM MANGANESE IRON AND ZIRCONIUM TWO IRON METAL GETTERS

    SciTech Connect

    E. LARSON; K. COOK

    2000-08-01

    A metal hydride-based tritium clean-up system has been successfully operated for more than four years on an 11 m{sup 3} helium/nitrogen glovebox which was used for handling metal tritide powders. The clean-up system consists of two beds: (1) a Zr-Mn-Fe (in a 10% by weight Al binder, SAES ST909) bed operating at 675 C followed by (2) a Zr{sub 2}Fe (SAES ST198) bed operating at 250 C. The Zr-Mn-Fe bed serves to condition the gas stream by cracking hydrogenous impurities (such as H{sub 2}O and hydrocarbons) and absorbing oxygen and carbon. The Zr{sub 2}Fe bed absorbs the hydrogen isotopes from the flowing stream by forming a solid hydride compound. These beds contain 3 kilograms of Zr{sub 2}Fe and have been loaded routinely with 230-250 STP liters of hydrogen isotopes in earlier trials. The Zr-Mn-Fe alloy exhibits an anomaly during activation, namely an exotherm upon initial exposure to nitrogen. The purpose of this work is to better understand this reaction. Nitrogen absorption studies were done in order to quantify the nitrogen taken up by the getter and to characterize the reaction kinetics. In addition, ST909 phases before and after the reaction were studied with x-ray diffraction.

  14. Separation techniques for the clean-up of radioactive mixed waste for ICP-AES/ICP-MS analysis

    SciTech Connect

    Swafford, A.M.; Keller, J.M.

    1993-03-17

    Two separation techniques were investigated for the clean-up of typical radioactive mixed waste samples requiring elemental analysis by Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) or Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). These measurements frequently involve regulatory or compliance criteria which include the determination of elements on the EPA Target Analyte List (TAL). These samples usually consist of both an aqueous phase and a solid phase which is mostly an inorganic sludge. Frequently, samples taken from the waste tanks contain high levels of uranium and thorium which can cause spectral interferences in ICP-AES or ICP-MS analysis. The removal of these interferences is necessary to determine the presence of the EPA TAL elements in the sample. Two clean-up methods were studied on simulated aqueous waste samples containing the EPA TAL elements. The first method studied was a classical procedure based upon liquid-liquid extraction using tri-n- octylphosphine oxide (TOPO) dissolved in cyclohexane. The second method investigated was based on more recently developed techniques using extraction chromatography; specifically the use of a commercially available Eichrom TRU[center dot]Spec[trademark] column. Literature on these two methods indicates the efficient removal of uranium and thorium from properly prepared samples and provides considerable qualitative information on the extraction behavior of many other elements. However, there is a lack of quantitative data on the extraction behavior of elements on the EPA Target Analyte List. Experimental studies on these two methods consisted of determining whether any of the analytes were extracted by these methods and the recoveries obtained. Both methods produced similar results; the EPA target analytes were only slightly or not extracted. Advantages and disadvantages of each method were evaluated and found to be comparable.

  15. Application of zirconium dioxide nanoparticle sorbent for the clean-up step in post-harvest pesticide residue analysis.

    PubMed

    Uclés, Ana; Herrera López, Sonia; Dolores Hernando, Maria; Rosal, Roberto; Ferrer, Carmen; Fernández-Alba, Amadeo R

    2015-11-01

    The use of yttria-stabilized zirconium dioxide nanoparticles as d-SPE clean-up sorbent for a rapid and sensitive liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) method for the determination of post-harvest fungicides (carbaryl, carbendazim, chlorpropham, diphenylamine, ethoxyquin, flutriafol, imazalil, iprodione, methomyl, myclobutanil, pirimiphos-methyl, prochloraz, pyrimethanil, thiabendazole, thiophanate-methyl and tolclofos-methyl) in orange and pear samples has been evaluated and validated. The sample preparation was a modification of the QuEChERS extraction method using yttria-stabilized zirconium dioxide and multi-walled carbon nanotubes (MWCNTs) nanoparticles as the solid phase extraction (d-SPE) clean-up sorbents prior to injecting the ten-fold diluted extracts into the LC system. By using the yttria-stabilized zirconium dioxide extraction method, more recoveries in the 70-120% range were obtained - thus this method was used for the validation. Quantification was carried out using a matrix-matched calibration curve which was linear in the 1-500 µg kg(-1) range for almost all the pesticides studied. The validated limit of quantification was 10 µg kg(-1) for most of the studied compounds, except chlorpropham, ethoxyquin and thiophanate-methyl. Pesticide recoveries at the 10 and 100 µg kg(-1) concentration levels were satisfactory, with values between 77% and 120% and relative standard deviations (RSD) lower than 10% (n=5). The developed method was applied for the determination of selected fungicides in 20 real orange and pear samples. Four different pesticide residues were detected in 10 of these commodities; 20% of the samples contained pesticide residues at a quantifiable level (equal to or above the LOQs) for at least one pesticide residue. The most frequently-detected pesticide residues were: carbendazim, thiabendazole and imazalil-all were below the MRL. The highest concentration found was imazalil at 1175 µg kg

  16. Effective clean-up and ultra high-performance liquid chromatography-tandem mass spectrometry for isoflavone determination in legumes.

    PubMed

    Vila-Donat, Pilar; Caprioli, Giovanni; Maggi, Filippo; Ricciutelli, Massimo; Torregiani, Elisabetta; Vittori, Sauro; Sagratini, Gianni

    2015-05-01

    Legumes are an excellent source of macronutrients and phytochemicals as isoflavones. The aim of this work was to develop a new analytical method for determining five isoflavone compounds, three of which are aglycons, namely daidzein, genistein, biochanin A, and two of which, daidzin and genistin, are glycosilated, in lentils and other pulses, using an effective clean-up system and UHPLC-MS/MS (triple quadrupole) method. The recoveries obtained by spiking the lentil samples with a standard mixture of isoflavones at three levels of fortification (5, 25 and 100 μg kg(-1)) were in the range of 54.4-111.1%, 68.6-91.1%, and 84.4-114%, respectively. The method was applied to analyse 48 lentil samples from central Italy and pulses for determining the isoflavone content, which was found to range from 1.1 to 95.6 μg kg(-1).

  17. 21 CFR 71.4 - Samples; additional information.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 1 2013-04-01 2013-04-01 false Samples; additional information. 71.4 Section 71.4 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES GENERAL COLOR... samples of the color additive, articles used as components thereof, or of the food, drug, or cosmetic...

  18. 21 CFR 71.4 - Samples; additional information.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 1 2012-04-01 2012-04-01 false Samples; additional information. 71.4 Section 71.4 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES GENERAL COLOR... samples of the color additive, articles used as components thereof, or of the food, drug, or cosmetic...

  19. From conceptual model to remediation: bioavailability, a key to clean up heavy metal contaminated soils.

    NASA Astrophysics Data System (ADS)

    Petruzzelli, Gianniantonio; Pedron, Francesca; Pezzarossa, Beatrice

    2013-04-01

    Processes of metal bioavailability in the soil To know the bioavailability processes at site specific levels is essential to understand in detail the risks associated with pollution, and to support the decision-making process, i.e. description of the conceptual model and choice of clean up technologies. It is particularly important to assess how chemical, physical and biological processes in the soil affect the reactions leading to adsorption, precipitation or release of contaminants. The measurement of bioavailability One of the main difficulties in the practical application of the bioavailability concept in soil remediation is the lack of consensus on the method to be used to measure bioavailability. The best strategy is to apply a series of tests to assess bioavailability, since no applicable method is universally valid under all conditions. As an example, bioavailability tests for phytotechnology application should consider two distinct aspects: a physico-chemical driven solubilization process and a physiologically driven uptake process. Soil and plant characteristics strongly influence bioavailability. Bioavailability as a tool in remediation strategies Bioavailability can be used at all stages in remediation strategies: development of the conceptual model, evaluation of risk assessment, and selection of the best technology, considering different scenarios and including different environmental objectives. Two different strategies can be followed: the reduction and the increase of bioavailability. Procedures that reduce bioavailability aim to prevent the movement of pollutants from the soil to the living organisms, essentially by: i) removal of the labile phase of the contaminant, i.e. the fraction which is intrinsic to the processes of bioavailability (phytostabilization); ii) conversion of the labile fraction into a stable fraction (precipitation or adsorption); iii) increase of the resistance to mass transfer of the contaminants (inertization). Procedures

  20. Sectored Clean-up Work Plan for Housekeeping Category Waste Sites

    SciTech Connect

    S. J. Nacht

    2000-02-01

    The Sectored Clean-up Work Plan (SCWP) replaces the Housekeeping Category Corrective Action Unit Work Plan and provides a strategy to be used for conducting housekeeping activities using a sectored clean-up approach. This work plan provides a process by which one or more existing housekeeping category Corrective Action Sites (CASS) from the Federal Facility Agreement and Consent Order and/or non-FFACO designated waste site(s) are grouped into a sector for simultaneous remediation and cleanup. This increases effectiveness and efficiencies in labor, materials, equipment, cost, and time. This plan is an effort by the U.S. Department of Energy to expedite work in a more organized and efficient approach. The objectives of this plan are to: Group housekeeping FFACO CASS and non-FFACO housekeeping sites into sectors and remediate during the same field visit; Provide consistent documentation on FFACO CAS and non-FFACO clean-up activities; Perform similar activities under one approved document; Remediate areas inside the Deactivation and Decommissioning facilities and compounds in a campaign-style remediation; and Increase efficiencies and cost-effectiveness, accelerate cleanups, reduce mobilization, demobilization, and remediation costs.

  1. On-line detection of metal pollutant spikes in MSW incinerator flue gases prior to clean-up

    SciTech Connect

    Poole, D. Sharifi, V.; Swithenbank, J.; Argent, B.; Ardelt, D.

    2007-07-01

    SUWIC's unique mobile metals emissions monitoring laboratory has been used to measure metal pollutant spikes in the flue gas from a municipal solid waste incinerator, prior to gas clean-up. The laboratory has a heated sampling probe that extends into the plant, allowing the simultaneous on-line measurement of the concentrations of more than 30 metals by Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). As little is known about temporal variation in metal concentrations, this capability is seen as a major advance. The graphs of continuous measurements show that the elemental loading is far from uniform, and that concentrations fluctuate far more than may have been conventionally expected. There are occasional significant spikes in the emission profiles for cadmium and mercury, which are believed to be due to specific items in the waste feed material. Continuous monitoring measurements are of significant value for those seeking to model metal behaviour in combustion and in pollution control devices.

  2. UTILIZING INNOVATIVE TECHNOLOGIES FOR ENVIRONMENTAL CLEAN-UP, SAVAHHAH RIVER SITE

    SciTech Connect

    Bergren, C

    2009-01-07

    The Savannah River Site (SRS) is a 310-square-mile United States Department of Energy nuclear facility located along the Savannah River near Aiken, South Carolina. During operations, which started in 1951, hazardous substances (chemicals and radionuclides) were released to the environment. The releases occurred as a result of inadvertent spills and waste disposal in unlined pits and basins which was common practice before environmental regulations existed. The hazardous substances have migrated to the vadose zone and groundwater in many areas of the SRS, resulting in 515 waste units and facilities that are required by environmental regulations, to undergo characterization and, if needed, remediation. In the initial years of the SRS environmental cleanup program (early 1990s), the focus was to use common technologies (such as pump and treat, air stripping, excavation and removal) that actively and tangibly removed contamination. Exclusive use of these technologies required continued and significant funding while often failing to meet acceptable clean-up goals and objectives. Recognizing that a more cost-effective approach was needed, SRS implemented new and complementary remediation methods focused on active and passive technologies targeted to solve specific remediation problems. Today, SRS uses technologies such as chemical/pH-adjusting injection, phytoremediation, underground cutoff walls, dynamic underground stripping, soil fracturing, microbial degradation, baroballs, electrical resistance heating, soil vapor extraction, and microblowers to more effectively treat contamination at lower costs. Additionally, SRS's remediation approach cost effectively maximizes cleanup as SRS works proactively with multiple regulatory agencies. Using GIS, video, animation, and graphics, SRS is able to provide an accurate depiction of the evolution of SRS groundwater and vadose zone cleanup activities to convince stakeholders and regulators of the effectiveness of various cleanup

  3. Operating experience from the Tidd PFBC hot gas clean up program

    SciTech Connect

    Mudd, M.J.; Hoffman, J.D.

    1995-12-31

    The Tidd PFBC Hot Gas Clean Up (HGCU) test facility, a $22-million project sponsored by the US Department of Energy (DOE), has accumulated over 4700 hours of coal fire operation between October 1992 and October 1994. The HGCU slip stream, which represents a 10 MWt system, utilizes a Westinghouse candle-based system to filter ash from one-seventh of the exhaust gas of the 70 MWe Tidd PFBC Demonstration Plant. This paper presents a description of the system, reviews the results of all test runs conducted during 1994, and discusses the lessons learned from this project which may be applicable in the design of commercial hot gas filtration systems.

  4. Clean-up of a pesticide-lanolin mixture by gel permeation chromatography.

    PubMed

    López-Mesas, M; Crespi, M; Brach, J; Mullender, J P

    2000-12-01

    In this study, the efficiency of a clean-up method by gel permeation chromatography (GPC) for the separation of pesticides from lanolin is analyzed. The pesticides analyzed belong to two different families, organophosphorous and synthetic pyrethroids. Lanolin, a standard mixture of the pesticides, and a lanolin-pesticides mixture are injected in a GPC column. The recoveries and elution times from the GPC column of lanolin (by a gravimetric method) and pesticides (by gas chromatography-electron capture detector) are determined. From this column, a good separation of the lanolin-pesticides mixture is observed.

  5. Use of sediment serial dilution series to establish biological effect levels and clean-up goals

    SciTech Connect

    Timmer, E.; DeLong, T.; Millard, J.; Dobroski, C.

    1995-12-31

    A sediment serial dilution study was used to determine biological effect levels for two freshwater invertebrates, Chironomus tentans and Hyalella azteca. The sediments for the test were collected from a New England brook which contained elevated levels of lead and polychlorinated aromatic hydrocarbons. The objective of the sediment dilution study was two-fold: (1 ) to provide a site-specific estimation of biological effect levels, thus reducing uncertainties associated with using literature-based values, and (2) to establish clean-up goals specific to this freshwater system.

  6. Early Aging in Chernobyl Clean-Up Workers: Long-Term Study

    PubMed Central

    Krasnov, V.; Kryukov, V.; Samedova, E.; Emelianova, I.; Ryzhova, I.

    2015-01-01

    This paper represents data of long-term open prospective study. 312 male clean-up workers, who participated in elimination of the Chernobyl disaster consequences in 1986-87, were observed and examined in Moscow Research Institute of Psychiatry. The average age of patients was 57,0 ± 6,8 years. All patients were diagnosed with psychoorganic syndrome, caused by combination of different factors, which led to early cerebrovascular pathology, which was confirmed by clinical, neuropsychological, and instrumental examination. Anamnesis and the level of social adaptation were also assayed. Clinical estimation was done with the use of specially developed Clinical Psychopathological Chart. All the symptoms were divided into 4 groups (asthenic, psychovegetative, dysthymic, and cognitive symptom-complexes). No pronounced signs of dementia were observed. The control group included 44 clean-up workers without mental disorders. Predomination of various exogenous factors before and after accident was noted. Therapy included different vasotropic remedies, as well as family therapy, art therapy, and cognitive training. The possibilities of the reverse development of symptoms were statistically proved. The results allow making a conclusion that these disorders could not be explained either by radiation effects or by PTSD but connected with cerebrovascular pathology. PMID:25692150

  7. Dosimetry for a study of low-dose radiation cataracts among Chernobyl clean-up workers.

    PubMed

    Chumak, V V; Worgul, B V; Kundiyev, Y I; Sergiyenko, N M; Vitte, P M; Medvedovsky, C; Bakhanova, E V; Junk, A K; Kyrychenko, O Y; Musijachenko, N V; Sholom, S V; Shylo, S A; Vitte, O P; Xu, S; Xue, X; Shore, R E

    2007-05-01

    A cohort of 8,607 Ukrainian Chernobyl clean-up workers during 1986-1987 was formed to study cataract formation after ionizing radiation exposure. Study eligibility required the availability of sufficient exposure information to permit the reconstruction of doses to the lens of the eye. Eligible groups included civilian workers, such as those who built the "sarcophagus" over the reactor, Chernobyl Nuclear Power Plant Workers, and military reservists who were conscripted for clean-up work. Many of the official doses for workers were estimates, because only a minority wore radiation badges. For 106 military workers, electron paramagnetic resonance (EPR) measurements of extracted teeth were compared with the recorded doses as the basis to adjust the recorded gamma-ray doses and provide estimates of uncertainties. Beta-particle doses to the lens were estimated with an algorithm devised to take into account the nature and location of Chernobyl work, time since the accident, and protective measures taken. A Monte Carlo routine generated 500 random estimates for each individual from the uncertainty distributions of the gamma-ray dose and of the ratio of beta-particle to gamma-ray doses. The geometric mean of the 500 combined beta-particle and gamma-ray dose estimates for each individual was used in the data analyses. The median estimated lens dose for the cohort was 123 mGy, while 4.4% received >500 mGy.

  8. Site-specific sediment clean-up objectives developed by the sediment quality triad

    SciTech Connect

    Redman, S.; Janisch, T.

    1995-12-31

    Sediment chemistry, sediment toxicity, and benthic macroinvertebrate community data were collected and evaluated in concert (1) to characterize adverse effects of hydrocarbon and metal contaminants in the sediments of a small inlet of Superior Bay, Lake Superior and a tributary creek and (2) to derive numeric objectives for the clean up of this system. Sediments from reference locations and eight study sites were analyzed for a range of contaminants, including hydrocarbons (measured both as diesel range organics (DRO) and oil and grease), lead, chromium, and ammonia. A range of sediment toxicity was observed across the eight study sites using a variety of tests and endpoints: Hyalella azteca (10 day survival and growth), Chironomus tentans (10 day survival and growth), Ceriodaphnia dubia (48 hour survival), and Daphnia magna (48 hour survival and 10 day survival and reproduction). A range of alterations of the benthic macroinvertebrate community compared with communities from reference locations were observed. Benthic community alterations were summarized quantitatively by taxa richness and Shannon-Weiner mean diversity. Lowest effect levels determined through this study included 150 {micro}g/g dry sediment for DRO (as measured in this study) and 40 {micro}g/g dry sediment for lead. Effects thresholds determined through this study included 1,500 {micro}g/g dry sediment for DRO and 90 {micro}g/g dry sediment for lead. These levels and concentrations measured in relevant reference locations are being used to define objectives for sediment clean up in the inlet and creek.

  9. EPA Awards $10.3 Million to Clean Up New England Brownfield Sites, Protect Health in Communities

    EPA Pesticide Factsheets

    EPA has awarded more than $10.3 million in Brownfield grants to municipalities and organizations working to protect people's health by assessing and cleaning up contaminated parcels in New England communities.

  10. Treasure Coast Regional Planning Council to Receives $300,000 to Clean up and Redevelop Contaminated Brownfields Sites

    EPA Pesticide Factsheets

    ATLANTA - Today the U.S. Environmental Protection Agency (EPA) announced that the Treasure Coast Regional Planning Council will receive $300,000 to clean up and redevelop contaminated brownfields sites in Florida. Nationally, approximat

  11. EPA Announces $300,000 in Supplemental Funds to Clean up Contaminated Brownfields Sites in South Carolina

    EPA Pesticide Factsheets

    ATLANTA - Today the U.S. Environmental Protection Agency (EPA) announced $300,000 in supplemental funding to help transform communities in South Carolina by cleaning up contaminated Brownfields properties.

  12. EPA Announces $13.2 Million in Supplemental Funds to Clean up Contaminated Brownfields Sites Across the Country

    EPA Pesticide Factsheets

    WASHINGTON - Today the U.S. Environmental Protection Agency (EPA) announced approximately $13.2 million in supplemental funding to help transform communities by cleaning up contaminated Brownfields properties. Supplemental funding of the Revolving L

  13. Hazardous Waste Clean-Up Information (CLU-IN) On-line Characterization and Remediation Databases Fact Sheet

    EPA Pesticide Factsheets

    This fact sheet provides an overview of the 10 on-line characterization and remediation databases available on the Hazardous Waste Clean-Up Information (CLU-IN) website sponsored by the U.S. Environmental Protection Agency.

  14. Estimation of the uncertainties of extraction and clean-up steps in pesticide residue analysis of plant commodities.

    PubMed

    Omeroglu, P Yolci; Ambrus, A; Boyacioglu, D

    2013-01-01

    Extraction and clean-up constitute important steps in pesticide residue analysis. For the correct interpretation of analytical results, uncertainties of extraction and clean-up steps should be taken into account when the combined uncertainty of the analytical result is estimated. In the scope of this study, uncertainties of extraction and clean-up steps were investigated by spiking (14)C-labelled chlorpyrifos to analytical portions of tomato, orange, apple, green bean, cucumber, jackfruit, papaya and starfruit. After each step, replicate measurements were carried out with a liquid scintillation counter. Uncertainties in extraction and clean-up steps were estimated separately for every matrix and method combination by using within-laboratory reproducibility standard deviation and were characterised with the CV of recoveries. It was observed that the uncertainty of the ethyl acetate extraction step varied between 0.8% and 5.9%. The relative standard uncertainty of the clean-up step with dispersive SPE used in the method known as QuEChERS was estimated to be around 1.5% for tomato, apple and green beans. The highest variation of 4.8% was observed in cucumber. The uncertainty of the clean-up step with gel permeation chromatography ranged between 5.3% and 13.1%, and it was relatively higher than that obtained with the dispersive SPE method.

  15. Case study: Using microbe molecular biology for Gulf oil spill clean up.

    PubMed

    Jones, Daniel R

    2011-01-01

    This case has the student actively investigate the regulation of expression of a novel bacterial gene in the context of attempts to solve a real world problem, clean up of the April 2010 Deep Water Horizon oil spill in the Gulf of Mexico. Although the case is fictitious, it is based on factual gene regulatory characteristics of oil-degrading microbes. The case is written for a sophomore Cell Biology lecture course at Indiana Wesleyan University that is taught to Biology/Pre-Med majors. This study is also appropriate for use in undergraduate microbiology, biochemistry, molecular biology, and molecular genetics courses. The case is intended to enhance coverage of transcription, translation, control of gene expression, and selected molecular biology techniques. Opportunities to practice critical thinking skills and to a lesser extent an introduction to the paradigm of life science research at the industry level are provided.

  16. Improved exposure estimation in soil screening and clean-up criteria for volatile organic chemicals.

    PubMed

    DeVaull, George E

    2017-02-18

    Soil clean-up criteria define acceptable concentrations of organic chemical constituents for exposed humans. These criteria sum the estimated soil exposure over multiple pathways. Assumptions for ingestion, dermal contact, and dust exposure generally presume a chemical persists in surface soils at a constant concentration level for the entire exposure duration. For volatile chemicals this is an unrealistic assumption. A calculation method is presented for surficial soil criteria which include volatile depletion of chemical for these uptake pathways. The depletion estimates compare favorably with measured concentration profiles and with field measurements of soil concentration. Corresponding volatilization estimates compare favorably with measured data for a wide range of volatile and semi-volatile chemicals, including instances with and without the presence of a mixed-chemical residual phase. Selected examples show application of the revised factors in estimating screening levels for benzene in surficial soils. This article is protected by copyright. All rights reserved.

  17. An effective clean-up technique for GC/EI-HRMS determination of developmental neurotoxicants in human breast milk.

    PubMed

    Čechová, Eliška; Seifertová, Marta; Kukučka, Petr; Vojta, Šimon; Quaak, Ilona; de Cock, Marijke; van de Bor, Margot; Kočan, Anton

    2017-02-01

    The increasing number of children suffering from developmental disorders has raised questions regarding their association with the presence of environmental contaminants in mothers and children. We therefore developed a new method for the determination of 78 proven and potential developmental neurotoxicants, including polychlorinated biphenyls, legacy pesticides, pyrethroids, and old and new halogenated flame retardants in breast milk. The essential part of sample preparation was dialysis as a non-destructive clean-up step which was newly used at 10 °C and showed more efficient lipid removal (up to 96%) than the conventional methods such as gel permeation chromatography or freezing-lipid filtration and thus ensured low limits of detection (LOD) by reducing the sample volume prior to injection. Next advantages were significant solvent reduction and no risk of sample cross-contamination. Gas chromatography coupled with high resolution mass spectrometry (GC-HRMS) was subsequently used for the separation and compound quantification. The method was validated using breast milk samples fortified with the analyzed compounds. Recoveries for most of the compounds ranged from 63 to 121% with a relative standard deviation of 2-25%, and LODs ranged between 0.001 and 0.87 ng g(-1) lipid weight. The method was applied to breast milk samples from a Dutch birth cohort where 35 out of the 78 compounds were quantified in more than 60% of the samples. For novel flame retardants, the method provides unique results regarding their occurrence in human matrices in Europe. Overall, the analysis of a complex mixture of developmental neurotoxicants could be useful for the assessment of the influence of the studied compounds to child health and development. Graphical abstract Flow diagram of the method and levels of the developmental neurotoxicants in Dutch human milk samples.

  18. Enamel Surface Roughness after Debonding of Orthodontic Brackets and Various Clean-Up Techniques

    PubMed Central

    Ahrari, Farzaneh; Akbari, Majid; Akbari, Javad; Dabiri, Ghahraman

    2013-01-01

    Objective: This study aimed to evaluate enamel roughness after adhesive removal using different burs and an Er:YAG laser. Materials and Methods: The buccal surfaces of forty human premolars were sealed by two layers of nail varnish, except for a circular area of 3 mm in diameter on the middle third. The enamel surfaces were initially subjected to profilometry analysis and four parameters of surface irregularity (Ra, Rq, Rt and Rz) were recorded. Following bracket bonding and debonding, adhesive remnants were removed by tungsten carbide burs in low- or high- speed handpieces (group 1 and 2, respectively), an ultrafine diamond bur (group 3) or an Er:YAG laser (250 mJ, long pulse, 4 Hz) (group 4), and surface roughness parameters were measured again. Then, the buccal surfaces were polished and the third profilometry measurements were performed. Results: The specimens that were cleaned with a low speed tungsten carbide bur showed no significant difference in surface irregularity between the different treatment stages (p>0.05). Surface roughness increased significantly after clean-up with the diamond bur and the Er:YAG laser (p<0.01). In comparison between groups, adhesive removal with tungsten carbide burs at slow- or high-speed handpieces produced the lowest, while enamel clean-up with the Er:YAG laser caused the highest values of roughness measurements (P<0.05). Conclusion: Under the study conditions, application of the ultrafine diamond bur or the Er:YAG laser caused irreversible enamel damage on tooth surface, and thus these methods could not be recommended for removing adhesive remnants after debonding of orthodontic brackets. PMID:23724206

  19. Extraction and clean-up methods for organochlorine pesticides determination in milk.

    PubMed

    Martins, Joana Gomes; Amaya Chávez, Araceli; Waliszewski, Stefan M; Colín Cruz, Arturo; García Fabila, María Magdalena

    2013-07-01

    Organochlorine pesticides (OCPs) can cause environmental damage and human health risks since they are lipophilic compounds with high resistance to degradation and long half-lives in humans. As most persistent OCPs have been banned years ago, it is expected to find these compounds at trace levels in environment. Therefore, increasingly sensitive and reliable analytical techniques are required to ensure effective monitoring of these compounds. The aim of this review is to discuss extraction and clean-up methods used to monitor OCP residues in milk, reported in the last 20 years. To carry out this review, an exhaustive bibliographic review was conducted. Despite the disadvantages of conventional extraction and clean-up methods, such as liquid-liquid, solid-phase or Soxhlet extractions, these procedures are still used due to their reliability. New extraction methods, like solid-phase microextraction, matrix solid-phase dispersion or QuEChERS, have not been thoroughly evaluated for OCP determination in milk. Almost all the methodologies analyzed in this review presented good performance characteristics according to the performance acceptability criteria set in SANCO's procedure. Comparison between limits of quantification (LOQ) and detection (LOD), for the reported methodologies, is not always possible due to the heterogeneity of the units. Thus, researchers should take into account an homogenization of LOD and LOQ units, according to the international regulations and MRLs established. Finally, more research is necessary to obtain the ideal methodology for OCPs determination in milk, which comprises the environmentally friendly characteristics of the new techniques and the reliability of the traditional methodologies.

  20. Studies of leukemia and thyroid disease among Chernobyl clean-up workers from the Baltics

    SciTech Connect

    Inskip, P.D.; Tekkel, M.; Rahu, M.

    1997-03-01

    Following the reactor accident at Chernobyl in late April of 1986, hundreds of thousands of men from throughout the former Soviet Union were sent to Chernobyl to entomb the damaged reactor, remove radioactive debris, and help decontaminate the local environment. They remained for an average of three months and were allowed to accumulate up to 25 cGy of radiation before being sent home. Doses for some workers may have exceeded the allowable limit. The experience of Chernobyl clean-up workers is potentially informative about cancer risk associated with protracted exposure to low levels of radiation. Cohorts of clean-up workers from the Baltic Republics were assembled for study, based on military records and other lists. The study population includes 4,833 men from Estonia 5,709 from Latvia and at least 5,446 from Lithuania, where a pilot study is underway. They are being monitored for cancer incidence through linkages with the corresponding national cancer registries. Biodosimetric assays, including fluorescent in situ hybridization (FISH) for chromosome translocation analysis and the glycophorin A (GPA) somatic cell mutation assay, are being used to supplement information about radiation doses from worker records and questionnaires. Thyroid screening examinations, including palpation, ultrasound and, selectively, fine-needle aspiration biopsies were performed on nearly 2,000 workers in the Estonian cohort (mean age, 40 y) during the spring of 1995, nine years after the reactor accident. The study is still in progress. Work began first in Estonia, and results presented here pertain to this subgroup except as otherwise noted. The average age at the time of arrival at Chernobyl was 31 years. 62% were sent in 1986. Possible reasons for the apparent absence or rarity of radiation-induced thyroid nodules include low and protracted doses, low susceptibility among men exposed as adults, and insufficient passage of time since the accident.

  1. Quantifying the clean-up of LNAPL lens and LNAPL entrapped in an aquifer composed of fractured permeable formation

    NASA Astrophysics Data System (ADS)

    Rubin, H.; Koengeter, J.

    2006-12-01

    This study has originated and motivated by a case history of a comparatively wide scale of kerosene (LNAPL) contamination in an aquifer composed of a fractured permeable formation. Presently, parts of the LNAPL are entrapped within the top layers of the aquifer, and other parts are incorporated with LNAPL lens on top of the flowing groundwater. The study develops conceptual, mathematical and numerical models for simulating the aquifer and LNAPL lens clean-up by a pump-and-treat procedure. The numerical simulations identify the importance of mechanisms of dissolution of the entrapped LNAPL ganglia and the LNAPL lens by films of contact. Clean-up of the LNAPL lens is also affected by mixing in fracture intersections located at the interface LNAPL-groundwater. Dimensionless parameters governing all involved processes are identified and their effects in different ranges are quantified. The clean-up of the LNAPL lens is mainly affected by the mobility number and the fracture segment orientation. These parameters also determine the depth of penetration of the organic solutes into the aquifer. Clean-up of the entrapped LNAPL is mainly affected by the dimensionless interphase mass transfer coefficient. The simulations indicate that at low mobility numbers rates of LNAPL lens clean-up may be faster or slower than clean-up of the LNAPL entrapped within the top layers of the aquifer, depending on the value of the interphase mass transfer coefficient. At high mobility numbers the clean- up rates of the LNAPL lens are always slower than those of the LNAPL entrapped within the top layers of the aquifer.

  2. Clean-up of triazines in vegetable extracts by molecularly-imprinted solid-phase extraction using a propazine-imprinted polymer.

    PubMed

    Cacho, C; Turiel, E; Martín-Esteban, A; Pérez-Conde, C; Cámara, C

    2003-06-01

    An analytical methodology based on a molecularly imprinted solid-phase extraction (MISPE) procedure was developed for the determination of several triazines (atrazine, simazine, desethylatrazine (DEA), desisopropylatrazine (DIA), and propazine) in vegetable samples. A methacrylic acid-based imprinted polymer was prepared by precipitation polymerisation using propazine as template and toluene as porogen. After removal of the template by Soxhlet extraction, the optimum loading, washing, and elution conditions for MISPE of the selected triazines were established. The optimised MISPE procedure was applied to the extraction of the selected triazines in pea, potato, and corn sample extracts and a high degree of clean-up was obtained. However, some remaining interferences, non-specifically and strongly bound to the polymeric matrix, appeared in the chromatogram, preventing quantification of DIA in potatoes and DIA, DEA, and propazine in corn samples. Thus, a new clean-up protocol based on the use of a non-imprinted polymer for removal of these interferences prior to the MISPE step was developed. By following the new two-step MISPE procedure, the matrix compounds were almost completely removed, allowing the determination of all the triazines selected at concentration levels below the established maximum residue limits, making the developed procedure suitable for monitoring these analytes in vegetable samples.

  3. Additional sampling directions improve detection range of wireless radiofrequency probes

    PubMed Central

    Mada, Marius; Carpenter, T. Adrian; Sawiak, Stephen J.; Williams, Guy B.

    2015-01-01

    Purpose While MRI is enhancing our knowledge about the structure and function of the human brain, subject motion remains a problem in many clinical applications. Recently, the use of wireless radiofrequency markers with three one‐dimensional (1D) navigators for prospective correction was demonstrated. This method is restricted in the range of motion that can be corrected, however, because of limited information in the 1D readouts. Methods Here, the limitation of techniques for disambiguating marker locations was investigated. It was shown that including more sampling directions extends the tracking range for head rotations. The efficiency of trading readout resolution for speed was explored. Results Tracking of head rotations was demonstrated from −19.2 to 34.4°, −2.7 to 10.0°, and −60.9 to 70.9° in the x‐, y‐, and z‐directions, respectively. In the presence of excessive head motion, the deviation of marker estimates from SPM8 was reduced by 17.1% over existing three‐projection methods. This was achieved by using an additional seven directions, extending the time needed for readouts by a factor of 3.3. Much of this increase may be circumvented by reducing resolution, without compromising accuracy. Conclusion Including additional sampling directions extends the range in which markers can be used, for patients who move a lot. Magn Reson Med 76:913–918, 2016. © 2015 The Authors. Magnetic Resonance in Medicine published by Wiley Periodicals, Inc. on behalf of International Society for Magnetic Resonance in Medicine. This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited. PMID:26418189

  4. Hanford tank clean up: A guide to understanding the technical issues

    SciTech Connect

    Gephart, R.E.; Lundgren, R.E.

    1995-12-31

    One of the most difficult technical challenges in cleaning up the US Department of Energy`s (DOE) Hanford Site in southeast Washington State will be to process the radioactive and chemically complex waste found in the Site`s 177 underground storage tanks. Solid, liquid, and sludge-like wastes are contained in 149 single- and 28 double-shelled steel tanks. These wastes contain about one half of the curies of radioactivity and mass of hazardous chemicals found on the Hanford Site. Therefore, Hanford cleanup means tank cleanup. Safely removing the waste from the tanks, separating radioactive elements from inert chemicals, and creating a final waste form for disposal will require the use of our nation`s best available technology coupled with scientific advances, and an extraordinary commitment by all involved. The purpose of this guide is to inform the reader about critical issues facing tank cleanup. It is written as an information resource for the general reader as well as the technically trained person wanting to gain a basic understanding about the waste in Hanford`s tanks -- how the waste was created, what is in the waste, how it is stored, and what are the key technical issues facing tank cleanup. Access to information is key to better understanding the issues and more knowledgeably participating in cleanup decisions. This guide provides such information without promoting a given cleanup approach or technology use.

  5. Design of a second generation secondary enclosure clean-up system

    SciTech Connect

    Heics, A.G.; Shmayda, W.T.

    1995-10-01

    An upgraded version of a metal hydride based clean-up system for tritium gloveboxes has been recently designed. An earlier version of a prototypical, recirculating system has been under evaluation in tritium service at OHT for nearly 2 years. A metal getter alloy, Zr{sub 2}Fe, is used to remove tritium and trace impurities from inert and nitrogen glovebox cover gas. The second generation SEC system features several notable improvements over its predecessor in areas of gas conductance, process instrumentation for tritium and moisture detection, and operator interface. A second bed has been added to enhance the removal of tritium and impurities. The system is controlled by computer programmed to automatically maintain the glovebox pressure, temperature and the impurity level of the glovebox cover gas, and to respond effectively to upset conditions by corrective action and to alarm the off-normal condition. The lifetime of the metal alloy getter is affected by the presence of impurities, notably moisture, which dictates the need to ensure system leak tightness. For example, the tritium concentration at the bed outlet will rise by approximately one order of magnitude as a result of introducing a continuous moisture load of 5 ppmv for 6 months while maintaining a flow rate of 2 L/s. The second generation system will be commissioned with tritium during 1995. 9 refs., 3 figs.

  6. Determination of pesticides in fatty matrices using gel permeation clean-up followed by GC-MS/MS and LC-MS/MS analysis: A comparison of low- and high-pressure gel permeation columns.

    PubMed

    David, Frank; Devos, Christophe; Dumont, Emmie; Yang, Zhen; Sandra, Pat; Huertas-Pérez, José Fernando

    2017-04-01

    Two low-pressure columns (Bio-Beads SX-3) and three high-pressure GPC columns were compared for clean-up of a wide range of pesticides in fatty matrices of vegetable or animal origin. The GPC fractions were analyzed by GC-MS/MS and LC-MS/MS without additional clean-up. The performance of the GPC clean-up on the five column types was compared in terms of solvent consumption, lipid removal, pesticide recovery and repeatability. It was found that for fatty matrices, mainly consisting of high molecular weight triglycerides i.e. most vegetable oils and animal fats, good fractionation is obtained for the majority of the pesticides. On the other hand, for fats and oils containing relatively high amounts of low molecular weight triglycerides, i.e. butter fat and palm kernel oil, none of the columns provided sufficient clean-up and cause interferences and system contamination, especially in the case of GC-MS/MS analysis. For the latter case, best results in terms of lipid removal and pesticide recovery were obtained on a set (2×300mmlength) of narrow bore (7.5mm ID) columns packed with 5µm PL Gel material. Column loadability is, however, much lower on that set of columns compared the other evaluated GPC columns, impairing overall method sensitivity.

  7. Young Children's Views Concerning Distribution of Clean-Up Duties in the Classroom: Responsibility and Self-Interest

    ERIC Educational Resources Information Center

    Penderi, Efthymia; Rekalidou, Galini

    2016-01-01

    The preschool setting offers many opportunities to promote development of responsibility in young children. Clean-up routines may support children's distributional judgments, and reveal their sense of responsibility about classroom duties. Although there is a large number of studies regarding children's views about resource distribution,…

  8. CSX Agrees to EPA Order for Clean-up of Areas Impacted by West Virginia Train Derailment

    EPA Pesticide Factsheets

    PHILADELPHIA (March 6, 2015 ) - CSX Transportation Inc. (CSX) has agreed with the U.S. Environmental Protection Agency to clean up and restore the areas affected by the Feb. 16 train derailment in Mount Carbon, W. Va. Twenty-seven cars derailed from

  9. EPA provides $200K to Kiowa County to clean up and revitalize abandoned property in downtown Eads, Colorado

    EPA Pesticide Factsheets

    (Denver, Colo. - May 28, 2015) The U.S. Environmental Protection Agency (EPA) has awarded Kiowa County $200K in Brownfields grant funding to clean up, demolish and redevelop a blighted former motel and residence at 1209 Maine Street in downtown Eads,

  10. Innovative integration of decommissioning and deactivation program with soil-groundwater clean up program has positive results on budget and schedule: a case study

    SciTech Connect

    Schappell, Bruce G.; Rucker, Gregory G.

    2007-07-01

    An innovative approach to integrate the activities of a decommissioning and deactivation program (D and D) with a soil-groundwater clean up program has had significant positive results saving both money and time at the Department of Energy's Savannah River Site. The accomplishments that have been achieved by the combining the two programs have been remarkable including significant cost savings, economies of scale for sampling and document generation, and alignment of common objectives. Because of the coordination of both activities area-wide 'end states' can be formulated and be consistent with the customers' cleanup goals and federal regulations. This coordinates and aligns both the environmental clean up and D and D objectives because each must be addressed simultaneously and comprehensively. In this respect, resources from both organizations can be pooled to take advantage of the strengths of each. The new approach allows more efficient use of lean financial resources and optimizes workforce activities to attain the common objectives while being more cost effective, more protective of the environment, and optimizing the use existing resources. (authors)

  11. Innovative Integration of Decommissioning and Deactivation Program with Soil-Groundwater Clean Up Program Has Positive Results on Budget and Schedule: A Case Study

    SciTech Connect

    Schappell, B; Rucker, G

    2007-07-25

    An innovative approach to integrate the activities of a decommissioning and deactivation program (D&D) with a soil-groundwater clean up program has had significant positive results saving both money and time at the Department of Energy's Savannah River Site. The accomplishments that have been achieved by the combining the two programs have been remarkable including significant cost savings, economies of scale for sampling and document generation, and alignment of common objectives. Because of the coordination of both activities area-wide ''end states'' can be formulated and be consistent with the customers' cleanup goals and federal regulations. This coordinates and aligns both the environmental clean up and D&D objectives because each must be addressed simultaneously and comprehensively. In this respect, resources from both organizations can be pooled to take advantage of the strengths of each. The new approach allows more efficient use of lean financial resources and optimizes workforce activities to attain the common objectives while being more cost effective, more protective of the environment, and optimizing the use existing resources.

  12. Determination of fusarium mycotoxins in wheat, maize and animal feed using on-line clean-up with high resolution mass spectrometry.

    PubMed

    Ates, E; Mittendorf, K; Stroka, J; Senyuva, H

    2013-01-01

    An automated method involving on-line clean-up and analytical separation in a single run using TurboFlow™ reversed phase liquid chromatography coupled to a high resolution mass spectrometer has been developed for the simultaneous determination of deoxynivalenol, T2 toxin, HT2 toxin, zearalenone and fumonisins B1 and B2 in maize, wheat and animal feed. Detection was performed in full scan mode at a resolution of R = 100,000 full width at half maximum with high energy collision cell dissociation for the determination of fragment ions with a mass accuracy below 5 ppm. The extract from homogenised samples, after blending with a 0.1% aqueous mixture of 0.1% formic acid/acetonitrile (43:57) for 45 min, was injected directly onto the TurboFlow™ (TLX) column for automated on-line clean-up followed by analytical separation and accurate mass detection. The TurboFlow™ column enabled specific binding of target mycotoxins, whereas higher molecular weight compounds, like fats, proteins and other interferences with different chemical properties, were removed to waste. Single laboratory method validation was performed by spiking blank materials with mycotoxin standards. The recovery and repeatability was determined by spiking at three concentration levels (50, 100 and 200% of legislative limits) with six replicates. Average recovery, relative standard deviation and intermediate precision values were 71 to 120%, 1 to 19% and 4 to 19%, respectively. The method accuracy was confirmed with certified reference materials and participation in proficiency testing.

  13. Policies to clean up toxic industrial contaminated sites of Gela and Priolo: a cost-benefit analysis

    PubMed Central

    2011-01-01

    Background Cost-benefit analysis is a transparent tool to inform policy makers about the potential effect of regulatory interventions, nevertheless its use to evaluate clean-up interventions in polluted industrial sites is limited. The two industrial areas of Gela and Priolo in Italy were declared "at high risk of environmental crisis" in 1990. Since then little has been done to clean the polluted sites and reduce the health outcomes attributable to pollution exposure. This study, aims to quantify the monetary benefits resulting from clean-up interventions in the contaminated sites of Gela and Priolo. Methods A damage function approach was used to estimate the number of health outcomes attributable to industrial pollution exposure. Extensive one way analyses and probabilistic analyses were conducted to investigate the sensitivity of results to different model assumptions. Results It has been estimated that, on average, 47 cases of premature death, 281 cases of cancer and 2,702 cases of non-cancer hospital admission could be avoided each year by removing environmental exposure in these two areas. Assuming a 20 year cessation lag and a 4% discount rate we calculate that the potential monetary benefit of removing industrial pollution is €3,592 million in Priolo and €6,639 million in Gela. Conclusions Given the annual number of health outcomes attributable to pollution exposure the effective clean-up of Gela and Priolo should be prioritised. This study suggests that clean-up policies costing up to €6,639 million in Gela and €3,592 million in Priolo would be cost beneficial. These two amounts are notably higher than the funds allocated thus far to clean up the two sites, €127.4 million in Gela and €774.5 million in Priolo, implying that further economic investments - even considerable ones - could still prove cost beneficial. PMID:21797993

  14. Acetonitrile extraction and dual-layer solid phase extraction clean-up for pesticide residue analysis in propolis.

    PubMed

    Oellig, Claudia

    2016-05-06

    Propolis is a very complex mixture of substances that is produced by honey bees and is known to be a rather challenging matrix for residue analysis. Besides resins, flavonoids and phenols, high amount of wax is co-extracted resulting in immense matrix effects. Therefore a suitable clean-up is crucial and indispensable. In this study, a reliable solid phase extraction (SPE) clean-up was developed for pesticide residue analysis in propolis. The clean-up success was quickly and easily monitored by high-performance thin-layer chromatography with different detection possibilities. The final method consists of the extraction of propolis with acetonitrile according to the QuEChERS method followed by an effective extract purification on dual-layer SPE cartridges with spherical hydrophobic polystyrene-divinylbenzene resin/primary secondary amine as sorbent and a mixture of toluene/acetone (95:5, v/v) for elution. Besides fat-soluble components like waxes, flavonoids, and terpenoids, more polar compounds like organic acids, fatty acids, sugars and anthocyanins were also removed to large extent. Method performance was assessed by recovery experiments at spiking levels of 0.5 and 1mg/kg (n=5) for fourteen pesticides that are relevant for propolis. Mean recoveries determined by HPLC-MS against solvent standards were between 40 and 101%, while calculation against matrix-matched standards provided recoveries of 79-104%. Precision of recovery, assessed by relative standard deviations, were below 9%. Thus, the developed dual-layer SPE clean-up enables the reliable pesticide residue analysis in propolis and provides a suitable alternative to time-consuming clean-up procedures proposed in literature.

  15. Oak Ridge Cleanup Vision: Moving to the Future by Cleaning Up the Past - 13291

    SciTech Connect

    Cange, Susan M.; Wieland, Christopher C.; DePaoli, Susan M.

    2013-07-01

    received buy-in from the leadership in Headquarters, the regulators, and the community. Issues EM was facing in 2009 are presented. Resulting lessons learned and subsequent changes that the Office has gone through in the past several years in order to improve performance in the safe execution of work, relationships with external stakeholders, and communications both internally and externally are discussed. Results of these efforts are provided as a summary of Program accomplishments, including a strong focus on the future. EM's motto, Moving to the Future by Cleaning up the Past, will be demonstrated through the Program's mission, which includes protecting the region's health and environment; ensuring the continuation of ongoing vital missions being conducted by DOE on the Oak Ridge Reservation; and making clean land available for future use at all three sites, with a near-term focus on Re-industrialization of ETTP. (authors)

  16. Rapid determination of 88 veterinary drug residues in milk using automated TurborFlow online clean-up mode coupled to liquid chromatography-tandem mass spectrometry.

    PubMed

    Zhu, Wei-xia; Yang, Ji-zhou; Wang, Zhao-xing; Wang, Cai-juan; Liu, Ya-feng; Zhang, Li

    2016-02-01

    A novel method based on TurborFlow online solid phase extraction (SPE) combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been established for simultaneous screening and confirmation of 88 wide-range veterinary drugs belonging to eight families (20 sulfonamides, 7 macrolides, 15 quinolones, 8 penicillins, 13 benzimidazoles, 4 tetracyclines, 2 sedatives, and 19 hormones) in milk. The preparation method consists of sample dilution and ultrasonic extraction, followed by an automated turbulent flow cyclone chromatography sample clean-up system. The detection was achieved in selected reaction monitoring mode (SRM). The total run time was within 39 min, including automated extraction, analytical chromatography and re-equilibration of the turboflow system. The optimization of different experimental parameters including extraction, purification, separation, and detection were evaluated separately in this study. The developed method was validated and good performing characteristics were obtained. The linear regression coefficients (R(2)) of matrix-match calibration standard curves established for quantification were higher than 0.9930. The limits of detection (LOD) were in the range of 0.2-2.0 μg/kg given by signal-noise ratio ≥3 (S/N) and the limits of quantification (LOQ, S/N≥10) ranged between 0.5 μg/kg and 10 μg/kg. Average recoveries of spiked target compounds with different levels were between 63.1% and 117.4%, with percentage relative standard deviations (RSD) in the range of 3.3-17.6%. The results indicated that the developed method has great potential for the routine laboratory analysis of large numbers of samples on measuring different classes of compounds. In comparison to traditional procedures, the automated sample clean-up ensures rapid, effective, sensitive analyses of veterinary drugs in milk.

  17. 52 additional reference population samples for the 55 AISNP panel.

    PubMed

    Pakstis, Andrew J; Haigh, Eva; Cherni, Lotfi; ElGaaied, Amel Ben Ammar; Barton, Alison; Evsanaa, Baigalmaa; Togtokh, Ariunaa; Brissenden, Jane; Roscoe, Janet; Bulbul, Ozlem; Filoglu, Gonul; Gurkan, Cemal; Meiklejohn, Kelly A; Robertson, James M; Li, Cai-Xia; Wei, Yi-Liang; Li, Hui; Soundararajan, Usha; Rajeevan, Haseena; Kidd, Judith R; Kidd, Kenneth K

    2015-11-01

    Ancestry inference for a person using a panel of SNPs depends on the variation of frequencies of those SNPs around the world and the amount of reference data available for calculation/comparison. The Kidd Lab panel of 55 AISNPs has been incorporated in commercial kits by both Life Technologies and Illumina for massively parallel sequencing. Therefore, a larger set of reference populations will be useful for researchers using those kits. We have added reference population allele frequencies for 52 population samples to the 73 previously entered so that there are now allele frequencies publicly available in ALFRED and FROG-kb for a total of 125 population samples.

  18. Ultrasonic extraction followed by a novel filtration and clean-up device for screening of some polyphenols in tobaccos.

    PubMed

    Gu, Xungang; Cai, Jibao; Yang, Jun; Su, Qingde

    2005-02-01

    A simple and efficient HPLC method using a diode array detector (DAD) was developed for simultaneous determination of six polyphenols in tobaccos. Ultrasonic extraction was employed at 25 degrees C to extract the polyphenols present in tobaccos into anhydrous methanol. A novel filtration device linked to a clean-up cartridge was designed for simultaneous extract filtration and clean-up. Optimized HPLC-DAD analysis, with multi-wavelength detection, was used for determination of the polyphenols. Because the content of some of the polyphenols is too low to be quantified directly, a concentration step was necessary. Anhydrous methanol was employed for extraction of the polyphenols because of its high extraction efficiency and its low boiling point in the concentration step. Using the proposed method, six polyphenols were quantified in tobaccos (Nicotina tobaccum L.).

  19. Building upon Historical Competencies: Next-generation Clean-up Technologies for World-Wide Application - 13368

    SciTech Connect

    Guevara, K.C.; Fellinger, A.P.; Aylward, R.S.; Griffin, J.C.; Hyatt, J.E.; Bush, S.R.

    2013-07-01

    The Department of Energy's Savannah River Site has a 60-year history of successfully operating nuclear facilities and cleaning up the nuclear legacy of the Cold War era through the processing of radioactive and otherwise hazardous wastes, remediation of contaminated soil and groundwater, management of nuclear materials, and deactivation and decommissioning of excess facilities. SRS recently unveiled its Enterprise.SRS (E.SRS) strategic vision to identify and facilitate application of the historical competencies of the site to current and future national and global challenges. E.SRS initiatives such as the initiative to Develop and Demonstrate Next generation Clean-up Technologies seek timely and mutually beneficial engagements with entities around the country and the world. One such ongoing engagement is with government and industry in Japan in the recovery from the devastation of the Fukushima Daiichi Nuclear Power Station. (authors)

  20. Variable-Sweep Transition Flight Experiment (VSTFE): Stability code development and clean-up glove data analysis

    NASA Technical Reports Server (NTRS)

    Rozendaal, Roger A.

    1987-01-01

    The primary objective of the Variable Sweep Transition Flight Experiment (VSTFE) was to establish an improved swept wing transition criterion. The development of the Unified Stability System gave a way of quickly examining disturbance growth for a wide variety of laminar boundary layers. The disturbance growth traces shown are too scattered to define a transition criteria to replace the F-111 data band, which has been used successfully to design NLF gloves. Still, a careful review of the clean-up glove data may yield cases for which the transition location is known more accurately. Liquid crystal photographs of the clean-up glove show much spanwise variation in the transition front for some conditions, and this further complicates the analyses. Several high quality cases are needed in which the transition front is well defined and at a relatively constant chordwise station.

  1. Joule-heated graphene-wrapped sponge enables fast clean-up of viscous crude-oil spill.

    PubMed

    Ge, Jin; Shi, Lu-An; Wang, Yong-Chao; Zhao, Hao-Yu; Yao, Hong-Bin; Zhu, Yin-Bo; Zhang, Ye; Zhu, Hong-Wu; Wu, Heng-An; Yu, Shu-Hong

    2017-04-03

    The clean-up of viscous crude-oil spills is a global challenge. Hydrophobic and oleophilic oil sorbents have been demonstrated as promising candidates for oil-spill remediation. However, the sorption speeds of these oil sorbents for viscous crude oil are rather limited. Herein we report a Joule-heated graphene-wrapped sponge (GWS) to clean-up viscous crude oil at a high sorption speed. The Joule heat of the GWS reduced in situ the viscosity of the crude oil, which prominently increased the oil-diffusion coefficient in the pores of the GWS and thus speeded up the oil-sorption rate. The oil-sorption time was reduced by 94.6% compared with that of non-heated GWS. Besides, the oil-recovery speed was increased because of the viscosity decrease of crude oil. This in situ Joule self-heated sorbent design will promote the practical application of hydrophobic and oleophilic oil sorbents in the clean-up of viscous crude-oil spills.

  2. Novel fracture technology proves marginal Viking prospect economic, part II: Well clean-up, flowback and testing

    SciTech Connect

    Haidar, S.; Rylance, M.; Tybero, G.

    1996-12-31

    Having completed both fracture treatments as discussed in a companion paper, this paper continues on to describe the post fracture shut-in, clean-up and well testing operations that took place on the Viking Wx exploration well 49/17-12. These operations involved the removal of Resin Coated Proppant (RCP) from the wellbore, via Coiled Tubing (CT), through the use of a specially designed jetting nozzle. The RCP pack stability at a concentration of 3.0 lb/ft{sup 2} (as per planned design) had already been tested in a flowback cell. The use of a Surface Read-Out (SRO) gauge, combined with gas, water and proppant flow rates as well as the viscosity of fracturing fluids returns, enabled real time calculation of the drag forces, on the proppant pack, during clean-up. The flow rate, in the field, was controlled such that the calculated drag forces remained below those observed in the laboratory. Following the clean-up a flow and build-up test was conducted, to evaluate the fracture half length and fracture conductivity, from which a Pseudo-radial skin was calculated. The Non-Darcy effects in the fracture were also evaluated, and finally the short term and long term well deliverabilities were assessed.

  3. Determination of BPA, BPB, BPF, BADGE and BFDGE in canned energy drinks by molecularly imprinted polymer cleaning up and UPLC with fluorescence detection.

    PubMed

    Gallo, Pasquale; Di Marco Pisciottano, Ilaria; Esposito, Francesco; Fasano, Evelina; Scognamiglio, Gelsomina; Mita, Gustavo Damiano; Cirillo, Teresa

    2017-04-01

    A new method for simultaneous determination of five bisphenols in canned energy drinks by UPLC with fluorescence detection, after clean up on molecularly imprinted polymers, is herein described. The method was validated at two concentration levels, calculating trueness, repeatability and within-laboratory reproducibility, specificity, linearity of detector response, the limits of quantifications and the limits of detection for each bisphenol. The method is specific, reliable and very sensitive, allowing for determination of bisphenol F diglycidyl ether (BFDGE), bisphenol A (BPA), bisphenol B (BPB), bisphenol F (BPF) and bisphenol A diglycidyl ether (BADGE) down to 0.50ng/mL; it was employed to determine contamination levels from these bisphenols in forty energy drinks of different brands, collected from the market in Naples. BPA was detected in 17 out of 40 samples (42.5%); in some energy drinks also BPF, BADGE and BFDGE were determined.

  4. Cleaning up the biogeography of Labroides dimidiatus using phylogenetics and morphometrics

    NASA Astrophysics Data System (ADS)

    Sims, C. A.; Riginos, C.; Blomberg, S. P.; Huelsken, T.; Drew, J.; Grutter, A. S.

    2014-03-01

    Cleaner fishes are some of the most conspicuous organisms on coral reefs due to their behaviour and prominent body pattern, consisting of a lateral stripe and blue/yellow colouration. All obligate cleaner fishes share this body stripe pattern, which is an important signal for attracting client fishes. However, variability in the cleaning signal of the cleaner fish Labroides dimidiatus has been documented across its range. Here, we investigate the geographic distribution of cleaner signal polymorphisms in L. dimidiatus and contrast this to phylogeographic variation in mitochondrial (mt) DNA. We used samples from 12 sites for genetic analyses, encompassing much of L. dimidiatus' range from the Red Sea to Fiji. We obtained morphometric measures of the cleaner signal body stripe width from individuals among six of the sites and qualitatively grouped tail stripe shape. mtDNA control region sequences were used for phylogenetic and population genetic analyses. We found that body stripe width was significantly correlated with tail stripe shape and geographical location, with Indian Ocean populations differing in morphology from western Pacific populations. L. dimidiatus haplotypes formed two reciprocally monophyletic clades, although in contrast to morphology, Japanese cleaner fish fell within the same clade as Indian Ocean cleaner fish and both clade types were sympatric in Papua New Guinea. An additional novel finding of our research was that the inclusion of two closely related cleaner fish species, Labroides pectoralis and Labroides bicolor, in the phylogenetic analysis rendered L. dimidiatus polyphyletic. Overall, the findings suggest the diversity within L. dimidiatus is underestimated.

  5. Enrichment of perfluorinated alkyl substances on polyethersulfone using 1-methylpyperidine as ion-pair reagent for the clean-up of carrot and amended soil extracts.

    PubMed

    Bizkarguenaga, Ekhiñe; Zabaleta, Itsaso; Iparraguirre, Arantza; Aguirre, Josu; Fernández, Luis Ángel; Berger, Urs; Prieto, Ailette; Zuloaga, Olatz

    2015-10-01

    The development of a simple, cheap and environment friendly analytical method for the simultaneous determination of different perfluoroalkyl substances (PFASs) including seven perfluoroalkyl carboxylic acids, three perfluoroalkane sulfonic acids and perfluorooctanesulfonamide in carrot and amended soil was carried out in the present work. The method was based on focused ultrasound solid-liquid extraction followed by extract clean-up through enrichment of the target compounds on a polymeric material using an ion-pair reagent and detection by liquid chromatography-tandem mass spectrometry. The following variables affecting the clean-up step were evaluated: the nature of the polymeric material (polyethersulfone, PES, versus silicone rod), the amount of the polymeric material (from 1 to 9 mg), the ion-pair reagent (1-methylpyperidine, 1-MP, versus tetrabutylammonium salts), the concentration of the ion-pair reagent (from 5 to 50 mM) and the extraction time (from 15 min to 24 h). Optimum clean-up conditions were obtained using preconcentration on 9 mg of PES polymeric material combined with 5 mM 1-MP as ion-pair reagent for 3h. The method was validated in terms of apparent recoveries in the range of 77-140% and 95-137% at the low concentration (50 ng g(-1)) and in the range of 70-136% and 79-132% at the high concentration (290 ng g(-1)) for amended soil and carrot, respectively, after correction with the corresponding labeled standards. Precision, as relative standard deviation, was within 2-23%, while method detection limits were 0.31-2.85 ng g(-1) for amended soil and 0.11-1.83 ng g(-1) for carrot. In the absence of a certified reference material for the target analytes in the matrices studied, inter-method comparison was carried out and the same samples were processed using two independent clean-up procedures, the one developed in the present work and a classical based on solid-phase extraction. Statistically comparable results were obtained according to the one

  6. Heterocyclic amines in griddled beef steak analysed using a single extract clean-up procedure.

    PubMed

    Toribio, F; Busquets, R; Puignou, L; Galceran, M T

    2007-04-01

    Heterocyclic amines (HAs), which are potent mutagenic and carcinogenic substances, are formed in muscle meats during their cooking under ordinary conditions. In this work, we measured the concentration of 15 HAs in different samples of griddled beef steak, which is one of the most consumed meat items is Spain. Three samples were obtained from different restaurants, and the other sample was cooked under controlled conditions to a well-done degree of doneness. A low-time consuming solid-phase extraction procedure was used to purify the samples, and liquid chromatography-tandem mass spectrometry with an ion trap mass analyzer was used as determination technique. A second well-established purification procedure was used to demonstrate the applicability of the method to the analysis of these kind of samples. 8-MeIQx, 4,8-DiMeIQx, PhIP and the comutagens Harman and Norharman were found in all the samples, at levels ranging from 0.28 to 21.2ngg(-1). AalphaC was found in three samples (0.18-1.41ngg(-1)), whereas Trp-P-1 was detected in two samples (0.35ngg(-1)). MeAalphaC was found in three samples but could only be quantified in one (0.15ngg(-1)). Trp-P-2 and DMIP were also detected in some cases at levels below their limit of quantification. The remaining HAs analyzed were not detected in any of the samples.

  7. Absorbent pads for Containment, Neutralization, and Clean-Up of Environmental Spills Containing Chemically-Reactive Agents

    NASA Technical Reports Server (NTRS)

    Davis, Dennis D. (Inventor)

    1997-01-01

    A pad for cleaning up liquid spills is described which contains a porous surface covering, and an absorbent interior containing chemically reactive reagents for neutralizing noxious chemicals within the spilled liquid. The porous surface and the absorbent component would normally consist of chemically resistant materials allowing tentative spill to pass. The absorbent interior which contains the neutralizing reagents can but is not required to be chemically resilient and conducts the liquid chemical spill towards the absorbent interior containing the chemically reactive reagents where the dangerous and undesirable chemicals within the chemical spill are then neutralized as well as removed from the premises.

  8. Absorbent Pads for Containment, neutralization, and clean-up of environmental spills containing chemically-reactive agents

    NASA Technical Reports Server (NTRS)

    Davis, Dennis D. (Inventor)

    1996-01-01

    A pad for cleaning up liquid spills is described which contains a porous surface covering, and an absorbent interior containing chemically reactive reagents for neutralizing noxious chemicals within the spilled liquid. The porous surface and the absorbent component would normally consist of chemically resistant materials allowing tentative spill to pass. The absorbent interior which contains the neutralizing reagents can but is not required to be chemically resilient and conducts the liquid chemically reactive reagents where the dangerous and undesirable chemicals within the chemical spill are then neutralized as well as removed from the premises.

  9. The use of immunoaffinity columns connected in tandem for selective and cost-effective mycotoxin clean-up prior to multi-mycotoxin liquid chromatographic-tandem mass spectrometric analysis in food matrices.

    PubMed

    Wilcox, Joyce; Donnelly, Carol; Leeman, David; Marley, Elaine

    2015-06-26

    This paper describes the use of two immunoaffinity columns (IACs) coupled in tandem, providing selective clean-up, based on targeted mycotoxins known to co-occur in specific matrices. An IAC for aflatoxins+ochratoxin A+fumonisins (AOF) was combined with an IAC for deoxynivalenol+zearalenone+T-2/HT-2 toxins (DZT); an IAC for ochratoxin A (O) was combined with a DZT column; and an aflatoxin+ochratoxin (AO) column was combined with a DZT column. By combining pairs of columns it was demonstrated that specific clean-up can be achieved as required for different matrices. Samples of rye flour, maize, breakfast cereal and wholemeal bread were analysed for mycotoxins regulated in the EU, by spiking at levels close to EU limits for adult and infant foods. After IAC clean-up extracts were analysed by LC-MS/MS with quantification using multiple reaction monitoring. Recoveries were found to be in range from 60 to 108%, RSDs below 10% depending on the matrix and mycotoxin combination and LOQs ranged from 0.1n g/g for aflatoxin B1 to 13.0 ng/g for deoxynivalenol. Surplus cereal proficiency test materials (FAPAS(®)) were also analysed with found levels of mycotoxins falling within the satisfactory range of concentrations (Z score ≤ ± 2), demonstrating the accuracy of the proposed multi-mycotoxin IAC methods.

  10. Development of a simple extraction and clean-up procedure for determination of organochlorine pesticides in soil using gas chromatography-tandem mass spectrometry.

    PubMed

    Rashid, A; Nawaz, S; Barker, H; Ahmad, I; Ashraf, M

    2010-04-23

    A procedure based on QuEChERS extraction and a simultaneous liquid-liquid partition clean-up was developed. The procedure involved extraction of hydrated soil samples using acetonitrile and clean-up by liquid-liquid partition into n-hexane. The hexane extracts produced were clean and suitable for determination using gas chromatography-tandem mass spectrometry (GC-MS/MS). The method was validated by analysis of soil samples, spiked at five levels between 1 and 200 microg kg(-1). The recovery values were generally between 70 and 100% and the relative standard deviation values (%RSDs) were at or below 20%. The procedure was validated for determination of 19 organochlorine (OC) pesticides. These were hexachlorobenzene (HCB), alpha-HCH, beta-HCH, gamma-HCH, heptachlor, heptachlor epoxide (trans), aldrin, dieldrin, chlordane (trans), chlordane (cis), oxychlordane, alpha-endosulfan, beta-endosulfan, endosulfan sulfate, endrin, p,p'-DDT, o,p'-DDT, p,p'-DDD and p,p'-DDE. The method achieved low limits of detection (LOD; typically 0.3 microg kg(-1)) and low limits of quantification (LOQ; typically 1.0 microg kg(-1)). The method performance was also assessed using five fortified soil samples with different physico-chemical properties and the method performance was consistent for the different types of soil samples. The proposed method was compared with an established procedure based on Soxtec extraction. This comparison was carried out using six soil samples collected from regions of Pakistan with a history of intensive pesticide use. The results of this comparison showed that the two procedures produced results with good agreement. The proposed method produced cleaner extracts and therefore led to lower limits of quantification. The proposed method was less time consuming and safer to use. The six samples tested during this comparison showed that soils from cotton growing regions contained a number of persistent OC residues at relatively low levels (<10 microg kg(-1)). These

  11. Method of and apparatus for preheating pressurized fluidized bed combustor and clean-up subsystem of a gas turbine power plant

    DOEpatents

    Cole, Rossa W.; Zoll, August H.

    1982-01-01

    In a gas turbine power plant having a pressurized fluidized bed combustor, gas turbine-air compressor subsystem and a gas clean-up subsystem interconnected for fluid flow therethrough, a pipe communicating the outlet of the compressor of the gas turbine-air compressor subsystem with the interior of the pressurized fluidized bed combustor and the gas clean-up subsystem to provide for flow of compressed air, heated by the heat of compression, therethrough. The pressurized fluidized bed combustor and gas clean-up subsystem are vented to atmosphere so that the heated compressed air flows therethrough and loses heat to the interior of those components before passing to the atmosphere.

  12. SIMPLE SAMPLE CLEAN UP PROCEDURE AND HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD FOR THE ANALYSIS OF CYANURIC ACID IN HUMAN URINE

    EPA Science Inventory

    Cyanuric acide (CA) is widely used as a chlorine stabilizer in outdoor pools. No simple method exists for CA measurement in the urine of exposed swimmers. The high hydrophilicity of CA makes usage of solid phase sorbents to extract it from urine nearly impossible because of samp...

  13. SUPERCRITICAL FLUID EXTRACTION AND CLEAN-UP PROCEDURES FOR DETERMINATION OF XENOBIOTICS IN BIOLOGICAL SAMPLES. (R825549C011)

    EPA Science Inventory

    The perspectives, information and conclusions conveyed in research project abstracts, progress reports, final reports, journal abstracts and journal publications convey the viewpoints of the principal investigator and may not represent the views and policies of ORD and EPA. Concl...

  14. Molecularly imprinted polymer-based solid phase clean-up for analysis of ochratoxin A in beer, red wine, and grape juice.

    PubMed

    Cao, Jiliang; Kong, Weijun; Zhou, Shujun; Yin, Lihui; Wan, Li; Yang, Meihua

    2013-04-01

    A simple, reliable, and low-cost method based on molecularly imprinted polymer as a selective sorbent of SPE was proposed for the determination of ochratoxin A (OTA) in beer, red wine, and grape juice by HPLC coupled with fluorescence detection (HPLC-FLD). Samples were diluted with water and cleaned up with an AFFINIMIP® SPE OTA column. After washing and eluting, the analyte was analyzed by HPLC-FLD. Under the optimized conditions, LOD and LOQ for OTA were 0.025 and 0.08 ng/mL, respectively. The recoveries of OTA from beer, red wine, and grape spiked at 0.1, 2, and 5 ng/mL ranged from 91.6 to 101.7%. Furthermore, after a simple regenerated procedure, the molecularly imprinted polymer based SPE column could be reused at least 14 times to achieve more than 80% recoveries of OTA in real samples. The developed method was applied to the detection of 30 beer, red wine, and grape juice samples and only four samples were contaminated by OTA with levels below the legal limits.

  15. Recovery of salt marsh vegetation after removal of storm-deposited anthropogenic debris: Lessons from volunteer clean-up efforts in Long Beach, NY.

    PubMed

    Ehl, Kaitlin M; Raciti, Steve M; Williams, Jason D

    2017-02-14

    Recovery of vegetation on a Long Island, NY salt marsh was investigated after the removal of hurricane-deposited large wooden debris through managed clean-ups involving volunteers. Two years after the removal of the debris, vegetation cover and species composition were not significantly different from controls. There was no significant difference in vegetation recovery among fall and spring debris removal treatments. Initial vegetation cover of the experimental and control plots was 95.8% and 1.2%, respectively; after two growing seasons cover was 78.7% and 71.2%, respectively. The effects of trampling by volunteers during debris removal were monitored and after one growing season, trails used during a single clean-up effort had a mean vegetation cover of 67% whereas those that were used during multiple clean-up efforts had only 30% cover. We use the results of this study to offer guidance for organizing effective salt marsh clean-up efforts.

  16. Development of a bi-functional silica monolith for electro-osmotic pumping and DNA clean-up/extraction using gel-supported reagents in a microfluidic device.

    PubMed

    Oakley, Jennifer A; Shaw, Kirsty J; Docker, Peter T; Dyer, Charlotte E; Greenman, John; Greenway, Gillian M; Haswell, Stephen J

    2009-06-07

    A silica monolith used to support both electro-osmotic pumping (EOP) and the extraction/elution of DNA coupled with gel-supported reagents is described. The benefits of the combined EOP extraction/elution system were illustrated by combining DNA extraction and gene amplification using the polymerase chain reaction (PCR) process. All the reagents necessary for both processes were supported within pre-loaded gels that allow the reagents to be stored at 4 degrees C for up to four weeks in the microfluidic device. When carrying out an analysis the crude sample only needed to be hydrodynamically introduced into the device which was connected to an external computer controlled power supply via platinum wire electrodes. DNA was extracted with 65% efficiency after loading lysed cells onto a silica monolith. Ethanol contained within an agarose gel matrix was then used to wash unwanted debris away from the sample by EOP (100 V cm(-1) for 5 min). The retained DNA was subsequently eluted from the monolith by water contained in a second agarose gel, again by EOP using an electric field of 100 V cm(-1) for 5 min, and transferred into the PCR reagent containing gel. The eluted DNA in solution was successfully amplified by PCR, confirming that the concept of a complete self-contained microfluidic device could be realised for DNA sample clean up and amplification, using a simple pumping and on-chip reagent storage methodology.

  17. Concurrent extraction, clean-up, and analysis of polybrominated diphenyl ethers, hexabromocyclododecane isomers, and tetrabromobisphenol A in human milk and serum.

    PubMed

    Shi, Zhixiong; Wang, Yifei; Niu, Piye; Wang, Jiandi; Sun, Zhiwei; Zhang, Shuhua; Wu, Yongning

    2013-10-01

    A method has been developed and validated for the concurrent extraction, clean-up, and analysis of polybrominated diphenyl ethers (PBDEs), α-, β-, and γ-hexabromocyclododecane (HBCD), and tetrabromobisphenol A (TBBPA) in human milk and serum. Milk and serum samples were extracted using accelerated solvent extraction with acetone/hexane 1:1, v/v and liquid-liquid extraction with methyl-tert-butyl ether/hexane 1:1, v/v, respectively. The removal of co-extracted biogenic materials was achieved by gel permeation chromatography followed by sulfuric acid treatment. The fractionation of the PBDEs and HBCD/TBBPA was performed using a Supelco LC-Si SPE cartridge. The detection of the PBDEs was then performed by GC-MS and that of the HBCDs and the TBBPA was performed using UPLC-MS/MS. The pretreatment procedure was optimized, and the characteristic ions and fragmentation of the analytes were studied by MS or MS/MS. A recovery test was performed using a matrix spiking test at concentrations of 0.05-10 ng/g. The recoveries ranged from 78.6-108.8% with RSDs equal to or lower than 14.04%. The LODs were 1.8-60 pg/g. The usefulness of the developed method was tested by the analysis of real human samples, and several brominated flame retardants in different samples were detected and analyzed.

  18. In-cell clean-up pressurized liquid extraction and gas chromatography-tandem mass spectrometry determination of hydrophobic persistent and emerging organic pollutants in coastal sediments.

    PubMed

    Pintado-Herrera, Marina G; González-Mazo, Eduardo; Lara-Martín, Pablo A

    2016-01-15

    The main goal of this work was to develop, optimize and validate a multi-residue method for the simultaneous determination of 97 contaminants, including fragrances, UV filters, repellents, endocrine disruptors, biocides, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), organophosphorus flame retardants, and several types of pesticides in marine sediment samples. Extraction and cleanup were integrated into the same step using pressurized liquid extraction (PLE) with in-cell clean-up (1g of alumina). The extraction was performed using dichloromethane at 100 °C, 1500 psi and 3 extraction cycles (5 min per cycle). Extracts were derivatized with N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA) to improve the signal and sensitivity of some target compounds (i.e., triclosan, 2-hydroxybenzophenone). Separation, identification and quantification of analytes were carried out by gas chromatography (GC) coupled to tandem mass spectrometry. Under optimal conditions, the optimized protocol showed good recovery percentages (70-100%), linearity (>0.99) and limits of detection below 1 ng g(-1) for all compounds. Finally, the method was applied to the analysis of sediment samples from different coastal areas from Andalusia (Spain), where occurrence and distribution of emerging contaminants in sediments is very scarce. Twenty five compounds out of 98 were detected in all samples, with the endocrine disruptor nonylphenol and the fragrance galaxolide showing the highest concentrations, up to 377.6 ng g(-1) and 237.4 ng g(-1), respectively.

  19. Results of the clean-up operation to reduce pollution on flooded agricultural fields after the red mud spill in Hungary.

    PubMed

    Uzinger, Nikolett; Anton, Áron Dániel; Ötvös, Károly; Tamás, Péter; Anton, Attila

    2015-07-01

    In Hungary, the dam of a red mud reservoir breached shortly after noon on October 4, 2010. Approximately 0.7-1 million m(3) highly alkaline red mud with very low dry matter content flowed into the Torna Creek and the surrounding area, covering 1017 ha of agricultural land. Results of the risk assessment of the accident indicated that the red mud should be removed from the surface of fields where it formed a continuous layer of more than 5 cm. After the removal, samples were taken manually from depths of 0.0-0.2 m and 0.2-0.4 m in a sampling grid and background samples unaffected by red mud from the depth of 0.0-0.3 m. Total element contents (Ag, As, Ba, Cd, Co, Cr, Cu, Hg, Mo, Ni, Pb, Sn, Zn, and Na) and pH values were measured, and the results were analysed using correlation analysis and the Kruskal-Wallis probe. Dependence of the measured variables from elevation above sea level was studied using a 10 m by 10 m digital elevation model. Only ∼6.5% of the flooded area was temporarily designated as unsuitable for the production of food and fodder crops. In summary, the clean-up operation can be said to have been a success.

  20. Phytoextraction for clean-up of low-level uranium contaminated soil evaluated.

    PubMed

    Vandenhove, H; Van Hees, M

    2004-01-01

    Spills in the nuclear fuel cycle have led to soil contamination with uranium. In case of small contamination just above release levels, low-cost yet sufficiently efficient remedial measures are recommended. This study was executed to test if low-level U contaminated sandy soil from a nuclear fuel processing site could be phytoextracted in order to attain the required release limits. Two soils were tested: a control soil (317 Bq 238U kg(-1)) and the same soil washed with bicarbonate (69 Bq 238U kg(-1)). Ryegrass (Lolium perenne cv. Melvina) and Indian mustard (Brassica juncea cv. Vitasso) were used as test plants. The annual removal of soil activity by the biomass was less than 0.1%. The addition of citric acid (25 mmol kg(-1)) 1 week before the harvest increased U uptake up to 500-fold. With a ryegrass and mustard yield of 15,000 and 10,000 kg ha(-1), respectively, up to 3.5% and 4.6% of the soil activity could be removed annually by the biomass. With a desired activity reduction level of 1.5 and 5 for the bicarbonate-washed and control soil, respectively, it would take 10-50 years to attain the release limit. However, citric acid addition resulted in a decreased dry weight production.

  1. Accelerated solvent extraction by using an 'in-line' clean-up approach for multiresidue analysis of pesticides in organic honey.

    PubMed

    Chiesa, Luca Maria; Labella, Giuseppe Federico; Panseri, Sara; Britti, Domenico; Galbiati, Fabrizio; Villa, Roberto; Arioli, Francesco

    2017-02-22

    The worldwide loss of honeybee colonies may be due to their exposure to several contaminants (i.e., pesticides); such contamination may also have impacts on consumers' health. Therefore, it is essential to develop quick and new methods to detect several pesticide residues in honey samples. In this study, the effectiveness of accelerated solvent extraction (ASE) was compared with QuEChERS methods for the analysis of 53 pesticides in organic honey by gas chromatography-triple quadrupole mass spectrometry. Two simple and rapid ASE methods with 'in-line' clean-up were optimised and then compared with QuEChERS. Hexane-ethyl acetate (Hex:EtAc) and Florisil were chosen as extraction solvent and retainer for the first ASE method respectively; acetonitrile and a primary-secondary amine phase (ACN-PSA) were selected for the second ASE method. The methods were validated according to the European Union SANTE/11945/2015 guidelines. The validation parameters showed that QuEChERS and ASE with PSA as retainer had better repeatability than ASE with Hex:EtAc and Florisil. In particular, QuEChERS and ASE (ACN-PSA) showed good recovery, according to the SANTE criteria, for the majority of investigated pesticides. Conversely, when ASE with Hex:EtAc and Florisil was used as the retainer, several compounds showed recoveries lower than the acceptable value of 70%. The ASE in-line method was finally applied to evaluate pesticide concentration in organic honey samples.

  2. Determination of isopropyl-9H-thioxanthen-9-one in packaged beverages by solid-phase extraction clean-up and liquid chromatography with tandem mass spectrometry detection.

    PubMed

    Sun, Cuilian; Chan, Sheot Harn; Lu, Dan; Lee, Hui Min Wendy; Bloodworth, Bosco Chen

    2007-03-02

    A simple method was developed and validated for the trace determination of 2-isopropylthioxanthone (ITX) in packaged drinks. Samples were extracted from the food matrix using acetonitrile:water (60:40, v/v), and further subjected to clean-up and preconcentration using solid-phase extraction prior to analysis by liquid chromatography-tandem mass spectrometry using multiple reaction monitoring (MRM) mode. The use of 2-isopropyl-[(2)H7]thioxanthen-9-one was incorporated into the method as an internal standard. Excellent 3-day interday precision data (RSD 0.72%, n=10), and intraday precision data (RSD 0.52%, n=10) were obtained on a 0.10 microg/L standard solution. Spiked samples (n=8) were used to gauge the accuracy of the method at the concentration levels of 2.5, 100, and 500 microg/kg in food; recoveries ranged from 97.0 to 103.0%. These excellent validation data suggest the exciting possibility of using this method for the determination of low levels of ITX migrating from printed food packaging materials into beverages with a method quantitation limit of 0.50 microg/kg. For the first time, analysis on a range of milk, juice, tea and yoghurt drinks, as well as their respective food packaging materials were performed for comparative studies on their ITX content.

  3. Cleaning up of a nuclear facility: Destocking of Pu radioactive waste and nuclear Non-Destructive Assays

    NASA Astrophysics Data System (ADS)

    Jallu, F.; Allinei, P.-G.; Bernard, Ph.; Loridon, J.; Pouyat, D.; Torreblanca, L.

    2012-07-01

    In view to clean up a nuclear facility located at the CEA, Cadarache, France, three Non Destructive Assay (NDA) methods have been combined to characterize 2714 old, 100 L radioactive waste drums produced between 1980 and 1997. The results of X-ray radiography, passive neutron measurement and gamma-ray spectrometry are used together to extract both the βγ and α activities, and the Pu mass contained in each drum. Those drums will then be re-conditioned and cemented in 870 L containers, in order to be sent to the adequate disposal or interim storage. This paper presents the principle of the three NDA methods, the dedicated measurement setups, and it gives details about the setups, which have been especially designed and developed for that application. Uncertainties are dealt with in the last part of the paper.

  4. [Comparative analysis of the combined treatment efficacy of the Chernobyl accident clean-up workers with essential hypertension].

    PubMed

    Habulavichene, Zh M

    2012-12-01

    It was shown the results of comparative evaluation of combined treatment in 111 clean-up workers of Chernobyl accident with essential hypertension (EH). This treatment consist of angiotensin-converting enzyme inhibitors, angiotensin receptor blockers in combination with calcium channel blockers and diuretics. The follow-up period lasted 12 months. It was found that combined therapy provides comparable and reliable blood pressure (BP) control during 24-hour, significant reduction of average daily BP, daytime and nighttime BP, an index of time of the BP, BP variability. Despite on achieved target blood pressure level, 4 weeks treatment is not enough for regression of left ventricular hypertrophy (LVH). Significant regress of LVH was found if treatment lasted during a year under the condition that BP remained at the target level. It was revealed the advantage of angiotensin-converting enzyme inhibitors and angiotensin receptor blockers intake combined with a diuretic on regress of left ventricular hypertrophy and dysfunction.

  5. SOx-NOx-Rox Box{trademark} flue gas clean-up demonstration. Final report

    SciTech Connect

    1995-09-01

    The SNRB{trademark} Flue Gas Cleanup Demonstration Project was cooperatively funded by the U.S. Department of Energy (DOE), the Ohio Coal Development Office (OCDO), B&W, the Electric Power Research Institute (EPRI), Ohio Edison, Norton Chemical Process Products Company and the 3M Company. The SNRB{trademark} technology evolved from the bench and laboratory pilot scale to be successfully demonstrated at the 5-MWe field scale. Development of the SNRB{trademark} process at B&W began with pilot testing of high-temperature dry sorbent injection for SO{sub 2} removal in the 1960`s. Integration of NO{sub x} reduction was evaluated in the 1970`s. Pilot work in the 1980`s focused on evaluation of various NO{sub x} reduction catalysts, SO{sub 2} sorbents and integration of the catalyst with the baghouse. This early development work led to the issuance of two US process patents to B&W - No. 4,309,386 and No. 4,793,981. An additional patent application for improvements to the process is pending. The OCDO was instrumental in working with B&W to develop the process to the point where a larger scale demonstration of the technology was feasible. This report represents the completion of Milestone M14 as specified in the Work Plan. B&W tested the SNRB{trademark} pollution control system at a 5-MWe demonstration facility at Ohio Edison`s R. E. Burger Plant located near Shadyside, Ohio. The design and operation were influenced by the results from laboratory pilot testing at B&W`s Alliance Research Center. The intent was to demonstrate the commercial feasibility of the SNRB{trademark} process. The SNRB{trademark} facility treated a 30,000 ACFM flue gas slipstream from Boiler No. 8. Operation of the facility began in May 1992 and was completed in May 1993.

  6. Cleaning up the 'Bigmessidae': Molecular phylogeny of scleractinian corals from Faviidae, Merulinidae, Pectiniidae and Trachyphylliidae

    PubMed Central

    2011-01-01

    other subclades, which cannot be explained using macromorphology. Indeed, wide geographic sampling here has revealed more instances of possible cryptic taxa confused by evolutionary convergence of gross coral morphology. Conclusions Numerous examples of cryptic taxa determined in this study support the assertion that diversity estimates of scleractinian corals are erroneous. Fortunately, the recovery of most 'Bigmessidae' genera with only minor degrees of paraphyly offers some hope for impending taxonomic amendments. Subclades are well defined and supported by subcorallite morphological features, providing a robust framework for further systematic work. PMID:21299898

  7. THE ROLE OF LIQUID WASTE PRETREATMENT TECHNOLOGIES IN SOLVING THE DOE CLEAN-UP MISSION

    SciTech Connect

    Wilmarth, B; Sheryl Bush, S

    2008-10-31

    The objective of this report is to describe the pretreatment solutions that allow treatment to be tailored to specific wastes, processing ahead of the completion schedules for the main treatment facilities, and reduction of technical risks associated with future processing schedules. Wastes stored at Hanford and Savannah River offer challenging scientific and engineering tasks. At both sites, space limitations confound the ability to effectively retrieve and treat the wastes. Additionally, the radiation dose to the worker operating and maintaining the radiochemical plants has a large role in establishing the desired radioactivity removal. However, the regulatory requirements to treat supernatant and saltcake tank wastes differ at the two sites. Hanford must treat and remove radioactivity from the tanks based on the TriParty Agreement and Waste Incidental to Reprocessing (WIR) documentation. These authorizing documents do not specify treatment technologies; rather, they specify endstate conditions. Dissimilarly, Waste Determinations prepared at SRS in accordance with Section 3116 of the 2005 National Defense Authorization Act along with state operating permits establish the methodology and amounts of radioactivity that must be removed and may be disposed of in South Carolina. After removal of entrained solids and site-specific radionuclides, supernatant and saltcake wastes are considered to be low activity waste (LAW) and are immobilized in glass and disposed of at the Hanford Site Integrated Disposal Facility (IDF) or formulated into a grout for disposal at the Savannah River Site Saltstone Disposal Facility. Wastes stored at the Hanford Site or SRS comprise saltcake, supernate, and sludges. The supernatant and saltcake waste fractions contain primarily sodium salts, metals (e.g., Al, Cr), cesium-137 (Cs-137), technetium-99 (Tc-99) and entrained solids containing radionuclides such as strontium-90 (Sr-90) and transuranic elements. The sludges contain many of the

  8. Evaluation of the persistence of functional and biological respiratory health effects in clean-up workers 6 years after the prestige oil spill.

    PubMed

    Zock, Jan-Paul; Rodríguez-Trigo, Gema; Rodríguez-Rodríguez, Emma; Souto-Alonso, Ana; Espinosa, Ana; Pozo-Rodríguez, Francisco; Gómez, Federico P; Fuster, Carme; Castaño-Vinyals, Gemma; Antó, Josep Maria; Barberà, Joan Albert

    2014-01-01

    Fishermen who had participated in clean-up activities of the Prestige oil spill showed increased bronchial responsiveness and higher levels of respiratory biomarkers 2 years later. We aimed to evaluate the persistence of these functional and biological respiratory health effects 6 years after clean-up work. In 2008/2009 a follow-up study was done in 230 never-smoking fishermen who had been exposed to clean-up work in 2002/2003 and 87 non-exposed fishermen. Lung function and bronchial responsiveness testing and the determination of respiratory biomarkers in exhaled breath condensate were done identically as in the baseline survey in 2004/2005. Associations between participation in clean-up work and respiratory health parameters were assessed using linear and logistic regression analyses adjusting for sex and age. Information from 158 exposed (69%) and 57 non-exposed (66%) fishermen was obtained. Loss to follow-up in the non-exposed was characterised by less respiratory symptoms at baseline. During the 4-year follow-up period lung function, bronchial hyperresponsiveness and the levels of respiratory biomarkers of oxidative stress and growth factors had deteriorated notably more among non-exposed than among exposed. At follow-up, respiratory health indices were similar or better in clean-up workers than in non-exposed. No clear differences between highly exposed and moderately exposed clean-up workers were found. In conclusion, we could not detect long-term respiratory health effects in clean-up workers 6 years after the Prestige oil spill. Methodological issues that need to be considered in this type of studies include the choice of a non-exposed control group and limitation of follow-up to subgroups such as never smokers.

  9. Determination of malachite green, crystal violet and their leuco-metabolites in fish by HPLC-VIS detection after immunoaffinity column clean-up.

    PubMed

    Xie, Jie; Peng, Tao; Chen, Dong-Dong; Zhang, Qing-Jie; Wang, Guo-Min; Wang, Xiong; Guo, Qi; Jiang, Fan; Chen, Dan; Deng, Jian

    2013-01-15

    A high performance liquid chromatography method with visible detection (HPLC-VIS) for the determination of malachite green (MG), crystal violet (CV), leucomalachite green (LMG), and leucocrystal violet (LCV) in fish has been developed after clean-up through an immunoaffinity column (IAC). Residues were simultaneously extracted from fish muscle with acetonitrile and ammonium acetate buffer. The leuco-forms, LMG and LCV, were oxidized quantitatively to the chromic CV and MG by reaction with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone. Extracts were then purified on an IAC which prepared by immobilizing the anti-MG-CV antibodies by the sol-gel method. Finally, the eluents were analyzed by HPLC-VIS. The limits of detection were 0.15, 0.1, 0.18 and 0.14ng/g for MG, CV, LMG and LCV, respectively. The average recoveries in samples fortified with MG, CV, LMG and LCV over the range 0.5-10ng/g were from 71.6% to 96.8% with RSDs of 5.1-12.3% (n=6). This novel method was confirmed by liquid chromatography-tandem mass spectrometry with electrospray interface in positive mode using multiple reaction monitoring.

  10. A multi-residue method for the determination of 90 pesticides in matrices with a high water content by LC-MS/MS without clean-up.

    PubMed

    Madureira, Fernando Diniz; da Silva Oliveira, Fabiano Aurélio; de Souza, Wesley Robert; Pontelo, Ana Paula; de Oliveira, Mauro Lúcio Gonçalves; Silva, Gilsara

    2012-01-01

    A method using QuEChERS extraction and LC-MS/MS in electrospray positive ionisation mode was developed and validated for the analysis of 90 pesticides in a high water content matrix (tomato) in a single chromatographic run. To assess the intra-laboratory reproducibility of the method, validation was conducted on four different days by two different analysts. The validation data was treated using a spreadsheet developed in-house, which sets the most appropriate model for linear fit by determining whether the residuals of the calibration curves are homocedastic or heterocedastic. A statistical test for the significance of regression was also carried out. Calibration was always matrix-matched and the curves were obtained over the range 0.0075-0.10 or 0.020-0.125 mg kg(-1). Identification of analytes was based on retention times and MRM ratios. Recoveries were assessed at four different levels for each analyte and were between 73 and 106%, with relative standard deviations under reproducibility conditions of <20%. The measurement uncertainties of the method for each pesticide analysed were below 50%. Previous validation of the same method, applied to papaya samples and satisfactory results obtained in various proficiency tests with different high water content matrices, demonstrated the applicability of the method to these classes of commodities, without clean-up. The validated method will be applied routinely in the pesticide residues monitoring programme that constitutes the National Residue and Contaminant Control Plan of Brazil.

  11. Sample handling strategies for the determination of persistent trace organic contaminants from biota samples.

    PubMed

    Fidalgo-Used, Natalia; Blanco-González, Elisa; Sanz-Medel, Alfredo

    2007-05-02

    Even after emergence of most advanced instrumental techniques for the final separation, detection, identification and determination of analytes, sample handling continues to play a basic role in environmental analysis of complex matrices. In fact, sample preparation steps are often the bottleneck for combined time and efficiency in many overall analytical procedures. Thus, it is not surprising that, in the last two decades, a lot of effort has been devoted to the development of faster, safer, and more environment friendly techniques for sample extraction and extract clean up, prior to actual instrumental analysis. This article focuses on the state of the art in sample preparation of environmental solid biological samples dedicated to persistent organic pollutants (POPs) analysis. Extraction techniques such as Soxhlet extraction, sonication-assisted extraction, supercritical fluid extraction (SFE), microwave-assisted extraction (MAE), pressurised liquid extraction (PLE) and matrix solid-phase dispersion (MSPD) are reviewed and their most recent applications to the determination of POPs in biota samples are provided. Additionally, classical as well as promising novel extraction/clean-up techniques such as solid phase microextraction (SPME) are also summarized. Finally, emerging trends in sample preparation able to integrate analytes extraction and their adequate clean-up are presented.

  12. Cleaning Up Your Environment

    ERIC Educational Resources Information Center

    Feldman, Sandra

    2004-01-01

    In this article the author discusses how inadequate ventilation, poor air quality, mold and other conditions can have a detrimental impact on the health of students and school staff. She states that, these unsafe environmental conditions can cause a negative effect on students' health as well as their achievement. Furthermore, she discusses…

  13. CLEAN-UP Act

    THOMAS, 112th Congress

    Sen. Mikulski, Barbara A. [D-MD

    2011-05-12

    05/12/2011 Read twice and referred to the Committee on Homeland Security and Governmental Affairs. (All Actions) Tracker: This bill has the status IntroducedHere are the steps for Status of Legislation:

  14. Cleaning up Silicon

    NASA Technical Reports Server (NTRS)

    2000-01-01

    A development program that started in 1975 between Union Carbide and JPL, led to Advanced Silicon Materials LLC's, formerly ASiMI, commercial process for producing silane in viable quantities. The process was expanded to include the production of high-purity polysilicon for electronic devices. The technology came out of JPL's Low Cost Silicon Array Project.

  15. Cleaning up the House

    SciTech Connect

    Hogue, C.

    2007-12-15

    Under the new 'Green the Capital' initiative, measures are making the House of Representatives a more energy efficient workplace. The Capital power plant, which burns mostly coal and natural gas to heat seven boilers, must operate in a carbon-neutral fashion by the end of 2008, by increasing energy efficiency and fuel switching. Roughly 103,000 MW hours of electricity will be bought each year from solar and wind-powered sources. Other measures being implemented are use of fluorescent light bulbs and recycled paper, and a boost in recycling of materials. 4 photos.

  16. Cleaning up Floor Care.

    ERIC Educational Resources Information Center

    Carr, Richard; McLean, Doug

    1995-01-01

    Discusses how educational-facility maintenance departments can cut costs in floor cleaning through careful evaluation of floor equipment and products. Tips for choosing carpet detergents are highlighted. (GR)

  17. Cleaning Up the Environment

    ERIC Educational Resources Information Center

    Pruett, Don; Pruett, Lindsay

    2005-01-01

    Environmental community service projects provide many opportunities for students to help the environment and connect with their communities. In Washington State, students are allowed to obtain a high school varsity letter in community service if they complete over 150 community service hours in a calendar year. To help students toward this goal,…

  18. CLEAN-UP Act

    THOMAS, 111th Congress

    Rep. Sarbanes, John P. [D-MD-3

    2009-06-04

    06/26/2009 Referred to the Subcommittee on Government Management, Organization, and Procurement. (All Actions) Tracker: This bill has the status IntroducedHere are the steps for Status of Legislation:

  19. Electrical field assisted matrix solid phase dispersion as a powerful tool to improve the extraction efficiency and clean-up of fluoroquinolones in bovine milk.

    PubMed

    da Silva, Mariana Cristina; Orlando, Ricardo Mathias; Faria, Adriana Ferreira

    2016-08-26

    This work presents a new method by electrical matrix solid phase dispersion for the extraction and clean-up of marbofloxacin, ofloxacin, norfloxacin, ciprofloxacin, enrofloxacin, difloxacin and sarafloxacin in bovine milk. Composition and pH of the eluent, applied electrical potential and polarity were optimized by experimental designs. The combination of the chromatographic and electrophoretic mechanisms allowed the extraction and clean-up in one step with low organic solvent consumption, high extraction throughput and elution automation. Linearity, precision, trueness and limit of quantification were evaluated and provided values in accordance with other methods recently developed for the analysis of fluoroquinolones in milk. This technique proved to be promising for the extraction and clean-up of ionizable analytes in different milk matrices.

  20. Development of molecularly imprinted poly(methacrylic acid)/silica for clean-up and selective extraction of cholesterol in milk prior to analysis by HPLC-UV.

    PubMed

    Clausen, D N; Visentainer, J V; Tarley, C R T

    2014-10-07

    In the present paper the assessment of a novel molecularly imprinted polymer, poly(methacrylic acid)/silica, for clean-up and selective extraction of cholesterol in milk samples is described. The relative selectivity coefficient (k) values for cholesterol/5-α-cholestane and cholesterol/7-dehydrocholesterol systems were found to be 5.08 and 6.08, respectively, thus attesting the selectivity of the MIP for cholesterol under competitive adsorption with structurally analogous steroid compounds. The milk analysis was initially based on saponification followed by liquid-liquid extraction with n-hexane. Then, the protocol of molecularly imprinted solid phase extraction (MISPE) was carried out by loading the milk hexanic extract through 200 mg of MIP or NIP (non-imprinted polymer) packed into SPE cartridges at a flow rate of 0.6 mL min(-1). The washing step was performed by using n-hexane followed by further elution with ethanol and HPLC-UV analysis at 208 nm. From the breakthrough curve the maximum adsorption capacity of the MIP towards cholesterol was found to be 29.51 mg g(-1). The precision of the MISPE protocol was assessed as intra- and inter-days yielding RSD (relative standard deviations) lower than 4.10%. Cleaner HPLC chromatograms were obtained for milk samples submitted to the MISPE protocol in comparison to the solid phase extraction using the NIP or modified octadecyl silica (C18). Recoveries varying from 96.6 up to 102.2% for milk samples spiked with cholesterol were achieved, thus ensuring the accuracy of the proposed method.

  1. 40 CFR 80.8 - Sampling methods for gasoline, diesel fuel, fuel additives, and renewable fuels.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... fuel, fuel additives, and renewable fuels. 80.8 Section 80.8 Protection of Environment ENVIRONMENTAL... Provisions § 80.8 Sampling methods for gasoline, diesel fuel, fuel additives, and renewable fuels. The..., blendstocks, fuel additives and renewable fuels for purposes of determining compliance with the...

  2. Improved heat recovery and high-temperature clean-up for coal-gas fired combustion turbines

    SciTech Connect

    Barthelemy, N.M.; Lynn, S.

    1991-07-01

    This study investigates the performance of an Improved Heat Recovery Method (IHRM) applied to a coal-gas fired power-generating system using a high-temperature clean-up. This heat recovery process has been described by Higdon and Lynn (1990). The IHRM is an integrated heat-recovery network that significantly increases the thermal efficiency of a gas turbine in the generation of electric power. Its main feature is to recover both low- and high-temperature heat reclaimed from various gas streams by means of evaporating heated water into combustion air in an air saturation unit. This unit is a packed column where compressed air flows countercurrently to the heated water prior to being sent to the combustor, where it is mixed with coal-gas and burned. The high water content of the air stream thus obtained reduces the amount of excess air required to control the firing temperature of the combustor, which in turn lowers the total work of compression and results in a high thermal efficiency. Three designs of the IHRM were developed to accommodate three different gasifying process. The performances of those designs were evaluated and compared using computer simulations. The efficiencies obtained with the IHRM are substantially higher those yielded by other heat-recovery technologies using the same gasifying processes. The study also revealed that the IHRM compares advantageously to most advanced power-generation technologies currently available or tested commercially. 13 refs., 34 figs., 10 tabs.

  3. Using integrated geospatial mapping and conceptual site models to guide risk-based environmental clean-up decisions.

    PubMed

    Mayer, Henry J; Greenberg, Michael R; Burger, Joanna; Gochfield, Michael; Powers, Charles; Kosson, David; Keren, Roger; Danis, Christine; Vyas, Vikram

    2005-04-01

    Government and private sector organizations are increasingly turning to the use of maps and other visual models to provide a depiction of environmental hazards and the potential risks they represent to humans and ecosystems. Frequently, the graphic presentation is tailored to address a specific contaminant, its location and possible exposure pathways, and potential receptors. Its format is usually driven by the data available, choice of graphics technology, and the audience being served. A format that is effective for displaying one contaminant at one scale at one site, however, may be ineffective in accurately portraying the circumstances surrounding a different contaminant at the same site, or the same contaminant at a different site, because of limitations in available data or the graphics technology being used. This is the daunting challenge facing the U.S. Department of Energy (DOE), which is responsible for the nation's legacy wastes from nuclear weapons research, testing, and production at over 100 sites in the United States. In this article, we discuss the development and use of integrated geospatial mapping and conceptual site models to identify hazards and evaluate alternative long-term environmental clean-up strategies at DOE sites located across the United States. While the DOE probably has the greatest need for such information, the Department of Defense and other public and private responsible parties for many large and controversial National Priority List or Superfund sites would benefit from a similar approach.

  4. Tackling the challenge of selective analytical clean-up of complex natural extracts: the curious case of chlorophyll removal.

    PubMed

    Bijttebier, Sebastiaan; D'Hondt, Els; Noten, Bart; Hermans, Nina; Apers, Sandra; Voorspoels, Stefan

    2014-11-15

    Alkaline saponification is often used to remove interfering chlorophylls and lipids during carotenoids analysis. However, saponification also hydrolyses esterified carotenoids and is known to induce artifacts. To avoid carotenoid artifact formation during saponification, Larsen and Christensen (2005) developed a gentler and simpler analytical clean-up procedure involving the use of a strong basic resin (Ambersep 900 OH). They hypothesised a saponification mechanism based on their Liquid Chromatography-Photodiode Array (LC-PDA) data. In the present study, we show with LC-PDA-accurate mass-Mass Spectrometry that the main chlorophyll removal mechanism is not based on saponification, apolar adsorption or anion exchange, but most probably an adsorption mechanism caused by H-bonds and dipole-dipole interactions. We showed experimentally that esterified carotenoids and glycerolipids were not removed, indicating a much more selective mechanism than initially hypothesised. This opens new research opportunities towards a much wider scope of applications (e.g. the refinement of oils rich in phytochemical content).

  5. Physicochemical regeneration of high silica zeolite Y used to clean-up water polluted with sulfonamide antibiotics.

    PubMed

    Braschi, I; Blasioli, S; Buscaroli, E; Montecchio, D; Martucci, A

    2016-05-01

    High silica zeolite Y has been positively evaluated to clean-up water polluted with sulfonamides, an antibiotic family which is known to be involved in the antibiotic resistance evolution. To define possible strategies for the exhausted zeolite regeneration, the efficacy of some chemico-physical treatments on the zeolite loaded with four different sulfonamides was evaluated. The evolution of photolysis, Fenton-like reaction, thermal treatments, and solvent extractions and the occurrence in the zeolite pores of organic residues eventually entrapped was elucidated by a combined thermogravimetric (TGA-DTA), diffractometric (XRPD), and spectroscopic (FT-IR) approach. The chemical processes were not able to remove the organic guest from zeolite pores and a limited transformation on embedded molecules was observed. On the contrary, both thermal treatment and solvent extraction succeeded in the regeneration of the zeolite loaded from deionized and natural fresh water. The recyclability of regenerated zeolite was evaluated over several adsorption/regeneration cycles, due to the treatment efficacy and its stability as well as the ability to regain the structural features of the unloaded material.

  6. A probabilistic model estimating oil spill clean-up costs--a case study for the Gulf of Finland.

    PubMed

    Montewka, Jakub; Weckström, Mia; Kujala, Pentti

    2013-11-15

    Existing models estimating oil spill costs at sea are based on data from the past, and they usually lack a systematic approach. This make them passive, and limits their ability to forecast the effect of the changes in the oil combating fleet or location of a spill on the oil spill costs. In this paper we make an attempt towards the development of a probabilistic and systematic model estimating the costs of clean-up operations for the Gulf of Finland. For this purpose we utilize expert knowledge along with the available data and information from literature. Then, the obtained information is combined into a framework with the use of a Bayesian Belief Networks. Due to lack of data, we validate the model by comparing its results with existing models, with which we found good agreement. We anticipate that the presented model can contribute to the cost-effective oil-combating fleet optimization for the Gulf of Finland. It can also facilitate the accident consequences estimation in the framework of formal safety assessment (FSA).

  7. Optimization of ultrasonic extraction and clean-up protocol for the determination of polycyclic aromatic hydrocarbons in marine sediments by high-performance liquid chromatography coupled with fluorescence detection

    NASA Astrophysics Data System (ADS)

    Peng, Xuewei; Yan, Guofang; Li, Xianguo; Guo, Xinyun; Zhou, Xiao; Wang, Yan

    2012-09-01

    The procedures of ultrasonic extraction and clean-up were optimized for the determination of polycyclic aromatic hydrocarbons (PAHs) in marine sediments. Samples were ultrasonically extracted, and the extracts were purified with a miniaturized silica gel chromatographic column and analyzed with high performance liquid chromatography (HPLC) with a fluorescence detector. Ultrasonication with methanol-dichloromethane (2:1, v/v) mixture gave higher extraction efficiency than that with dichloromethane. Among the three elution solvents used in clean-up step, dichloromethane-hexane (2:3, v/v) mixture was the most satisfactory. Under the optimized conditions, the recoveries in the range of 54.82% to 94.70% with RSDs of 3.02% to 23.22% for a spiked blank, and in the range of 61.20% to 127.08% with RSDs of 7.61% to 26.93% for a spiked matrix, were obtained for the 15 PAHs studied, while the recoveries for a NIST standard reference SRM 1941b were in the range of 50.79% to 83.78% with RSDs of 5.24% to 21.38%. The detection limits were between 0.75 ng L-1 and 10.99 ng L-1for different PAHs. A sample from the Jiaozhou Bay area was examined to test the established methods.

  8. Simultaneous determination of 36 pesticide residues in spinach and cauliflower by LC-MS/MS using multi-walled carbon nanotubes-based dispersive solid-phase clean-up.

    PubMed

    Fan, Sufang; Zhao, Pengyue; Yu, Chuanshan; Pan, Canping; Li, Xuesheng

    2014-01-01

    A multi-residue method based on a modified QuEChERS sample preparation with multi-walled carbon nanotubes (MWCNTs) as reversed-dispersive solid-phase extraction (r-DSPE) material and LC-MS/MS determination by MRM mode was validated for 36 representative pesticides in spinach and cauliflower. It was demonstrated that MWCNTs can be used as effective r-DSPE materials with the QuEChERS method for the clean-up of extract from different matrices. However, MWCNTs could absorb pyrimethanil, diflubenzuron, and chlorbenzuron in both spinach and cauliflower, which leads to the low recoveries compared with PSA. The LODs and LOQs for 36 pesticides ranged from 0.1 to 5 μg kg(-1) and from 2 to 30 μg kg(-1), respectively. Good linearity was found for all pesticides with coefficients better than 0.995 in a range of 0.02-0.5 mg l(-1). The developed method with MWCNTs clean-up was successfully used to determine the 36 pesticides in real samples.

  9. Joint IDF-IUPAC-IAEA(FAO) interlaboratory validation for determining aflatoxin M1 in milk by using immunoaffinity clean-up before thin-layer chromatography.

    PubMed

    Grosso, F; Fremy, J M; Bevis, S; Dragacci, S

    2004-04-01

    A collaborative study was conducted under the auspices of the International Dairy Federation (IDF), the International Union of Pure and Applied Chemistry (IUPAC) and the International Atomic Energy Agency (IAEA), a collaborative Food and Agricultural Organization (FAO) body fully to validate a method combining immunoaffinity clean-up to thin-layer chromatography for the determination of aflatoxin M(1) in milk. Work was done in order to afford those laboratories not equipped with high-performance liquid chromatography, mainly from developing countries, with a simplified but fully validated method as an alternative to the European validated immunoaffinity-high performance liquid chromatography method published as an EN ISO Standard 14501, February 1999. The validation study was carried out on samples of aflatoxin M(1)-contaminated milk and milk powder at levels close to the tolerable level of 0.5 microg l(-1) as recommended by the Codex Alimentarius and to the regulatory level of 0.05 microg l(-1) as laid down by the European Commission. Fourteen laboratories representing 11 countries participated in the trial. The relative standard deviations for repeatability and reproducibility based on raw data were in the range 27-48 and 35-54%, respectively. The recovery rate varied from 32 to 120%. The mishandling of two crucial steps of the protocol such as matrix sample reconstitution and extract evaporation could explain the wide variation of the recovery rate. For this reason, data were then corrected for recovery. Consequently, the relative standard deviations for repeatability and reproducibility were recalculated after correction for recovery and were in the range 26-54 and 34-53%, respectively. The method will be published as a standard ISO/DIS 14674--IDF 190.

  10. Simultaneous multi-mycotoxin determination in nutmeg by ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection.

    PubMed

    Kong, Wei-Jun; Liu, Shu-Yu; Qiu, Feng; Xiao, Xiao-He; Yang, Mei-Hua

    2013-05-07

    A simple and sensitive analytical method based on ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with high performance liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection (USLE-IAC-HPLC-PCD-FLD) has been developed for simultaneous multi-mycotoxin determination of aflatoxins B1, B2, G1, G2 (AFB1, AFB2, AFG1, AFG2) and ochratoxin A (OTA) in 13 edible and medicinal nutmeg samples marketed in China. AFs and OTA were extracted from nutmeg samples by ultrasonication using a methanol : water (80 : 20, v/v) solution, followed by an IAC clean-up step. Different USL extraction conditions, pre-processing ways for nutmeg sample and clean-up columns for mycotoxins, as well as HPLC-PCD-FLD parameters (mobile phase, column temperature, elution procedure, excitation and emission wavelengths) were optimized. This method, which was appraised for analyzing nutmeg samples, showed satisfactory results with reference to limits of detection (LODs) (from 0.02 to 0.25 μg kg(-1)), limits of quantification (LOQs) (from 0.06 to 0.8 μg kg(-1)), linear ranges (up to 30 ng mL(-1) for AFB1, AFG1 and OTA and 9 ng mL(-1) for AFB2 and AFG2), intra- and inter-day variability (all <2%) and average recoveries (from 79.6 to 90.8% for AFs and from 93.6 to 97.3% for OTA, respectively). The results of the application of developed method in nutmeg samples have elucidated that four samples were detected with contamination of AFs and one with OTA. AFB1 was the most frequently found mycotoxin in 30.8% of nutmeg samples at contamination levels of 0.73-16.31 μg kg(-1). At least two different mycotoxins were co-occurred in three samples, and three AFs were simultaneously detected in one sample.

  11. Evaluation of affinity-based serum clean-up in mass spectrometric analysis: Plastic vs monoclonal antibodies.

    PubMed

    Rossetti, Cecilia; Levernæs, Maren C S; Reubsaet, Léon; Halvorsen, Trine G

    2016-11-04

    Mass spectrometric assays are now of great relevance for trace compound analysis in complex matrices such as serum and plasma samples. Especially in the quantification of low abundant protein-biomarkers, the choice of the sample preparation is crucial. In the present paper immunocapture and Molecular Imprinted Polymers (MIPs) have been applied in the determination of pro-gastrin-releasing peptide, a Small Cell Lung Cancer marker. These affinity-based techniques were compared in terms of matrix effect, limits of detection, repeatability and extraction specificity. In addition, protein precipitation was included for comparison as it is a typical sample preparation method of biological matrices. The results highlighted differences in the methods' performance and specificity, strongly affecting the outcome of the mass spectrometric determination. Plastic and monoclonal antibodies confirmed to be sensitive and specific sample preparations able to determine ProGRP at clinical relevant concentration, although only the use of monoclonal antibodies allowed the reliable quantification of ProGRP at reference levels (8pM). In addition better insight in the specificity of the three sample preparation techniques was gained. This might also be of interest for other biological applications.

  12. Advances in sample preparation in electromigration, chromatographic and mass spectrometric separation methods.

    PubMed

    Gilar, M; Bouvier, E S; Compton, B J

    2001-02-16

    The quality of sample preparation is a key factor in determining the success of analysis. While analysis of pharmaceutically important compounds in biological matrixes has driven forward the development of sample clean-up procedures in last 20 years, today's chemists face an additional challenge: sample preparation and analysis of complex biochemical samples for characterization of genotypic or phenotypic information contained in DNA and proteins. This review focuses on various sample pretreatment methods designed to meet the requirements for the analysis of biopolymers and small drugs in complex matrices. We discuss the advances in development of solid-phase extraction (SPE) sorbents, on-line SPE, membrane-based sample preparation, and sample clean-up of biopolymers prior to their analysis by mass spectrometry.

  13. 49 CFR 199.111 - Retention of samples and additional testing.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... SAFETY DRUG AND ALCOHOL TESTING Drug Testing § 199.111 Retention of samples and additional testing. (a...) Since some analytes may deteriorate during storage, detected levels of the drug below the...

  14. 49 CFR 199.111 - Retention of samples and additional testing.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... SAFETY DRUG AND ALCOHOL TESTING Drug Testing § 199.111 Retention of samples and additional testing. (a...) Since some analytes may deteriorate during storage, detected levels of the drug below the...

  15. Additives

    NASA Technical Reports Server (NTRS)

    Smalheer, C. V.

    1973-01-01

    The chemistry of lubricant additives is discussed to show what the additives are chemically and what functions they perform in the lubrication of various kinds of equipment. Current theories regarding the mode of action of lubricant additives are presented. The additive groups discussed include the following: (1) detergents and dispersants, (2) corrosion inhibitors, (3) antioxidants, (4) viscosity index improvers, (5) pour point depressants, and (6) antifouling agents.

  16. City of Atlanta and the Development Authority of DeKalb County to each Receive $300,000 to Clean up and Redevelop Contaminated Brownfields Sites

    EPA Pesticide Factsheets

    ATLANTA - Today the U.S. Environmental Protection Agency (EPA) announced that the city of Atlanta and the Development Authority of DeKalb County will each receive $300,000 to clean up and redevelop contaminated brownfields sites in Georgia. Na

  17. EPA to Hold a Public Meeting About Proposed Plan to Clean Up Soil Contamination at Benfield Industries, Inc. Superfund Site in Waynesville, N.C.

    EPA Pesticide Factsheets

    ATLANTA - On Tuesday, Jan. 13, the U.S. Environmental Protection Agency (EPA) will hold a public meeting about plans to clean up residual soil contamination at the Benfield Industries, Inc. Superfund Site in Waynesville, N.C. The meeting will be hel

  18. Acetate biostimulation as an effective treatment for cleaning up alkaline soil highly contaminated with Cr(VI).

    PubMed

    Lara, Paloma; Morett, Enrique; Juárez, Katy

    2016-08-15

    Stimulation of microbial reduction of Cr(VI) to the less toxic and less soluble Cr(III) through electron donor addition has been regarded as a promising approach for the remediation of chromium-contaminated soil and groundwater sites. However, each site presents different challenges; local physicochemical characteristics and indigenous microbial communities influence the effectiveness of the biostimulation processes. Here, we show microcosm assays stimulation of microbial reduction of Cr(VI) in highly alkaline and saline soil samples from a long-term contaminated site in Guanajuato, Mexico. Acetate was effective promoting anaerobic microbial reduction of 15 mM of Cr(VI) in 25 days accompanied by an increase in pH from 9 to 10. Our analyses showed the presence of Halomonas, Herbaspirillum, Nesterenkonia/Arthrobacter, and Bacillus species in the soil sample collected. Moreover, from biostimulated soil samples, it was possible to isolate Halomonas spp. strains able to grow at 32 mM of Cr(VI). Additionally, we found that polluted groundwater has bacterial species different to those found in soil samples with the ability to resist and reduce chromate using acetate and yeast extract as electron donors.

  19. Pesticides in seaweed: optimization of pressurized liquid extraction and in-cell clean-up and analysis by liquid chromatography-mass spectrometry.

    PubMed

    Lorenzo, R A; Pais, S; Racamonde, I; García-Rodríguez, D; Carro, A M

    2012-07-01

    Chemical residues, such as insecticides and anthelmintics, are frequently redistributed from the aquatic environment to marine species. This work reports on a fast validated protocol for the analysis of azamethiphos, three avermectins, two carbamates and two benzoylurea pesticides and chemotherapeutic agents in seaweeds based on pressurized liquid extraction and separation of analytes by liquid chromatography coupled with tandem mass spectrometry. The variables affecting the efficiency of pressurized liquid extraction, including temperature, number of extraction cycles, static extraction time and percent acetonitrile flush volume, were studied using a Doehlert design. The optimum parameters were 100 °C and one cycle of 3 min with 70 % acetonitrile. Adequate in-cell clean-up of the seaweeds was achieved using 0.8 g of Florisil over 0.1 g of graphitized carbon black on the bottom of the cell. The optimized method was validated using an analyte-free seaweed sample fortified at different concentrations. The limits of quantification ranged from 3.6 μg kg(-1) (azamethiphos) to 31.5 μg kg(-1) (abamectin). The recovery was from 87 to 120 % in most cases at different spiking levels. Finally, the reproducibility of the method expressed as the relative standard deviation and evaluated at concentrations of 10 and 50 μg kg(-1) was in the range 9-14.3 % and 6.1-12.3 %, respectively. The applicability of the method was evaluated with five commercial and 12 wild edible seaweeds, and four target compounds were detected in two wild seaweeds at a concentration below the quantification limit.

  20. Copper clean-up procedure for ultrasonic extraction and analysis of pyrethroid and phenylpyrazole pesticides in sediments by gas chromatography-electron capture detection.

    PubMed

    Wu, Jun; Lin, Youjian; Lu, Jian; Wilson, Chris

    2011-08-15

    A rapid ultrasonic extraction method coupled with a heated-copper clean-up procedure for removing interfering constituents was developed for analyzing pyrethroid and phenylpyrazole pesticides in sediments. Incubation of the 60 mL extract with 12 g copper granules at 60 °C for 2h was determined to be the optimal conditions for removing the interfering constituents. Eleven pyrethroid and phenylpyrazole pesticides were spiked into sediment samples to determine the effectiveness of the ultrasonic extraction method. The average recoveries of pyrethroids and phenylpyrazoles in sediment at 4 °C storage on day 0, 1, 7, 14, and 21 ranged from 98.6 to 120.0%, 79.2 to 116.0%, 85.0 to 119.7%, 93.6 to 118.7%, and 92.1 to 118.2%, respectively, with all percent relative standard deviations less than 10% (most <6%). This illustrated the stability of pyrethroids and phenylpyrazoles in sediment during sediment aging at 4 °C. Recoveries of the pesticides ranged from 98.6% to 120.0% for lowest fortification level (2-16 μg kg⁻¹), from 97.8% to 117.9% for middle fortification level (10-80 μg kg⁻¹), and from 94.3% to 118.1% for highest fortification level (20-160 μg kg⁻¹). Relative standard deviations of pesticide recoveries were usually less than 7%. Method detection limits of target pesticides ranged from 0.22 μg kg⁻¹ to 3.72 μg kg⁻¹. Furthermore, field sediment samples collected from four residential lakes during a three-month monitoring period were analyzed to evaluate the effectiveness of this method. Bifenthrin was detected in all of sediment samples (highest concentration 260.33±41.71 μg kg⁻¹, lowest concentration 5.68±0.38 μg kg⁻¹, and fipronil sulfone was detected at least once in sediment samples collected from three sites with concentrations ranging from 1.73±0.53 to 7.53±0.01 μg kg⁻¹.

  1. A Strategy for Skills to meet the demands of Nuclear Decommissioning and Clean-up in the UK

    SciTech Connect

    Brownridge, M.; Ensor, B.

    2008-07-01

    The NDA remit as set out within the Energy Act includes - 'to ensure the availability of skills required to deliver the overall decommissioning and nuclear clean-up mission'. The NDA approach to meeting their statutory obligation is by: - finding the best ways of re-training, re-skilling or re-deploying people in a way that encourages a more flexible workforce; - identifying and communicating the skills and workforce requirements to deliver the mission; and - developing the infrastructure and capability initiatives in line with long term needs, for example, a National Skills Academy for Nuclear, Nuclear Institute, National Graduate Scheme, and - developing locally specific provision. Firstly, NDA has set the requirement for nuclear sites to write down within the Life Time Plans (LTP), at a high level, their Site Skills Strategies; furthermore, a National Skills Working Group has been established to develop tactical cross sector solutions to support the NDA's Skills Strategy. In support of the short, medium and long term needs to meet demands of the NDA sites and the nuclear decommissioning sector, as well as being aware of the broader nuclear sector, investments have been made in infrastructure and skills programmes such as: - A National Skills Academy for Nuclear - including UK wide representation of the whole nuclear sector; - A Nuclear Institute in partnership with the University of Manchester focussing on world class research and skills in Radiation Sciences and Decommissioning Engineering; - Post Graduate sponsorship for decommissioning related projects; - A National Graduate Scheme partnership with nuclear related employers; - Vocational qualifications and Apprenticeship Schemes - Engaging 14-19 year old students to encourage the take up of Science related subjects; and - A sector wide 'Skills Passport'. In conclusion: The skills challenge has many dimensions but requires addressing due to the clear link to improved business performance and the availability

  2. An improved dispersive solid-phase extraction clean-up method for the gas chromatography-negative chemical ionisation tandem mass spectrometric determination of multiclass pesticide residues in edible oils.

    PubMed

    Deme, Pragney; Azmeera, Tirupathi; Prabhavathi Devi, B L A; Jonnalagadda, Padmaja R; Prasad, R B N; Vijaya Sarathi, U V R

    2014-01-01

    An improved sample preparation using dispersive solid-phase extraction clean-up was proposed for the trace level determination of 35 multiclass pesticide residues (organochlorine, organophosphorus and synthetic pyrethroids) in edible oils. Quantification of the analytes was carried out by gas chromatography-mass spectrometry in negative chemical ionisation mode (GC-NCI-MS/MS). The limit of detection and limit of quantification of residues were in the range of 0.01-1ng/g and 0.05-2ng/g, respectively. The analytes showed recoveries between 62% and 110%, and the matrix effect was observed to be less than 25% for most of the pesticides. Crude edible oil samples showed endosulfan isomers, p,p'-DDD, α-cypermethrin, chlorpyrifos, and diazinon residues in the range of 0.56-2.14ng/g. However, no pesticide residues in the detection range of the method were observed in refined oils.

  3. Automated clean-up, separation and detection of polycyclic aromatic hydrocarbons in particulate matter extracts from urban dust and diesel standard reference materials using a 2D-LC/2D-GC system.

    PubMed

    Ahmed, Trifa M; Lim, Hwanmi; Bergvall, Christoffer; Westerholm, Roger

    2013-10-01

    A multidimensional, on-line coupled liquid chromatographic/gas chromatographic system was developed for the quantification of polycyclic aromatic hydrocarbons (PAHs). A two-dimensional liquid chromatographic system (2D-liquid chromatography (LC)), with three columns having different selectivities, was connected on-line to a two-dimensional gas chromatographic system (2D-gas chromatography (GC)). Samples were cleaned up by combining normal elution and column back-flush of the LC columns to selectively remove matrix constituents and isolate well-defined, PAH enriched fractions. Using this system, the sequential removal of polar, mono/diaromatic, olefinic and alkane compounds from crude extracts was achieved. The LC/GC coupling was performed using a fused silica transfer line into a programmable temperature vaporizer (PTV) GC injector. Using the PTV in the solvent vent mode, excess solvent was removed and the enriched PAH sample extract was injected into the GC. The 2D-GC setup consisted of two capillary columns with different stationary phase selectivities. Heart-cutting of selected PAH compounds in the first GC column (first dimension) and transfer of these to the second GC column (second dimension) increased the baseline resolutions of closely eluting PAHs. The on-line system was validated using the standard reference materials SRM 1649a (urban dust) and SRM 1975 (diesel particulate extract). The PAH concentrations measured were comparable to the certified values and the fully automated LC/GC system performed the clean-up, separation and detection of PAHs in 16 extracts in less than 24 h. The multidimensional, on-line 2D-LC/2D-GC system eliminated manual handling of the sample extracts and minimised the risk of sample loss and contamination, while increasing accuracy and precision.

  4. 31. VIEW FROM SOUTHWEST TO CORNER WHERE SAMPLING/CRUSHING ADDITIONS ABUT ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    31. VIEW FROM SOUTHWEST TO CORNER WHERE SAMPLING/CRUSHING ADDITIONS ABUT CRUSHED OXIDIZED ORE BIN. INTACT BARREN SOLUTION TANK VISIBLE IN FRONT OF CRUSHED ORE BIN. - Bald Mountain Gold Mill, Nevada Gulch at head of False Bottom Creek, Lead, Lawrence County, SD

  5. A review of polymer nanofibres by electrospinning and their application in oil-water separation for cleaning up marine oil spills.

    PubMed

    Sarbatly, Rosalam; Krishnaiah, Duduku; Kamin, Zykamilia

    2016-05-15

    The growths of oil and gas exploration and production activities have increased environmental problems, such as oil spillage and the resulting pollution. The study of the methods for cleaning up oil spills is a critical issue to protect the environment. Various techniques are available to contain oil spills, but they are typically time consuming, energy inefficient and create secondary pollution. The use of a sorbent, such as a nanofibre sorbent, is a technique for controlling oil spills because of its good physical and oil sorption properties. This review discusses about the application of nanofibre sorbent for oil removal from water and its current developments. With their unique physical and mechanical properties coupled with their very high surface area and small pore sizes, nanofibre sorbents are alternative materials for cleaning up oil spills.

  6. Studies of levels of biogenic amines in meat samples in relation to the content of additives.

    PubMed

    Jastrzębska, Aneta; Kowalska, Sylwia; Szłyk, Edward

    2016-01-01

    The impact of meat additives on the concentration of biogenic amines and the quality of meat was studied. Fresh white and red meat samples were fortified with the following food additives: citric and lactic acids, disodium diphosphate, sodium nitrite, sodium metabisulphite, potassium sorbate, sodium chloride, ascorbic acid, α-tocopherol, propyl 3,4,5-trihydroxybenzoate (propyl gallate) and butylated hydroxyanisole. The content of spermine, spermidine, putrescine, cadaverine, histamine, tyramine, tryptamine and 2-phenylethylamine was determined by capillary isotachophoretic methods in meat samples (fresh and fortified) during four days of storage at 4°C. The results were applied to estimate the impact of the tested additives on the formation of biogenic amines in white and red meat. For all tested meats, sodium nitrite, sodium chloride and disodium diphosphate showed the best inhibition. However, cadaverine and putrescine were characterised by the biggest changes in concentration during the storage time of all the additives. Based on the presented data for the content of biogenic amines in meat samples analysed as a function of storage time and additives, we suggest that cadaverine and putrescine have a significant impact on meat quality.

  7. Enantioseparation and determination of triticonazole enantiomers in fruits, vegetables, and soil using efficient extraction and clean-up methods.

    PubMed

    Zhang, Qing; Gao, Beibei; Tian, Mingming; Shi, Haiyan; Hua, Xiude; Wang, Minghua

    2016-01-15

    An efficient and novel enantioseparation and determination method was developed to quantify the enantiomers of chiral triazole fungicide triticonazole in fruit, vegetable, and soil samples. Under the optimal chromatographic conditions, the enantiomers of triticonazole were completely enantioseparated on a cellulose tris(3-chloro-4-methyl phenyl carbamate) column with relatively good resolution (Rs=14.04). Two cleanup methods were compared to quantify the enantiomers of triticonazole. The modified QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction procedure was achieved with sufficient recoveries and low detection limits. Good recoveries were obtained for the two enantiomers ranging from 84.1% to 103.2% in the six matrices, and the relative standard deviation values ranged from 1.7% to 8.4%. Under the optimal conditions, the obtained limits of detection (LODs) were in the range of 0.0012-0.0031mg/kg for the two enantiomers, and the limits of quantification (LOQs) were in the range of 0.0036-0.0091mg/kg, which were lower than the maximum residue levels established in Japan. In addition, the stereochemical structure of triticonazole enantiomers were determined for the first time using a combination of experimental and predicted electronic circular dichroism (ECD) spectra. The first eluted enantiomer was confirmed to be (+)-(S)-triticonazole. These results indicate that the proposed method is convenient and reliable for the enantioselective detection of triticonazole in authentic samples. The proposed method could be widely applicable for investigating the stereoselective degradation of triticonazole in food and environmental matrices, providing additional information for reliable risk assessment of triazole fungicides.

  8. On the asymptotic improvement of supervised learning by utilizing additional unlabeled samples - Normal mixture density case

    NASA Technical Reports Server (NTRS)

    Shahshahani, Behzad M.; Landgrebe, David A.

    1992-01-01

    The effect of additional unlabeled samples in improving the supervised learning process is studied in this paper. Three learning processes. supervised, unsupervised, and combined supervised-unsupervised, are compared by studying the asymptotic behavior of the estimates obtained under each process. Upper and lower bounds on the asymptotic covariance matrices are derived. It is shown that under a normal mixture density assumption for the probability density function of the feature space, the combined supervised-unsupervised learning is always superior to the supervised learning in achieving better estimates. Experimental results are provided to verify the theoretical concepts.

  9. Role of radiation and non-radiation factors on the development of coronary heart disease in the Chornobyl clean-up workers: epidemiological study results.

    PubMed

    Krasnikova, L I; Buzunov, V O

    2014-09-01

    Objective. The objective of this study was to establish the risks for coronary heart disease in the Chornobyl clean-up workers with regard to a whole-body external radiation dose and non-radiation (biological, social-and-hygienic and behavioral) factors. Materials and methods. Risk-analysis was based on the cohort of the Chornobyl male clean-up workers 1986-1987 (8,625 men, including 3,623 with available whole-body external doses). Data of clinical-and-epidemiological registry, National Research Centre for Radiation Medicine were used for 1992-2013 monitoring period. We used the internal control group with radiation doses less than 0.05 Gy. Results. Statistically significant radiation risks in the Chornobyl clean-up workers were established for the coronary heart disease at doses 0.15-0.249 Gy, 0.25-0.99 Gy, 1 Gy and more (dose group 0.15-0.249 Gy RRY=1.9 (1.2; 3.1), ERR=4.6 (1.5; 14.9) Gy-1, EAR=64.2 cases per 1000 person-years, Gy); among exposed people aged 40 years and older - at doses 0.5-0.99 Gy (RRY=1.4 (1.05; 1.81), ERR=0.5 (0.03; 1.1) Gy-1, EAR=30.5 cases per 1000 person-years, Gy). Statistically significant risks for the disease under consideration were also identified with regard to non-radiation factors (smoking, improper physical training, adverse working conditions, diseases etc; age and psychoemotional overstrain were of a particular impact). Non-radiation factors are at most responsible for development of coronary heart disease. For this reason the control of potential confounding factors is required to assess the effect of the radiation factor both at a stage of comparison groups selection and analysis using the Mantel-Haenszel method.

  10. Multiplex short tandem repeat amplification of low template DNA samples with the addition of proofreading enzymes.

    PubMed

    Davis, Carey P; Chelland, Lynzee A; Pavlova, Victoria R; Illescas, María J; Brown, Kelly L; Cruz, Tracey Dawson

    2011-05-01

    With <100 pg of template DNA, routine short tandem repeat (STR) analysis often fails, resulting in no or partial profiles and increased stochastic effects. To overcome this, some have investigated preamplification methods that include the addition of proofreading enzymes to the PCR cocktail. This project sought to determine whether adding proofreading polymerases directly in the STR amplification mixture would improve the reaction when little template DNA is available. Platinum Taq High Fidelity and GeneAmp High Fidelity were tested in Profiler Plus™ STR reactions alone and in combination with AmpliTaq(®) Gold. All reactions included the additional step of a post-PCR purification step. With both pristine low template DNA and casework samples, the addition of these polymerases resulted in comparable or no improvement in the STR amplification signal. Further, stochastic effects and artifacts were observed equally across all enzyme conditions. Based on these studies, the addition of these proofreading enzymes to a multiplex STR amplification is not recommended for low template DNA work.

  11. Falcon: Visual analysis of large, irregularly sampled, and multivariate time series data in additive manufacturing

    DOE PAGES

    Steed, Chad A.; Halsey, William; Dehoff, Ryan; ...

    2017-02-16

    Flexible visual analysis of long, high-resolution, and irregularly sampled time series data from multiple sensor streams is a challenge in several domains. In the field of additive manufacturing, this capability is critical for realizing the full potential of large-scale 3D printers. Here, we propose a visual analytics approach that helps additive manufacturing researchers acquire a deep understanding of patterns in log and imagery data collected by 3D printers. Our specific goals include discovering patterns related to defects and system performance issues, optimizing build configurations to avoid defects, and increasing production efficiency. We introduce Falcon, a new visual analytics system thatmore » allows users to interactively explore large, time-oriented data sets from multiple linked perspectives. Falcon provides overviews, detailed views, and unique segmented time series visualizations, all with adjustable scale options. To illustrate the effectiveness of Falcon at providing thorough and efficient knowledge discovery, we present a practical case study involving experts in additive manufacturing and data from a large-scale 3D printer. The techniques described are applicable to the analysis of any quantitative time series, though the focus of this paper is on additive manufacturing.« less

  12. Statistical inference for the additive hazards model under outcome-dependent sampling.

    PubMed

    Yu, Jichang; Liu, Yanyan; Sandler, Dale P; Zhou, Haibo

    2015-09-01

    Cost-effective study design and proper inference procedures for data from such designs are always of particular interests to study investigators. In this article, we propose a biased sampling scheme, an outcome-dependent sampling (ODS) design for survival data with right censoring under the additive hazards model. We develop a weighted pseudo-score estimator for the regression parameters for the proposed design and derive the asymptotic properties of the proposed estimator. We also provide some suggestions for using the proposed method by evaluating the relative efficiency of the proposed method against simple random sampling design and derive the optimal allocation of the subsamples for the proposed design. Simulation studies show that the proposed ODS design is more powerful than other existing designs and the proposed estimator is more efficient than other estimators. We apply our method to analyze a cancer study conducted at NIEHS, the Cancer Incidence and Mortality of Uranium Miners Study, to study the risk of radon exposure to cancer.

  13. Statistical inference for the additive hazards model under outcome-dependent sampling

    PubMed Central

    Yu, Jichang; Liu, Yanyan; Sandler, Dale P.; Zhou, Haibo

    2015-01-01

    Cost-effective study design and proper inference procedures for data from such designs are always of particular interests to study investigators. In this article, we propose a biased sampling scheme, an outcome-dependent sampling (ODS) design for survival data with right censoring under the additive hazards model. We develop a weighted pseudo-score estimator for the regression parameters for the proposed design and derive the asymptotic properties of the proposed estimator. We also provide some suggestions for using the proposed method by evaluating the relative efficiency of the proposed method against simple random sampling design and derive the optimal allocation of the subsamples for the proposed design. Simulation studies show that the proposed ODS design is more powerful than other existing designs and the proposed estimator is more efficient than other estimators. We apply our method to analyze a cancer study conducted at NIEHS, the Cancer Incidence and Mortality of Uranium Miners Study, to study the risk of radon exposure to cancer. PMID:26379363

  14. Comparison of two clean-up methodologies for the gas chromatographic/mass spectrometric determination of low nanogram/gram levels of polynuclear aromatic hydrocarbons in seafood.

    PubMed

    Nyman, P J; Perfetti, G A; Joe, F L; Diachenko, G W

    1993-01-01

    The March 1989 oil spill in Alaska prompted the Food and Drug Administration (FDA) to conduct a thorough investigation of clean-up methodologies aimed at determining low ng/g (ppb) levels of polynuclear aromatic hydrocarbons (PAHs) in seafood. The clean-ups from a modified FDA method and a National Marine Fisheries Service (NMFS) method were evaluated on the basis of the determination of 18 PAHs at levels ranging from 1 to 5 ppb by gas chromatography/mass spectrometry. In the modified FDA method, seafood extracts were purified by a liquid-liquid partition followed by a three-step elution through silica, alumina, and C18 solid-phase extraction cartridges. In the NMFS method, seafood extracts were purified by column chromatography through a deactivated silica gel/alumina column and a gel permeation high performance liquid chromatography column. Both methods quantitated 18 PAHs at levels ranging from 1 to 5 ppb. With the exception of naphthalene, average recoveries based on internal deuterated standards ranged from 73 to 144% for the modified FDA method and 63 to 106% for the NMFS method.

  15. CLEANING UP PESTICIDE CONTAMINATED SOILS: COMPARING EFFECTIVENESS OF SUPERCRITICAL FLUID EXTRACTION WITH SOLVENT EXTRACTION AND LOW TEMPERATURE THERMAL DESORPTION

    EPA Science Inventory

    Bench-scale supercritical fluid extraction (SFE) studies were performed on soil samples obtained from a Superfund site that is contaminated with high levels of p,p,-DDT, p,p,-DDD, p,p,-DDE, toxaphene and hexachlorocyclohexane. The effectiveness of supercritical fluid extraction ...

  16. Simultaneous determination of a variety of endocrine disrupting compounds in carrot, lettuce and amended soil by means of focused ultrasonic solid-liquid extraction and dispersive solid-phase extraction as simplified clean-up strategy.

    PubMed

    Mijangos, L; Bizkarguenaga, E; Prieto, A; Fernández, L A; Zuloaga, O

    2015-04-10

    The present study is focused on the development of an analytical method based on focused ultrasonic solid-liquid extraction (FUSLE) followed by dispersive solid-phase extraction (dSPE) clean-up and liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS) optimised for the simultaneous analysis of certain endocrine disrupting compounds (EDCs), including alkylphenols (APs), bisphenol A (BPA), triclosan (TCS) and several hormones and sterols in vegetables (lettuce and carrot) and amended soil samples. Different variables affecting the chromatographic separation, the electrospray ionisation and mass spectrometric detection were optimised in order to improve the sensitivity of the separation and detection steps. Under the optimised extraction conditions (sonication of 5min at 33% of power with pulse times on of 0.8s and pulse times off of 0.2s in 10mL of n-hexane:acetone (30:70, v:v) mixture using an ice bath), different dSPE clean-up sorbents, such as Florisil, Envi-Carb, primary-secondary amine bonded silica (PSA) and C18, or combinations of them were evaluated for FUSLE extracts before LC-MS/MS. Apparent recoveries and precision in terms of relative standard deviation (RSDs %) of the method were determined at two different fortification levels (according to the matrix and the analyte) and values in the 70-130% and 2-27% ranges, respectively, were obtained for most of the target analytes and matrices. Matrix-matched calibration approach and the use of labelled standards as surrogates were needed for the properly quantification of most analytes and matrices. Method detection limits (MDLs), estimated with fortified samples, in the ranges of 0.1-100ng/g for carrot, 0.2-152ng/g for lettuce and 0.9-31ng/g for amended soil were obtained. The developed methodology was applied to the analysis of 11 EDCs in both real vegetable bought in a local market and in compost (from a local wastewater treatment plant, WWTP) amended soil samples.

  17. Detection of multiple steroidal compounds in synthetic urine using comprehensive gas chromatography-mass spectrometry (GC×GC-MS) combined with a molecularly imprinted polymer clean-up protocol.

    PubMed

    Zulfiqar, Adnan; Morgan, Geraint; Turner, Nicholas W

    2014-10-07

    A method capable of screening for multiple steroids in urine has been developed, using a series of twelve structurally similar, and commercially relevant compounds as target analytes. A molecularly imprinted solid phase extraction clean-up step was used to make the sample suitable for injection onto a GC×GC-MS setup. Significant improvements compared to a commercially available C-18 material were observed. Each individual steroid was able to be separated and identified, using both the retention profile and diagnostic fragmentation ion monitoring abilities of the comprehensive chromatographic-mass spectrometry method. Effective LODs of between 11.7 and 27.0 pg were calculated for individual steroids, effectively equivalent to concentration levels of between 0.234 and 0.540 ng mL(-1) in urine, while the application of multiple screen was demonstrated using a 10 ng mL(-1) mixed sample. The nature of this study also removes the need for sample derivitisation which speeds up the screening process.

  18. Molecularly imprinted polymer beads for clean-up and preconcentration of β-lactamase-resistant penicillins in milk.

    PubMed

    Urraca, Javier L; Chamorro-Mendiluce, Raquel; Orellana, Guillermo; Moreno-Bondi, Maria C

    2016-03-01

    This work describes the development and application of class-selective molecularly imprinted polymers (MIPs) for the analysis of beta-lactamase-resistant penicillins, namely cloxacillin (CLOXA), oxacillin (OXA), and dicloxacillin (DICLOXA), in milk samples. Our method is based on molecularly imprinted solid-phase extraction (MISPE) coupled to high-performance liquid chromatography (HPLC) with diode-array detection (DAD). 2-Biphenylylpenicillin (2BPEN), a surrogate with a close resemblance to beta-lactamase-resistant penicillins in terms of size, shape, hydrophobicity, and functionality, was synthesized and used as the template for the polymer synthesis. A MIP library was prepared and screened to select the optimum functional monomer, N-(2-aminoethyl)methacrylamide, and cross-linker, trimethylolpropane trimethacrylate, that provided the best recognition for the target antibiotics. For the MISPE application, the MIPs were prepared in the form of microspheres, using porous silica beads (40-75 μm) as sacrificial scaffolds. The developed MISPE method enables efficient extraction from aqueous samples and analysis of the antimicrobials, when followed by a selective washing with 2 mL acetonitrile-water (20:80 v/v) and elution with 1 mL 0.05 mol L(-1) tetrabutylammonium in methanol. The analytical method was validated according to EU guideline 2002/657/EC. The limits of quantification (S/N = 10) were in the 5.3-6.3 μg kg(-1) range, well below the maximum residue limits (MRLs) currently established. Inter-day mean recoveries were in the range 99-102 % with RSDs below 9 %, improving on the performance of previously reported MISPE methods for the analysis of CLOXA, OXA, or DICLOXA in milk samples.

  19. Cleaning up the Legacy of the Cold War: Plutonium Oxides and the Role of Synchrotron Radiation Research

    SciTech Connect

    Clark, David Lewis

    2015-01-21

    The deceptively simple binary formula of AnO2 belies an incredibly complex structural nature, and propensity to form mixed-valent, nonstoichiometric phases of composition AnO2±x. For plutonium, the very formation of PuO2+x has challenged a long-established dogma, and raised fundamental questions for long-term storage and environmental migration. This presentation covers two aspects of Los Alamos synchrotron radiation studies of plutonium oxides: (1) the structural chemistry of laboratory-prepared AnO2+x systems (An = U, Pu; 0 ≤ x ≤ 0.25) determined through a combination of x-ray absorption fine structure spectroscopy (XAFS) and x-ray scattering of laboratory prepared samples; and (2) the application of synchrotron radiation towards the decontamination and decommissioning of the Rocky Flats Environmental Technology Site. Making the case for particle transport mechanisms as the basis of plutonium and americium mobility, rather than aqueous sorption-desorption processes, established a successful scientific basis for the dominance of physical transport processes by wind and water. The scientific basis was successful because it was in agreement with general theory on insolubility of PuO2 in oxidation state IV, results of ultrafiltration analyses of field water/sediment samples, XAFS analyses of soil, sediment, and concrete samples, and was also in general agreement with on-site monitoring data. This understanding allowed Site contractors to rapidly move to application of soil erosion and sediment transport models as the means of predicting plutonium and americium transport, which led to design and application of site-wide soil erosion control technology to help control downstream concentrations of plutonium and americium in streamflow.

  20. Radiation and non-radiation factors and their impact on the natural history of coronary heart disease in Chornobyl accident clean-up workers.

    PubMed

    Bilyi, D O; Nastina, O M; Gabulavichene, Zh M; Sydorenko, G V; Bazyka, O D; Bilaya, V V; Kovalyov, O S

    2014-09-01

    The objective of the study was to evaluate the impact of a range of risk factors and ionizing radiation on the severity of clinical presentation of coronary heart disease (CHD) in Chornobyl accident clean-up workers (ACW). Materials and methods. A total of 376 ACW and 123 Kiev city residents with no exposure to radiation participated in the study. Study scope included the case history recording, clinical check-up, electrocardiography (ECG), daily ECG-monitoring, daily arterial blood pressure monitoring, exercise ECG, Doppler ultrasound (Doppler echocardiography), and serum lipid profile assay. The severity of CHD was scored as a sum of functional class (FC) of angina pectoris and stage of heart failure (HF) to estimate the combined impact of several risk factors. Participation in the clean-up work, age, gender, body mass excess, hypercholesterolemia, CHD, diabetes mellitus (DM), survived myocardial infarction (MI) and acute cerebral stroke, heart rhythm abnormalities, and a complete bundle branch block were accounted as risk factors. Both separate and combined impact of those factors was assayed. The combined effect was scored as a sum where value zero corresponded to no sign and value one corresponded to its presence, whereas values from 1 to 4 explained the expression of a sign according to severity or stage of a disease according to contemporary classifications. Results and conclusions. Despite the fact that clinical characterization, functional state of cardiovascular system, and comorbidities in ACW were almost similar to that in control group the onset of CHD in ACW was significantly earlier (55.9 vs. 59.8 years old). According to Spearman's rank-order correlation data there was a reliable link of FC grades and HF severity values sum to the sum of indices scoring the age group of patients, their gender, presence of arterial hypertension, MI in a history, DM type 2, heart rhythm abnormalities, and a complete bundle branch block. Cluster of risk factors

  1. Versatile fabrication of a superhydrophobic and ultralight cellulose-based aerogel for oil spillage clean-up.

    PubMed

    Zhang, Hui; Li, Yuqi; Xu, Yaoguang; Lu, Zexiang; Chen, Lihui; Huang, Liulian; Fan, Mizi

    2016-10-12

    To deal with marine oil spillage and chemical leakage issues, a highly efficient absorbent (cellulose based aerogel) with a low density (ρ < 0.034 g cm(-3), φ > 98.5%) and high mechanical strength was fabricated via a novel physical-chemical foaming method, plasma treatment and subsequent silane modification process. This aerogel has a perfect 3D skeleton and interconnected pores similar to honeycomb, which are favorable to oil adsorption and storage. More importantly, without introducing additional micro/nanoparticles, the rough micro/nano structure of the surface was directly constructed using plasma irradiation in this study. The low surface energy substrate was further introduced using a simple physical-soaking method and the resulting aerogel exhibited excellent superhydrophobicity (WCA > 156°) and superoleophilicity (OCA = 0°), which can selectively and efficiently absorb various oils or organic solvents from polluted water. In addition, this aerogel has a high storage capacity and absorption capacity (up to 4300% and 99% of its weight and volume, respectively). More interestingly, this aerogel exhibits excellent mechanical abrasion resistance and corrosion resistance even in strong acid, alkali solution and salt marine environment. The aerogel could be reused more than 30 times after removal of the absorbed oil by rinsing with ethanol.

  2. Environmental impact of a flocculant used to enhance solids transport during well bore clean-up operations

    SciTech Connect

    Yunus, M.N.M.; Procyk, A.D.; Malbrel, C.A.; Ling, K.L.C.

    1995-12-01

    This paper investigates particle flocculation as a mechanism to remove residual contaminants in well bores during completion operations. Laboratory tests and field trials were conducted demonstrating the ability of flocculating polymer sweeps to improve well bore cleaning efficiency. This process reduces the volume of fluid accumulated in the well bore that is discharged to the environment and minimizes the risk of formation damage by residuals left in the well bore. In addition, a comprehensive environmental impact study was performed on the flocculating polymers which included 72 hrs-EC50, 48 hrs-LC50, 10 day- LC50 tests on a variety of marine organisms, and bioaccumulation and biodegradability tests. In all cases, the flocculating polymers were shown to be environmentally safe at the recommended concentrations.

  3. Ultra-fast liquid chromatography with tandem mass spectrometry determination of ochratoxin A in traditional Chinese medicines based on vortex-assisted solid-liquid microextraction and aptamer-affinity column clean-up.

    PubMed

    Yang, Xihui; Hu, Yichen; Kong, Weijun; Chu, Xianfeng; Yang, Meihua; Zhao, Ming; Ouyang, Zhen

    2014-11-01

    A rapid, selective, and sensitive ultra-fast liquid chromatography with tandem mass spectrometry method was developed for the determination of ochratoxin A in traditional Chinese medicines based on vortex-assisted solid-liquid microextraction and aptamer-affinity column clean-up. Through optimizing the sample pretreatment procedures and chromatographic conditions, good linearity (r(2) ≥ 0.9993), low limit of detection (0.5-0.8 μg/kg), and satisfactory recovery (83.54-94.44%) expressed the good reliability and applicability of the established method in various traditional Chinese medicines. Moreover, the aptamer-affinity column, prepared in-house, showed an excellent feasibility owing to its specific identification of ochratoxin A in various kinds of selected traditional Chinese medicines. The maximum adsorption amount and applicability value were 188.96 ± 10.56 ng and 72.3%, respectively. The matrix effects were effectively eliminated, especially for m/z 404.2→358.0 of ochratoxin A. The application of the developed method for screening the natural contamination levels of ochratoxin A in 25 random traditional Chinese medicines on the market in China indicated that only eight samples were contaminated with low levels below the legal limit (5.0 μg/kg) set by the European Union. This study provided a preferred choice for the rapid and accurate monitoring of ochratoxin A in complex matrices.

  4. Use of gel permeation chromatography for clean-up in the analysis of coccidiostats in eggs by liquid chromatography-tandem mass spectrometry.

    PubMed

    Chico, J; Rúbies, A; Centrich, F; Companyó, R; Prat, M D; Granados, M

    2013-05-01

    An analytical method for determination and confirmation of nine coccidiostatics in eggs is reported. Ethyl acetate is used as extraction solvent, with satisfactory results, and simple automated clean-up is based on gel-permeation chromatography (GPC) . The target compounds are then analysed by liquid chromatography-electrospray ionization-tandem mass spectrometry. The method was validated in-house in accordance with Commission Decision 2002/657/EC. Trueness and precision were determined at four concentrations, and the mean errors obtained were <10 %, with relative standard deviations ranging from 3 to 18 %. For three non-authorized coccidiostatics (clopidol, ethopabate, and ronizadole), decision limit and detection capability were in the ranges 0.12-0.16 and 0.18-0.23 μg kg(-1), respectively. The results obtained prove the suitability of this new analytical method for routine monitoring of these substances in eggs.

  5. Rapid detection of chloramphenicol in animal products without clean-up using LC-high resolution mass spectrometry.

    PubMed

    Xu, Hong; Zhang, Jun; He, Jia; Mi, Jibo; Liu, Lishuang

    2011-10-01

    A rapid confirmatory and quantitative method using liquid chromatography-high resolution mass spectrometry (LC-HRMS) was developed to determine sub-µg/kg levels of chloramphenicol (CAP) in meat products. The sample plus deuterated chloramphenicol internal standard was homogenised, extracted with ethyl acetate, centrifuged and the supernatant evaporated to dryness. The residue was re-dissolved in methanol/5% ammonium acetate solution (20:80, v/v), defatted with hexane and directly injected into the LC-MS. Chromatographic separation was performed on a C(18) column using methanol/water (60:40, v/v) as the mobile phase. CAP was detected using selected ion monitoring of the high accurate mass of the molecular ion [M-H](-) of CAP using a LTQ-Orbitrap mass spectrometer in negative electrospray ionisation mode (ESI(-)). The limit of quantification of the method was 0.1 µg/kg using isotope internal standard. Recoveries of CAP spiked at levels of 0.1-1.0 µg/kg ranged from 73 to 99%, and the relative standard deviation ranged 3.9-8.1%.

  6. Evidence That Certain Waste Tank Headspace Vapor Samples Were Contaminated by Semivolatile Polymer Additives

    SciTech Connect

    Huckaby, James L.

    2006-02-09

    Vapor samples collected from the headspaces of the Hanford Site high-level radioactive waste tanks in 1994 and 1995 using the Vapor Sampling System (VSS) were reported to contain trace levels of phthalates, antioxidants, and certain other industrial chemicals that did not have a logical origin in the waste. This report examines the evidence these chemicals were sampling artifacts (contamination) and identifies the chemicals reported as headspace constituents that may instead have been contaminants. Specific recommendations are given regarding the marking of certain chemicals as suspect on the basis they were sampling manifold contaminants.

  7. Liquid chromatography-high resolution mass spectrometry with immunoaffinity clean-up for the determination of the oxidative stress biomarker 8-iso-prostaglandin F2alpha in wastewater.

    PubMed

    Ryu, Yeonsuk; Reid, Malcolm J; Thomas, Kevin V

    2015-08-28

    A reliable oxidative stress biomarker, 8-iso-prostaglandin F2α (8-iso-PGF2α), was for the first time quantitatively analysed in wastewater using an analytical method consisting of liquid chromatography-high resolution mass spectrometry coupled to immunoaffinity clean-up (IAC-LC-HRMS). Factors influencing the method's robustness were investigated, including analyte stability in sewage and enzymatic deconjugation with β-glucuronidase. The IAC-LC-HRMS method was linear over the range of 0.1-100ng/mL with correlation coefficient (R(2)) of 0.999. The quantification limits were sufficiently low to detect 8-iso-PGF2α in sewage (method quantification limit of 0.3ng/L) and precision, expressed as relative standard deviation was less than 7% and the accuracy expressed as relative recovery was in the 103-113% range. As a result, the application of the method to 24-h composite wastewater samples from Oslo showed 8-iso-PGF2α concentrations of 18.9-23.3ng/L for 8 days in March 2015. This study demonstrates a standard method to analyse 8-iso-PGF2α in sewage that will contribute to the further investigation of the potential use of 8-iso-PGF2α as a sewage biomarker for assessing the status of community health.

  8. Determination of vitamins D2, D3, K1 and K3 and some hydroxy metabolites of vitamin D3 in plasma using a continuous clean-up-preconcentration procedure coupled on-line with liquid chromatography-UV detection.

    PubMed

    Ortiz Boyer, F; Fernández Romero, J M; Luque de Castro, M D; Quesada, J M

    1999-03-01

    A semi-automatic procedure for the continuous clean-up and concentration of several fat-soluble vitamins prior to their separation by HPLC and UV detection is reported. The procedure is based on the use of a minicolumn packed with aminopropylsilica as sorbent located prior to the chromatographic detection system. The overall process was developed and applied to the main liposoluble vitamins (A, D2, D3, E, K1, K3) and several hydroxy metabolites of vitamin D3 [25-(OH)-D3,24,25-(OH)2-D3 and 1,25-(OH)2-D3]. All the analytes were monitored at a compromise wavelength of 270 nm. Calibration graphs were constructed between 0.01 and 100 ng ml-1 for vitamin D2 and D3 and their hydroxy metabolites, between 0.1 and 100 ng ml-1 for vitamin A, K1 and K3 and between 1 and 100 ng ml-1 for vitamin E, with excellent regression coefficients (> or = 0.9901) in all cases. The precision was established at two concentration levels with acceptable RSDs in all instances (between 3.6 and 8.7%). The method was appropriate for the determination of vitamin D2, D3, K1 and K3 and the 24,25-dihydroxy and 25-hydroxy metabolites of vitamin D3 in human plasma. The method was applied to plasma samples spiked with the target analytes and the recoveries ranged between 78 and 109%.

  9. Cleaning Up in New England

    EPA Pesticide Factsheets

    A page that links to information about cleanups (Superfund, Brownfields, RCRA Corrective Action and Emergency Responses) in EPA's Region 1, covering Connecticut, Maine, Massachusetts, New Hampshire, Vermont and Rhode Island.

  10. Coal cleans up its act

    SciTech Connect

    Liang-Shih Fan; Mahesh Lyer

    2006-10-15

    The paper gives an overview of current clean coal conversion processes. Gasification of coal is seen as preferable to combustion, along with CO{sub 2} separation technologies. One scheme which minimises the parasitic energy requirement for CO{sub 2} separation is based on the calcium-based carbonation-calcination reaction (CCR) process which utilises limestone at 600-700{sup o}C. The key to success lies in process integration by combining various modules in one step of operation. Current stages of development vary from conceptualisation to pilot demonstration and commercial process construction. Projects mentioned include the FutureGen project and the HyPr-ring chemical looping process. 2 figs.

  11. Optimization of an online heart-cutting multidimensional gas chromatography clean-up step for isotopic ratio mass spectrometry and simultaneous quadrupole mass spectrometry measurements of endogenous anabolic steroid in urine.

    PubMed

    Casilli, Alessandro; Piper, Thomas; de Oliveira, Fábio Azamor; Padilha, Monica Costa; Pereira, Henrique Marcelo; Thevis, Mario; de Aquino Neto, Francisco Radler

    2016-11-01

    Measuring carbon isotope ratios (CIRs) of urinary analytes represents a cornerstone of doping control analysis and has been particularly optimized for the detection of the misuse of endogenous steroids. Isotope ratio mass spectrometry (IRMS) of appropriate quality, however, necessitates adequate purities of the investigated steroids, which requires extensive pre-analytical sample clean-up steps due to both the natural presence of the target analytes and the high complexity of the matrix. In order to accelerate the sample preparation and increase the automation of the process, the use of multidimensional gas chromatography (MDGC) prior to IRMS experiments, was investigated. A well-established instrumental configuration based on two independent GC ovens and one heart-cutting device was optimized. The first dimension (1D) separation was obtained by a non-polar column which assured high efficiency and good loading capacity, while the second dimension (2D), based on a mid-polar stationary phase, provided good selectivity. A flame ionization detector monitored the 1D, and the 2D was simultaneously recorded by isotope ratio and quadrupole mass spectrometry. The assembled MDGC set-up was applied for measuring testosterone, 5α- and 5β-androstanediol, androsterone, and etiocholanolone as target compounds and pregnanediol as endogenous reference compound. The urine sample were pretreated by conventional sample preparation steps comprising solid-phase extraction, hydrolysis, and liquid-liquid extraction. The extract obtained was acetylated and different aliquots were injected into the MDGC system. Two high performance liquid chromatography steps, conventionally adopted prior to CIR measurements, were replaced by the MDGC approach. The obtained values were consistent with the conventional ones. Copyright © 2016 John Wiley & Sons, Ltd.

  12. 49 CFR 199.111 - Retention of samples and additional testing.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... request, the sample may be discarded following the end of the 365-day period. (b) If the medical review officer (MRO) determines there is no legitimate medical explanation for a confirmed positive test result... and Human Services. The operator may require the employee to pay in advance the cost of shipment...

  13. Screening of pollution control and clean-up materials for river chemical spills using the multiple case-based reasoning method with a difference-driven revision strategy.

    PubMed

    Liu, Rentao; Jiang, Jiping; Guo, Liang; Shi, Bin; Liu, Jie; Du, Zhaolin; Wang, Peng

    2016-06-01

    In-depth filtering of emergency disposal technology (EDT) and materials has been required in the process of environmental pollution emergency disposal. However, an urgent problem that must be solved is how to quickly and accurately select the most appropriate materials for treating a pollution event from the existing spill control and clean-up materials (SCCM). To meet this need, the following objectives were addressed in this study. First, the material base and a case base for environment pollution emergency disposal were established to build a foundation and provide material for SCCM screening. Second, the multiple case-based reasoning model method with a difference-driven revision strategy (DDRS-MCBR) was applied to improve the original dual case-based reasoning model method system, and screening and decision-making was performed for SCCM using this model. Third, an actual environmental pollution accident from 2012 was used as a case study to verify the material base, case base, and screening model. The results demonstrated that the DDRS-MCBR method was fast, efficient, and practical. The DDRS-MCBR method changes the passive situation in which the choice of SCCM screening depends only on the subjective experience of the decision maker and offers a new approach to screening SCCM.

  14. A food web model of mercury transfer from stream sediment to predators of fish for ecological risk based clean-up goals

    SciTech Connect

    Burns, T.P.; Hadden, C.T.; Cornaby, B.W.; Mitz, S.V.

    1997-09-01

    A linear steady-state model of the food web linking sediment to piscivorous predators was used to derive ecological risk based clean-up concentrations for mercury in sediment of East Fork Poplar Creek (EFPC), Oak Ridge, TN. The model partitions aquatic invertebrates into two classes based on the primary source of exposure to mercury in sediment, and the prey-fish community into three classes based on differences in their diets and feeding habits. Biotransfer factors for the links between sediment and sediment-dwelling invertebrates, water and aquatic biota and fish, and prey and predators are published values. The model uses site specific data on the fraction of methylmercury in sediment, the relative abundance of prey fish, and the predicted flux of mercury from sediment. Monte Carlo analysis quantifies the uncertainty in the risk to top predators of fish. At 96 mg/kg mercury in sediment, less than 20% of the exposures exceed dietary limits for endpoint receptors. The fraction of methylmercury in sediment, the three biotransfer factors for methylmercury, and diet are sensitive parameters.

  15. A systematic assessment of the state of hazardous waste clean-up technologies. Quarterly technical progress report, April 1--June 30, 1993

    SciTech Connect

    Berg, M.T.; Reed, B.E.; Gabr, M.

    1993-07-01

    West Virginia University (WVU) and the US DOE Morgantown Energy Technology Center (METC) entered into a Cooperative Agreement on August 29, 1992 entitled ``Decontamination Systems Information and Research Programs.`` Stipulated within the Agreement is the requirement that WVU submit to METC a series of Technical Progress Report for Year 1 of the Agreement. This report reflects the progress and/or efforts performed on the following nine technical projects encompassed by the Year 1 Agreement for the period of April 1 through June 30, 1993: Systematic assessment of the state of hazardous waste clean-up technologies; site remediation technologies -- drain-enhanced soil flushing (DESF) for organic contaminants removal; site remediation technologies -- in situ bioremediation of organic contaminants; excavation systems for hazardous waste sites; chemical destruction of polychlorinated biphenyls; development of organic sensors -- monolayer and multilayer self-assembled films for chemical sensors; Winfield lock and dam remediation; Assessments of Technologies for hazardous waste site remediation -- non-treatment technologies and pilot scale test facility implementation; and remediation of hazardous sites with stream reforming.

  16. [Analysis of lead in unknown samples based on the standard addition method using laser induced breakdown spectroscopy].

    PubMed

    Fang, Li; Zhao, Nan-jing; Meng, De-shuo; Yuan, Jing; Tang, Jie; Wang, Yin; Yu, Yang; Ma, Ming-jun; Hu, Li; Zhang, Da-hai; Xiao, Xue; Wang, Yu; Liu, Jian-guo; Liu, Wen-qing

    2015-01-01

    The standard addition method with laser induced breakdown spectroscopy was used to analyze an unknown sample taken from a lead battery factory. the matrix influence on the results was effectively avoided when the external or internal standard method was used, and the pretreatment of samples was simple and quick. The Nd ' YAG pulse laser with wavelength 1 064 nm was used as the excitation source. The echelle spectroscopy with high resolution and wide spectral range was used as the spectral separation device, and the intensified charge coupled device (ICCD) as the spectral detection device in the experiment. The characteristic line at 405. 78 nrn was chosen as the analysis line to measure Pb concentration. Fe I : 404. 58 line was chosen as the internal standard. Pre-experiment was carried out to confirm the appropriate condition. Under the laser energy of 128. 5 mJ, the delay time of 2. 5 tps, and the gate width of 3 ps, it was determined that with the addition of Pb to the sample in the range of 0 and 25 000 mg . kg-1, there wasn't self-absorption. There was a good linear relationship between the intensity of the spectral line of 405. 78 nm and the addition of Pb. The appropriate concentration of Pb added into the sample for analysis was determined by this series of samples. On this basis, four samples were prepared with three parallel samples for each sample in order to verify the repeatability and reliability of the method, i. e. 5 000, 10 000, 15 000, 20 000 mg . kg-1 Pb was added into the original sample. The results were compared with the result of ICP-MS. The twelve samples' relative errors were between -24. 6% and 17. 6%. The average result was 43 069 mg . kg-1 with the relative error -2. 44%.

  17. Olivibacter oleidegradans sp. nov., a hydrocarbon-degrading bacterium isolated from a biofilter clean-up facility on a hydrocarbon-contaminated site.

    PubMed

    Szabó, István; Szoboszlay, Sándor; Kriszt, Balázs; Háhn, Judit; Harkai, Péter; Baka, Erzsébet; Táncsics, András; Kaszab, Edit; Privler, Zoltán; Kukolya, József

    2011-12-01

    A novel hydrocarbon-degrading, Gram-negative, obligately aerobic, non-motile, non-sporulating, rod-shaped bacterium, designated strain TBF2/20.2(T), was isolated from a biofilter clean-up facility set up on a hydrocarbon-contaminated site in Hungary. It was characterized by using a polyphasic approach to determine its taxonomic position. Phylogenetic analysis based on 16S rRNA gene sequences indicated that the isolate is affiliated with the genus Olivibacter in the family Sphingobacteriaceae. It was found to be related most closely to Olivibacter ginsengisoli Gsoil 060(T) (93.3% 16S rRNA gene sequence similarity). Strain TBF2/20.2(T) grew at pH 6-9 (optimally at pH 6.5-7.0) and at 15-42 °C (optimally at 30-37 °C). The major fatty acids were iso-C(15:0) (39.4%), summed feature 3 (iso-C(15:0) 2-OH and/or C(16:1)ω7c; 26.0%), iso-C(17:0) 3-OH (14.5%) and C(16:0) (4.5%). The major menaquinone was MK-7 and the predominant polar lipid was phosphatidylethanolamine. The DNA G+C content of strain TBF2/20.2(T) was 41.2 mol%. Physiological and chemotaxonomic data further confirmed the distinctiveness of strain TBF2/20.2(T) from recognized members of the genus Olivibacter. Thus, strain TBF2/20.2(T) is considered to represent a novel species of the genus Olivibacter, for which the name Olivibacter oleidegradans sp. nov. is proposed. The type strain is TBF2/20.2(T) (=NCAIM B 02393(T) =CCM 7765(T)).

  18. Deriving site-specific soil clean-up values for metals and metalloids: rationale for including protection of soil microbial processes.

    PubMed

    Kuperman, Roman G; Siciliano, Steven D; Römbke, Jörg; Oorts, Koen

    2014-07-01

    Although it is widely recognized that microorganisms are essential for sustaining soil fertility, structure, nutrient cycling, groundwater purification, and other soil functions, soil microbial toxicity data were excluded from the derivation of Ecological Soil Screening Levels (Eco-SSL) in the United States. Among the reasons for such exclusion were claims that microbial toxicity tests were too difficult to interpret because of the high variability of microbial responses, uncertainty regarding the relevance of the various endpoints, and functional redundancy. Since the release of the first draft of the Eco-SSL Guidance document by the US Environmental Protection Agency in 2003, soil microbial toxicity testing and its use in ecological risk assessments have substantially improved. A wide range of standardized and nonstandardized methods became available for testing chemical toxicity to microbial functions in soil. Regulatory frameworks in the European Union and Australia have successfully incorporated microbial toxicity data into the derivation of soil threshold concentrations for ecological risk assessments. This article provides the 3-part rationale for including soil microbial processes in the development of soil clean-up values (SCVs): 1) presenting a brief overview of relevant test methods for assessing microbial functions in soil, 2) examining data sets for Cu, Ni, Zn, and Mo that incorporated soil microbial toxicity data into regulatory frameworks, and 3) offering recommendations on how to integrate the best available science into the method development for deriving site-specific SCVs that account for bioavailability of metals and metalloids in soil. Although the primary focus of this article is on the development of the approach for deriving SCVs for metals and metalloids in the United States, the recommendations provided in this article may also be applicable in other jurisdictions that aim at developing ecological soil threshold values for protection of

  19. Deriving site-specific soil clean-up values for metals and metalloids: Rationale for including protection of soil microbial processes

    PubMed Central

    Kuperman, Roman G; Siciliano, Steven D; Römbke, Jörg; Oorts, Koen

    2014-01-01

    Although it is widely recognized that microorganisms are essential for sustaining soil fertility, structure, nutrient cycling, groundwater purification, and other soil functions, soil microbial toxicity data were excluded from the derivation of Ecological Soil Screening Levels (Eco-SSL) in the United States. Among the reasons for such exclusion were claims that microbial toxicity tests were too difficult to interpret because of the high variability of microbial responses, uncertainty regarding the relevance of the various endpoints, and functional redundancy. Since the release of the first draft of the Eco-SSL Guidance document by the US Environmental Protection Agency in 2003, soil microbial toxicity testing and its use in ecological risk assessments have substantially improved. A wide range of standardized and nonstandardized methods became available for testing chemical toxicity to microbial functions in soil. Regulatory frameworks in the European Union and Australia have successfully incorporated microbial toxicity data into the derivation of soil threshold concentrations for ecological risk assessments. This article provides the 3-part rationale for including soil microbial processes in the development of soil clean-up values (SCVs): 1) presenting a brief overview of relevant test methods for assessing microbial functions in soil, 2) examining data sets for Cu, Ni, Zn, and Mo that incorporated soil microbial toxicity data into regulatory frameworks, and 3) offering recommendations on how to integrate the best available science into the method development for deriving site-specific SCVs that account for bioavailability of metals and metalloids in soil. Although the primary focus of this article is on the development of the approach for deriving SCVs for metals and metalloids in the United States, the recommendations provided in this article may also be applicable in other jurisdictions that aim at developing ecological soil threshold values for protection of

  20. Association between health information, use of protective devices and occurrence of acute health problems in the Prestige oil spill clean-up in Asturias and Cantabria (Spain): a cross-sectional study

    PubMed Central

    Carrasco, José Miguel; Lope, Virginia; Pérez-Gómez, Beatriz; Aragonés, Nuria; Suárez, Berta; López-Abente, Gonzalo; Rodríguez-Artalejo, Fernando; Pollán, Marina

    2006-01-01

    Background This paper examines the association between use of protective devices, frequency of acute health problems and health-protection information received by participants engaged in the Prestige oil spill clean-up in Asturias and Cantabria, Spain. Methods We studied 133 seamen, 135 bird cleaners, 266 volunteers and 265 paid workers selected by random sampling, stratified by type of worker and number of working days. Information was collected by telephone interview conducted in June 2003. The association of interest was summarized, using odds ratios (OR) obtained from logistic regression. Results Health-protection briefing was associated with use of protective devices and clothing. Uninformed subjects registered a significant excess risk of itchy eyes (OR:2.89; 95%CI:1.21–6.90), nausea/vomiting/dizziness (OR:2.25; 95%CI:1.17–4.32) and throat and respiratory problems (OR:2.30; 95%CI:1.15–4.61). There was a noteworthy significant excess risk of headaches (OR:3.86: 95%CI:1.74–8.54) and respiratory problems (OR:2.43; 95%CI:1.02–5.79) among uninformed paid workers. Seamen, the group most exposed to the fuel-oil, were the worst informed and registered the highest frequency of toxicological problems. Conclusion Proper health-protection briefing was associated with greater use of protective devices and lower frequency of health problems. Among seamen, however, the results indicate poorer dissemination of information and the need of specific guidelines for removing fuel-oil at sea. PMID:16390547

  1. Rapid estimation of readily leachable triazine residues in soils using automatic kinetic bioaccessibility assays followed by on-line sorptive clean-up as a front-end to liquid chromatography.

    PubMed

    Vida, Ana C F; Cocovi-Solberg, David J; Zagatto, Elias A G; Miró, Manuel

    2016-08-15

    An automatic batchwise bioaccessibility test was proposed for on-line monitoring of readily mobile pools of ametryn and atrazine residues in agricultural soils with different physicochemical properties. A 0.01molL(-1) CaCl2 solution mimicking rainwater percolation through the soil profiles was used for the herbicide extractions. The extract aliquots were successively sampled at regular time intervals in order to investigate the extraction kinetics. For extract clean-up and retention of freely dissolved target species, 30mg of restricted-access like copolymer were used as in-line sorptive material followed by elution with methanol and on-line heart-cut injection towards a C18 silica reversed-phase monolithic column (100×4.6mm) in a liquid chromatographic system. A mathematical model emphasized that the readily available pools vs time can be in most instances described by a first-order exponential equation, thus an asymptotical value is approached. Consequently, the leaching assays can be performed without attaining chemical equilibrium. Enhancement factors and detection limits were 10.2 and 18.8, and 0.40 and 0.37mgkg(-1) for ametryn and atrazine, respectively. The automatic method features good repeatability for leaching tests (r.s.d.: 11.8-10.2% for sandy and 3.7-6.2% for clayey soil). Reliable data, demonstrated with relative recoveries in the soil leachates ranging from 86 to 104%, were achieved in less than 35min, thus avoiding the need for up to 24h as recommended by standard leaching methods.

  2. Sample data processing in an additive and reproducible taxonomic workflow by using character data persistently linked to preserved individual specimens

    PubMed Central

    Kilian, Norbert; Henning, Tilo; Plitzner, Patrick; Müller, Andreas; Güntsch, Anton; Stöver, Ben C.; Müller, Kai F.; Berendsohn, Walter G.; Borsch, Thomas

    2015-01-01

    We present the model and implementation of a workflow that blazes a trail in systematic biology for the re-usability of character data (data on any kind of characters of pheno- and genotypes of organisms) and their additivity from specimen to taxon level. We take into account that any taxon characterization is based on a limited set of sampled individuals and characters, and that consequently any new individual and any new character may affect the recognition of biological entities and/or the subsequent delimitation and characterization of a taxon. Taxon concepts thus frequently change during the knowledge generation process in systematic biology. Structured character data are therefore not only needed for the knowledge generation process but also for easily adapting characterizations of taxa. We aim to facilitate the construction and reproducibility of taxon characterizations from structured character data of changing sample sets by establishing a stable and unambiguous association between each sampled individual and the data processed from it. Our workflow implementation uses the European Distributed Institute of Taxonomy Platform, a comprehensive taxonomic data management and publication environment to: (i) establish a reproducible connection between sampled individuals and all samples derived from them; (ii) stably link sample-based character data with the metadata of the respective samples; (iii) record and store structured specimen-based character data in formats allowing data exchange; (iv) reversibly assign sample metadata and character datasets to taxa in an editable classification and display them and (v) organize data exchange via standard exchange formats and enable the link between the character datasets and samples in research collections, ensuring high visibility and instant re-usability of the data. The workflow implemented will contribute to organizing the interface between phylogenetic analysis and revisionary taxonomic or monographic work

  3. Additional variability at the D12S391 STR locus in an Austrian population sample: sequencing data and allele distribution.

    PubMed

    Glock, B; Dauber, E M; Schwartz, D W; Mayr, W R

    1997-12-01

    The highly polymorphic STR locus D12S391 was investigated in an Austrian population sample (N = 150) by PCR-amplification, comparative detection on native and denaturing polyacrylamide gels and solid phase single stranded sequencing of three size variant alleles and several additional alleles. A total of 15 alleles, distinguishable by size under denaturing conditions, could be detected. No deviations from Hardy-Weinberg equilibrium were observed in the population investigated (P = 0.52). Sequencing of size variants designated 17.3 and 18.3 showed an incomplete (GAT) repeat unit at position two of the tandem region. Additional new sequence variants due to varying compositions of the number of (AGAT) and (AGAC) repeats could be identified. Due to distinct electrophoretical mobilities of alleles of the same size but different sequence structures, denaturing detection conditions should be employed when the aim is standardization.

  4. Focused ultrasound and molecularly imprinted polymers: a new approach to organotin analysis in environmental samples.

    PubMed

    Gallego-Gallegos, Mercedes; Liva, María; Olivas, Riansares Muñoz; Cámara, Carmen

    2006-05-05

    There is a high interest in speciation of organotin compounds (OTCs) in biota and marine sediment samples, due to their influence in the transmission of the contamination in the trophic chain. Sample treatment is still the most "compromising" step of speciation analysis. Extraction methods are in general time-consuming due to long extraction times and several analytical steps involved. In addition, in most cases there are problems of low recovery, especially for MBT. These drawbacks, added to the high matrix effects generally present in biota samples, make the sample treatment for organotin analysis a serious challenge for environmental issues. Here we present a novel, fast and efficient two steps method for organotin speciation in mussel and oyster tissue as well as in marine sediments. The first step based on the use of ultrasonic probe extraction for species leaching allowed us to quantitatively extract these compounds in a few minutes. Matrix interferences drastically decreased by applying a clean-up step based on the use of an imprinted polymer especially designed for tributyltin (TBT). This procedure increased accuracy and precision of the GC-FPD analysis and improving the limit of detection, Besides, this new method prevents the use of standard addition calibration method, which is mandatory without the clean-up step. The optimization and validation has been performed by using three reference materials: mussel tissue CRM-477, oyster candidate T-38 and sediment PACS-2.

  5. Towards a phylogenetic generic classification of Thelypteridaceae: Additional sampling suggests alterations of neotropical taxa and further study of paleotropical genera.

    PubMed

    Almeida, Thaís Elias; Hennequin, Sabine; Schneider, Harald; Smith, Alan R; Batista, João Aguiar Nogueira; Ramalho, Aline Joseph; Proite, Karina; Salino, Alexandre

    2016-01-01

    Thelypteridaceae is one of the largest fern families, having about 950 species and a cosmopolitan distribution but with most species occurring in tropical and subtropical regions. Its generic classification remains controversial, with different authors recognizing from one up to 32 genera. Phylogenetic relationships within the family have not been exhaustively studied, but previous studies have confirmed the monophyly of the lineage. Thus far, sampling has been inadequate for establishing a robust hypothesis of infrafamilial relationships within the family. In order to understand phylogenetic relationships within Thelypteridaceae and thus to improve generic reclassification, we expand the molecular sampling, including new samples of Old World taxa and, especially, many additional neotropical representatives. We also explore the monophyly of exclusively or mostly neotropical genera Amauropelta, Goniopteris, Meniscium, and Steiropteris. Our sampling includes 68 taxa and 134 newly generated sequences from two plastid genomic regions (rps4-trnS and trnL-trnF), plus 73 rps4 and 72 trnL-trnF sequences from GenBank. These data resulted in a concatenated matrix of 1980 molecular characters for 149 taxa. The combined data set was analyzed using maximum parsimony and bayesian inference of phylogeny. Our results are consistent with the general topological structure found in previous studies, including two main lineages within the family: phegopteroid and thelypteroid. The thelypteroid lineage comprises two clades; one of these included the segregates Metathelypteris, Coryphopteris, and Amauropelta (including part of Parathelypteris), whereas the other comprises all segregates of Cyclosorus s.l., such as Goniopteris, Meniscium, and Steiropteris (including Thelypteris polypodioides, previously incertae sedis). The three mainly neotropical segregates were found to be monophyletic but nested in a broadly defined Cyclosorus. The fourth mainly neotropical segregate, Amauropelta

  6. Assessing the matrix effects of hemolyzed samples in bioanalysis.

    PubMed

    Hughes, Nicola C; Bajaj, Navgeet; Fan, Juan; Wong, Ernest Y K

    2009-09-01

    Validation of LC-MS/MS assays includes an assessment of matrix effects. Hemolysis effect, a special type of matrix effect, can also have an impact on analyte quantitation. In situations where the hemolysis effect is marginal, this can be resolved simply by dilution of hemolyzed samples with plasma prior to analysis. However, in some cases, the impact can be so dramatic that analytes are completely immeasurable. In such situations, modification to the bioanalytical method will be required, including, but not limited to, adjusting the chromatographic conditions to separate interferences present in hemolyzed samples; additional sample clean-up techniques such as protein precipitation in combination with SPE or a change in extraction technique such as from SPE to a liquid-liquid extraction method. Here, we report examples from four bioanalytical methods, where the presence of hemolyzed blood in plasma was found to have an impact on analyte quantitation and a description of the solutions adopted to resolve this are provided.

  7. ION COMPOSITION ELUCIDATION (ICE): A HIGH RESOLUTION MASS SPECTROMETRIC TOOL FOR IDENTIFYING ORGANIC COMPOUNDS IN COMPLEX EXTRACTS OF ENVIRONMENTAL SAMPLES

    EPA Science Inventory


    Unidentified Organic Compounds. For target analytes, standards are purchased, extraction and clean-up procedures are optimized, and mass spectra and retention times for the chromatographic separation are obtained for comparison to the target compounds in environmental sample ...

  8. Combining the quick, easy, cheap, effective, rugged and safe approach and clean-up by immunoaffinity column for the analysis of 15 mycotoxins by isotope dilution liquid chromatography tandem mass spectrometry.

    PubMed

    Desmarchelier, Aurélien; Tessiot, Sabine; Bessaire, Thomas; Racault, Lucie; Fiorese, Elisa; Urbani, Alessandro; Chan, Wai-Chinn; Cheng, Pearly; Mottier, Pascal

    2014-04-11

    Optimization and validation of a multi-mycotoxin method by LC-MS/MS is presented. The method covers the EU-regulated mycotoxins (aflatoxins, fumonisins, ochratoxin A, deoxynivalenol, zearalenone, T-2 and HT-2), as well as nivalenol and 3- and 15-acetyldeoxynivalenol for analysis of cereals, cocoa, oil, spices, infant formula, coffee and nuts. The proposed procedure combines two clean-up strategies: First, a generic preparation suitable for all mycotoxins based on the QuEChERS (for quick, easy, cheap, effective, rugged and safe) protocol. Second, a specific clean-up devoted to aflatoxins and ochratoxin A using immunoaffinity column (IAC) clean-up. Positive identification of mycotoxins in matrix was conducted according to the confirmation criteria defined in EU Commission Decision 2002/657/EC while quantification was performed by isotopic dilution using (13)C-labeled mycotoxins as internal standards. Limits of quantification were at or below the maximum levels set in the EC/1886/2006 document for all mycotoxin/matrix combinations under regulation. In particular, the inclusion of an IAC step allowed achieving LOQs as low as 0.05 and 0.25μg/kg in cereals for aflatoxins and ochratoxin A, respectively. Other performance parameters like linearity [(r)(2)>0.99], recovery [71-118%], precision [(RSDr and RSDiR)<33%], and trueness [78-117%] were all compliant with the analytical requirements stipulated in the CEN/TR/16059 document. Method ruggedness was proved by a verification process conducted by another laboratory.

  9. Predictors of victim disclosure in child sexual abuse: Additional evidence from a sample of incarcerated adult sex offenders.

    PubMed

    Leclerc, Benoit; Wortley, Richard

    2015-05-01

    The under-reporting of child sexual abuse by victims is a serious problem that may prolong the suffering of victims and leave perpetrators free to continue offending. Yet empirical evidence indicates that victim disclosure rates are low. In this study, we perform regression analysis with a sample of 369 adult child sexual offenders to examine potential predictors of victim disclosure. Specifically, we extend the range of previously examined potential predictors of victim disclosure and investigate interaction effects in order to better capture under which circumstances victim disclosure is more likely. The current study differs from previous studies in that it examines the impact of victim and offense variables on victim disclosure from the perspective of the offender. In line with previous studies, we found that disclosure increased with the age of the victim and if penetration had occurred. In addition, we found that disclosure increased when the victim came from a non-dysfunctional family and resisted the abuse. The presence of an interaction effect highlighted the impact of the situation on victim disclosure. This effect indicated that as victims get older, they are more likely to disclose the abuse when they are not living with the offender at the time of abuse, but less likely to do so when they are living with the offender at the time of abuse. These findings are discussed in relation to previous studies and the need to facilitate victim disclosure.

  10. Evaluation of alternative sorbents for dispersive solid-phase extraction clean-up in the QuEChERS method for the determination of pesticide residues in rice by liquid chromatography with tandem mass spectrometry.

    PubMed

    Cabrera, Liziara da C; Caldas, Sergiane S; Prestes, Osmar D; Primel, Ednei G; Zanella, Renato

    2016-05-01

    Many compounds are used for pest control during the production and storage of rice, making it necessary to employ multiclass methods for pesticide residues determination. For this purpose, QuEChERS-based methods are very efficient, fast and accurate, and improvements in the clean-up step are important, especially for complex matrices, like cereals. In this work, different sorbents such as chitosan, florisil(®) , alumina, diatomaceous earth, graphitized carbon black, besides the commonly used primary secondary amine and octadecylsilane, were evaluated for dispersive solid-phase extraction clean-up in acetate-buffered QuEChERS method for the determination of residues of 20 representative pesticides and one metabolite in rice by liquid chromatography coupled to tandem mass spectrometry. The sorbent C18 presented the best results, however, chitosan showed similar results, and the best performance among the unconventional sorbents evaluated. The method limit of quantification, attending accuracy (70-120% recovery) and precision (RSD ≤20%) criteria, ranged from 5 to 20 μg/kg. Results showed that chitosan is an effective alternative to reduce analysis costs, maintaining the method reliability and accuracy.

  11. Can Women Bat Clean-Up, or Must They Simply Do the Cleaning? A Look at Women as Organizational Team Players.

    ERIC Educational Resources Information Center

    Gips, Crystal J.; And Others

    This study focused on the concept of "team player" among women in managerial positions in colleges and universities, and among their immediate supervisors. Female managers defined "team player" in fairly consistent terms. The male superiors tended to agree with the women's definitions but also extended the definitions with the addition of stronger…

  12. Simultaneous determination of 30 hormones illegally added to anti-ageing functional foods using UPLC-MS/MS coupled with SPE clean-up.

    PubMed

    He, Xiaoqin; Xi, Cunxian; Tang, Bobin; Wang, Guomin; Chen, Dongdong; Peng, Tao; Mu, Zhaode

    2014-01-01

    A novel analytical method employing solid-phase extraction (SPE) coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of 30 hormones in anti-ageing functional foods (capsules, powders and tablets). The analytes were extracted with acetic acid-acetonitrile (1-99 v/v), methanol and acetone, respectively. The extract was purified using a combined column, followed by analyte detection with electrospray ionisation in positive- or negative-ion modes. The results indicated that the 30 compounds had good linear correlations in the range of 1-1000 μg kg⁻¹, and the correlation coefficients were above 0.99. The limits of detection (LOD) and limits of quantification (LOQ) were 0.03-2 and 0.1-5 μg kg⁻¹, respectively. The average recovery of 30 compounds at the three spiked levels varied from 74.7% to 124.1%, and the relative standard deviation (RSD) was 2.4-15.0%. This method was applied to the analysis of hormones in 14 real samples of which seven hormones (such as estrone, dienestrol) were detected in four samples, but the remainder of the hormones were not detected. The developed method is sensitive, efficient, reliable and applicable to real samples.

  13. Modelling uncertainty estimation for the determination of aflatoxin M(1) in milk by visual and densitometric thin-layer chromatography with immunoaffinity column clean-up.

    PubMed

    Carvalho, K L; Gonçalves, G A A; Lopes, A L; Santos, E A; Vargas, E A; Magalhães, W F

    2012-01-01

    The uncertainty of aflatoxin M(1) concentration in milk, determined by thin-layer chromatography (TLC) with visual and densitometric quantification of the fluorescence intensities of the spots, was estimated using the cause-and-effect approach proposed by ISO GUM (Guide to the expression of uncertainty in measurement) following its main four steps. The sources of uncertainties due to volume measurements, visual and densitometric TLC calibration curve, allowed range for recovery variation and intermediary precision to be taken into account in the uncertainty budget. For volume measurements the sources of uncertainties due to calibration, resolution, laboratory temperature variation and repeatability were considered. For the quantification by visual readings of the intensity of the aflatoxin M(1) in the TLC the uncertainty arising from resolution calibration curves was modelled based on the intervals of concentrations between pairs of the calibration standard solutions. The uncertainty of the densitometric TLC quantification arising from the calibration curve was obtained by weighted least square (WLS) regression. Finally, the repeatability uncertainty of the densitometric peak areas or of the visual readings for the test sample solutions was considered. For the test samples with aflatoxin M(1) concentration between 0.02 and 0.5 µg l(-1), the relative expanded uncertainties, with approximately 95% of coverage probability, obtained for visual TLC readings were between 60% and 130% of the values predicted by the Horwitz model. For the densitometric TLC determination they were about 20% lower. The main sources of uncertainties in both visual and densitometric TLC quantification were the intermediary precision, calibration curve and recovery. The main source of uncertainty in the calibration curve in the visual TLC analysis was due to the resolution of the visual readings, whereas in the densitometric analysis it was due to the peak areas of test sample solutions

  14. From a Mere Clean-up Contract to Changing Lives - Engaging the Local Stakeholders during the Remediation of Christmas Island, Pacific Ocean

    SciTech Connect

    Steadman, J.P.

    2006-07-01

    This paper describes the work undertaken by Safety and Ecology Corporation Ltd (SEC) on Kiritimati, formerly known as Christmas Island. The discussion describes the project growing from merely removing the remains of the nuclear testing, to appreciating the sensitivities of its economic impact on the island and developing a programme of redevelopment and community involvement. The remediation work has had a number of positive effects on the island, notably upgrading the infrastructure and removing more than 23,000 cubic meters of waste material, primarily metal scrap in the form of vehicles, in addition to spent batteries, extensive areas of tar contaminated soils and radioactive luminous vehicle dials. (authors)

  15. Comparative study of different clean-up techniques for the determination of λ-cyhalothrin and cypermethrin in palm oil matrices by gas chromatography with electron capture detection.

    PubMed

    Muhamad, Halimah; Zainudin, Badrul Hisyam; Abu Bakar, Nor Kartini

    2012-10-15

    Solid phase extraction (SPE) and dispersive solid-phase extraction (d-SPE) were compared and evaluated for the determination of λ-cyhalothrin and cypermethrin in palm oil matrices by gas chromatography with an electron capture detector (GC-ECD). Several SPE sorbents such as graphitised carbon black (GCB), primary secondary amine (PSA), C(18), silica, and florisil were tested in order to minimise fat residues. The results show that mixed sorbents using GCB and PSA obtained cleaner extracts than a single GCB and PSA sorbents. The average recoveries obtained for each pesticide ranged between 81% and 114% at five fortification levels with the relative standard deviation of less than 7% in all cases. The limits of detection for these pesticides were ranged between 0.025 and 0.05 μg/g. The proposed method was applied successfully for the residue determination of both λ-cyhalothrin and cypermethrin in crude palm oil samples obtained from local mills throughout Malaysia.

  16. An Optimized High Throughput Clean-Up Method Using Mixed-Mode SPE Plate for the Analysis of Free Arachidonic Acid in Plasma by LC-MS/MS.

    PubMed

    Wang, Wan; Qin, Suzi; Li, Linsen; Chen, Xiaohua; Wang, Qunjie; Wei, Junfu

    2015-01-01

    A high throughput sample preparation method was developed utilizing mixed-mode solid phase extraction (SPE) in 96-well plate format for the determination of free arachidonic acid in plasma by LC-MS/MS. Plasma was mixed with 3% aqueous ammonia and loaded into each well of 96-well plate. After washing with water and methanol sequentially, 3% of formic acid in acetonitrile was used to elute arachidonic acid. The collected fraction was injected onto a reversed phase column at 30°C with mobile phase of acetonitrile/water (70 : 30, v/v) and detected by LC-MS/MS coupled with electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode. The calibration curve ranged from 10 to 2500 ng/mL with sufficient linearity (r (2) = 0.9999). The recoveries were in the range of 99.38% to 103.21% with RSD less than 6%. The limit of detection is 3 ng/mL.

  17. NCW 2002: Chemistry Keeps Us Clean. Chemists Clean Up: A History and Exploration of the Craft of Soapmaking How Soap Came to be Common in America

    NASA Astrophysics Data System (ADS)

    Kostka, Kim; McKay, David D.

    2002-10-01

    Soap is an article whose commonplace presence and obvious necessity we take for granted at the dawn of the twenty-first century. For most of American history bath soap, however, was a luxury product. This paper explores the confluence of the cultural and technological changes that led to its transformation into the ubiquitous and well-used object it is today. We pick up the timeline for the development of soap in the early American republic when soapmaking was a householder's task and soap use was generally limited to laundering clothes. We then trace the rise of the American cleanliness movement and correlate this rise to the increased manufacturing capabilities of the nation's large soapmakers. This technological forward movement included improvements in producing alkalis as well as the inception and growth of the oleochemicals industry. Additional growth agents were the development of market analysis, advertising campaigns, and factory-scale hydrolysis of fatty acids from their parent fats.

    See Featured Molecules.

  18. Detection of triazole deicing additives in soil samples from airports with low, mid, and large volume aircraft deicing activities.

    PubMed

    McNeill, K S; Cancilla, D A

    2009-03-01

    Soil samples from three USA airports representing low, mid, and large volume users of aircraft deicing fluids (ADAFs) were analyzed by LC/MS/MS for the presence of triazoles, a class of corrosion inhibitors historically used in ADAFs. Triazoles, specifically the 4-methyl-1H-benzotriazole and the 5-methyl-1H-benzotriazole, were detected in a majority of samples and ranged from 2.35 to 424.19 microg/kg. Previous studies have focused primarily on ground and surface water impacts of larger volume ADAF users. The detection of triazoles in soils at low volume ADAF use airports suggests that deicing activities may have a broader environmental impact than previously considered.

  19. Electrofishing and the effects of depletion sampling on fish health: A review and recommendations for additional study

    USGS Publications Warehouse

    Panek, F.M.; Densmore, Christine L.; Cipriano, R.C.; Bruckner, A.W.; Shchelkunov, I.S.

    2011-01-01

    Depletion sampling in combination with multiple-pass electrofishing is an important fisheries management tool for wadeable streams. This combination of techniques has been used routinely by federal and state fishery management agencies for several decades as a reliable means to obtain quantitative data on trout populations or to describe fish community structure. In this paper we review the effects of electrofishing on fish and discuss this within the context of depletion sampling and multiple exposures of fishes to electric fields. The multiple wave forms most commonly used in sampling (alternating current, direct current, and pulsed direct current) are discussed as well as electrofishing induced response, injury and physiological stress. Fish that survive electrofishing injuries are more likely to suffer short and long-term adverse effects to their behavior, health, growth, or reproduction. Of greatest concern are the native, non-target species that may be subjected to multiple electrical shocks during the course of a 3-pass depletion survey. These exposures and their effects on the non-target species warrant further study as do the overall effects of electrofishing on populations and community structure. 

  20. Sample Preparation Strategies for the Effective Quantitation of Hydrophilic Metabolites in Serum by Multi-Targeted HILIC-MS/MS.

    PubMed

    Tsakelidou, Elisavet; Virgiliou, Christina; Valianou, Lemonia; Gika, Helen G; Raikos, Nikolaos; Theodoridis, Georgios

    2017-03-30

    The effect of endogenous interferences of serum in multi-targeted metabolite profiling HILIC-MS/MS analysis was investigated by studying different sample preparation procedures. A modified QuEChERS dispersive SPE protocol, a HybridSPE protocol, and a combination of liquid extraction with protein precipitation were compared to a simple protein precipitation. Evaluation of extraction efficiency and sample clean-up was performed for all methods. SPE sorbent materials tested were found to retain hydrophilic analytes together with endogenous interferences, thus additional elution steps were needed. Liquid extraction was not shown to minimise matrix effects. In general, it was observed that a balance should be reached in terms of recovery, efficient clean-up, and sample treatment time when a wide range of metabolites are analysed. A quick step for removing phospholipids prior to the determination of hydrophilic endogenous metabolites is required, however, based on the results from the applied methods, further studies are needed to achieve high recoveries for all metabolites.

  1. Cleaning Up Contaminated Wood-Treating Sites

    DTIC Science & Technology

    1995-09-01

    treating sites throughout the United States. OTA found that there are many Superfund wood-treatment sites located in this country that are very...hazardous waste cleanup at wood- pany Superfund site, in Texarkana, Texas. The treating sites throughout the country. OTA has 25-acre site, a former...could be applied to mental Protection Agency (EPA) Superfund site other sites in the future. OTA has not recom- in 1986 (27). Wood products had been

  2. Cleaning up the Streets of Denver

    SciTech Connect

    Stegen, R.L.; Wood, T.R.; Hackett, J.R.; Sogue, A.

    2006-07-01

    Between 1913 and 1924, several Denver area facilities extracted radium from carnotite ore mined from the Paradox basin region of Colorado. Tailings or abandoned ores from these facilities were apparently incorporated into asphalt used to pave approximately 7.2 kilometers (4.5 miles) of streets in Denver. A majority of the streets are located in residential areas. The radionuclides are bound within the asphalt matrix and pose minimal risk unless they are disturbed. The City and County of Denver (CCoD) is responsible for controlling repairs and maintenance on these impacted streets. Since 2002, the CCoD has embarked on a significant capital improvement project to remove the impacted asphalt for secure disposal followed by street reconstruction. To date, Parsons has removed approximately 55 percent of the impacted asphalt. This paper discusses the history of the Denver Radium Streets and summarizes on-going project efforts. (authors)

  3. Navajo Nation: Cleaning Up Abandoned Uranium Mines

    EPA Pesticide Factsheets

    This site provides information about the progress of EPA's cleanup of abandoned uranium mines on Navajo and Hopi lands and in other areas of Arizona and New Mexico, including health impacts, major enforcement and removal milestones, and community actions.

  4. Cleaning up: Battling Germs in School Facilities

    ERIC Educational Resources Information Center

    Gerba, Charles P.

    2009-01-01

    Every school year, parents, teachers, and administrators must deal with an overwhelming number of sick children. In fact, according to the Centers for Disease Control and Prevention, the average child catches at least eight colds a year, and kids in the United States miss as many as 189 million school days annually due to colds. Good hygiene…

  5. Cleaning Up Electronic Waste (E-Waste)

    EPA Pesticide Factsheets

    While accurate data on the amount of e-waste being exported from the U.S. are not available, the United States government is concerned that these exports are being mismanaged abroad, causing serious public health and environmental hazards.

  6. "Z" Facility Dielectric Oil Clean-Up

    SciTech Connect

    Alessandri, Daniel; Bloomquist, Doug; Donovan, Guy; Feltz, Greg; Grelle, Nibby; Guthrie, Doug; Harris, Mark; Horry, Mike; Lockas, Mike; Potter, Jimmy; Pritchard, Chuck; Steedly, Jim

    1999-06-30

    In August of 1998 the Z facility leaked approximately 150 gallons of deionized water into the dielectric oil of the Energy Storage Section (ESS). After processing the oil to remove existing particulate and free water the dielectric breakdown strength increased from the mid 20kV range to values in excess of 40 kV. 40 kV is above historical operating levels of about 35 kV. This, however, was not enough to allow 90 kV charging of the Marx Generators in the ESS. Further analysis of the oil showed dissolved water at a saturated level (70 - 80 ppm) and some residual particulate contamination smaller than 3 microns. The dissolved water and particulate combination was preventing the 90 kV charging of the Marx Generators in the ESS. After consulting with the oil industry it was determined that nitrogen sparging could be used to remove the dissolved water. Further particulate filtering was also conducted. After approximately 20 hours of sparging the water content in the ESS was reduced to 42 ppm which enabled Marx charging to 90 kV.

  7. Clean Up Your School Custodial Program.

    ERIC Educational Resources Information Center

    Steller, Arthur W.; Pell, Carroll

    1986-01-01

    Administrators can improve their school's custodial program by following steps that increase productivity, reduce costs, and provide long-term benefits of higher cleanliness standards. Administrators should work toward improved building cleanliness by insisting on a school board policy that establishes objectives for the custodial department.…

  8. Tanker industry progressing in cleaning up operations

    SciTech Connect

    Knott, D.

    1993-10-18

    The international tanker industry has made significant strides in improving the safety and environmental awareness of its operations in recent years. With a string of mishaps following the Exxon Valdez spill, public scrutiny focused on the tanker industry and found it lacking. The U.S. government reacted strongly with the Oil Pollution Act of 1990. OPA 90 set narrow requirements for tanker construction, forced the creation of a national spill response program, and made tanker operators solely liable for spill damage. The Aegean Sea and Braer accidents around the end of last year forced the pace of European legislation. Since then global initiatives have been announced to improve design and maintenance of tankers and take steps toward eliminating substandard ships and operators. The paper discusses priorities, tanker design, the tanker fleet, OPA status, spill response, the Tampa Bay spill, spill liability, European spills, EC legislation, and the Department of Transportation inquiry.

  9. Progress and challenges in cleaning up Hanford

    SciTech Connect

    Wagoner, J.D.

    1997-08-01

    This paper presents captioned viewgraphs which briefly summarize cleanup efforts at the Hanford Site. Underground waste tank and spent nuclear fuel issues are described. Progress is reported for the Plutonium Finishing Plant, PUREX plant, B-Plant/Waste Encapsulation Storage Facility, and Fast Flux Test Facility. A very brief overview of costs and number of sites remediated and/or decommissioned is given.

  10. Lymphatic vessels clean up your arteries.

    PubMed

    Fernández-Hernando, Carlos

    2013-04-01

    Reverse cholesterol transport (RCT) is the pathway by which cholesterol accumulated in peripheral tissues, including the artery wall, is transported to the liver for excretion. There is strong evidence suggesting that interventions that increase macrophage cholesterol efflux and RCT would be antiatherogenic. In this issue of the JCI, Martel et al. investigate the contribution of lymphatic vasculature to RCT. Their results support the concept that the lymphatic vessel route is critical for RCT from atherosclerotic plaques. Therefore, strategies to improve lymphatic transport might be useful for treating atherosclerotic vascular disease.

  11. Upton bill offers clean-up incentives

    SciTech Connect

    Black, B.

    1994-07-01

    Like castor oil, the Superfund law can be difficult medicine to swallow, and no one wants to volunteer for a dose. Indeed, the law`s harsh and unbending liability scheme sometimes hinders the cleanup of contaminated property. Confronted with the choice of redeveloping an old {open_quotes}brownfield{close_quotes} urban industrial site or building at a pristine new {open_quotes}greenfield{close_quotes} location, most companies opt for the latter. The brownfield problem is especially troubling because the law often prevents voluntary cleanups at relatively low priority sites that usually don`t get caught up in the Superfund program. This paper describes the Upton Bill which would require the US EPA to establish cleanup standards for hazrdous substances, allow for public comment on a proposed response plan, and require a voluntary party to submit detailed annual reports and maintain records.

  12. Slow clean-up for fast reactor

    NASA Astrophysics Data System (ADS)

    Banks, Michael

    2008-05-01

    The year 2300 is so distant that one may be forgiven for thinking of it only in terms of science fiction. But this is the year that workers at the Dounreay power station in Northern Scotland - the UK's only centre for research into "fast" nuclear reactors - term as the "end point" by which time the site will be completely clear of radioactive material. More than 180 facilities - including the iconic dome that housed the Dounreay Fast Reactor (DFR) - were built at at the site since it opened in 1959, with almost 50 having been used to handle radioactive material.

  13. Percent recoveries of anthropogenic organic compounds with and without the addition of ascorbic acid to preserve finished-water samples containing free chlorine, 2004-10

    USGS Publications Warehouse

    Valder, Joshua F.; Delzer, Gregory C.; Bender, David A.; Price, Curtis V.

    2011-01-01

    This report presents finished-water matrix-spike recoveries of 270 anthropogenic organic compounds with and without the addition of ascorbic acid to preserve water samples containing free chlorine. Percent recoveries were calculated using analytical results from a study conducted during 2004-10 for the National Water-Quality Assessment (NAWQA) Program of the U.S. Geological Survey (USGS). The study was intended to characterize the effect of quenching on finished-water matrix-spike recoveries and to better understand the potential oxidation and transformation of 270 anthropogenic organic compounds. The anthropogenic organic compounds studied include those on analytical schedules 1433, 2003, 2033, 2060, 2020, and 4024 of the USGS National Water Quality Laboratory. Three types of samples were collected from 34 NAWQA locations across the Nation: (1) quenched finished-water samples (not spiked), (2) quenched finished-water matrix-spike samples, and (3) nonquenched finished-water matrix-spike samples. Percent recoveries of anthropogenic organic compounds in quenched and nonquenched finished-water matrix-spike samples are presented. Comparisons of percent recoveries between quenched and nonquenched spiked samples can be used to show how quenching affects finished-water samples. A maximum of 18 surface-water and 34 groundwater quenched finished-water matrix-spike samples paired with nonquenched finished-water matrix-spike samples were analyzed. Percent recoveries for the study are presented in two ways: (1) finished-water matrix-spike samples supplied by surface-water or groundwater, and (2) by use (or source) group category for surface-water and groundwater supplies. Graphical representations of percent recoveries for the quenched and nonquenched finished-water matrix-spike samples also are presented.

  14. Study Design and Percent Recoveries of Anthropogenic Organic Compounds With and Without the Addition of Ascorbic Acid to Preserve Water Samples Containing Free Chlorine, 2004-06

    USGS Publications Warehouse

    Valder, Joshua F.; Delzer, Gregory C.; Price, Curtis V.; Sandstrom, Mark W.

    2008-01-01

    The National Water-Quality Assessment (NAWQA) Program of the U.S. Geological Survey (USGS) began implementing Source Water-Quality Assessments (SWQAs) in 2002 that focus on characterizing the quality of source water and finished water of aquifers and major rivers used by some of the larger community water systems in the United States. As used for SWQA studies, source water is the raw (ambient) water collected at the supply well prior to water treatment (for ground water) or the raw (ambient) water collected from the river near the intake (for surface water). Finished water is the water that is treated, which typically involves, in part, the addition of chlorine or other disinfection chemicals to remove pathogens, and is ready to be delivered to consumers. Finished water is collected before the water enters the distribution system. This report describes the study design and percent recoveries of anthropogenic organic compounds (AOCs) with and without the addition of ascorbic acid to preserve water samples containing free chlorine. The percent recoveries were determined by using analytical results from a laboratory study conducted in 2004 by the USGS's National Water Quality Laboratory (NWQL) and from data collected during 2004-06 for a field study currently (2008) being conducted by the USGS's NAWQA Program. The laboratory study was designed to determine if preserving samples with ascorbic acid (quenching samples) adversely affects analytical performance under controlled conditions. During the laboratory study, eight samples of reagent water were spiked for each of five analytical schedules evaluated. Percent recoveries from these samples were then compared in two ways: (1) four quenched reagent spiked samples analyzed on day 0 were compared with four quenched reagent spiked samples analyzed on day 7 or 14, and (2) the combined eight quenched reagent spiked samples analyzed on day 0, 7, or 14 were compared with eight laboratory reagent spikes (LRSs). Percent

  15. New approach of a transient ICP-MS measurement method for samples with high salinity.

    PubMed

    Hein, Christina; Sander, Jonas Michael; Kautenburger, Ralf

    2017-03-01

    In the near future it is necessary to establish a disposal for high level nuclear waste (HLW) in deep and stable geological formations. In Germany typical host rocks are salt or claystone. Suitable clay formations exist in the south and in the north of Germany. The geochemical conditions of these clay formations show a strong difference. In the northern ionic strengths of the pore water up to 5M are observed. The determination of parameters like Kd values during sorption experiments of metal ions like uranium or europium as homologues for trivalent actinides onto clay stones are very important for long term safety analysis. The measurement of the low concentrated, not sorbed analytes commonly takes place by inductively coupled plasma mass spectrometry (ICP-MS). A direct measurement of high saline samples like seawater with more than 1% total dissolved salt content is not possible. Alternatives like sample clean up, preconcentration or strong dilution have more disadvantages than advantages for example more preparation steps or additional and expensive components. With a small modification of the ICP-MS sample introduction system and a home-made reprogramming of the autosampler a transient analysing method was developed which is suitable for measuring metal ions like europium and uranium in high saline sample matrices up to 5M (NaCl). Comparisons at low ionic strength between the default and the transient measurement show the latter performs similarly well to the default measurement. Additionally no time consuming sample clean-up or expensive online dilution or matrix removal systems are necessary and the analysation shows a high sensitivity due to the data processing based on the peak area.

  16. Determination of carbamates in edible vegetable oils by ultra-high performance liquid chromatography-tandem mass spectrometry using a new clean-up based on zirconia for QuEChERS methodology.

    PubMed

    Moreno-González, David; Huertas-Pérez, José F; García-Campaña, Ana M; Gámiz-Gracia, Laura

    2014-10-01

    In this study a fast, selective and sensitive multiresidue method based on QuEChERS methodology has been evaluated and validated for the determination of carbamate pesticides, in edible vegetable oils by UHPLC-MS/MS. A new clean-up sorbent, Supel(TM) QuE Z-Sep(+), has been successfully applied in vegetable oil extracts. Z-Sep(+) was compared with other sorbents (i.e. mixture of C18 and PSA) previously used for dispersive solid phase extraction of these matrices, reducing more effectively matrix effects without a significant decrease of analyte recoveries. Matrix effect was studied in different matrices (extra-virgin olive, sunflower, maize, linseed and sesame oil) being ≤│30│% for most of the studied pesticides. Under optimum conditions, recoveries ranged from 74% to 101%, with relative standard deviations lower than 10%. Limits of quantification ranged from 0.09 to 2.0 µg kg(-1), allowing their determination at the low concentration levels demanding by current legislation.

  17. The role of methanol addition to water samples in reducing analyte adsorption and matrix effects in liquid chromatography-tandem mass spectrometry.

    PubMed

    Li, Wei; Liu, Yucan; Duan, Jinming; Saint, Christopher P; Mulcahy, Dennis

    2015-04-10

    Liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis coupled simply with water filtering before injection has proven to be a simple, economic and time-saving method for analyzing trace-level organic pollutants in aqueous environments. However, the linearity, precision and detection limits of such methods for late-eluting analytes were found to be much poorer than for early-eluting ones due to adsorption of the analytes in the operating system, such as sample vial, flow path and sample loop, creating problems in quantitative analysis. Addition of methanol (MeOH) into water samples as a modifier was shown to be effective in alleviating or even eliminating the negative effect on signal intensity for the late-eluting analytes and at the same time being able to reduce certain matrix effects for real water samples. Based on the maximum detection signal intensity obtained on desorption of the analytes with MeOH addition, the ratio of the detection signal intensity without addition of MeOH to the maximum intensity can be used to evaluate the effectiveness of methanol addition. Accordingly, the values of <50%, 50-80%, 80-120% could be used to indicate strong, medium and no effects, respectively. Based on this concept, an external matrix-matched calibration method with the addition of MeOH has been successfully established for analyzing fifteen pesticides with diverse physico-chemical properties in surface and groundwater with good linearity (r(2): 0.9929-0.9996), precision (intra-day relative standard deviation (RSD): 1.4-10.7%, inter-day RSD: 1.5-9.4%), accuracy (76.9-126.7%) and low limits of detection (0.003-0.028μg/L).

  18. Ultrasound-assisted leaching-dispersive solid-phase extraction followed by liquid-liquid microextraction for the determination of polybrominated diphenyl ethers in sediment samples by gas chromatography-tandem mass spectrometry.

    PubMed

    Fontana, Ariel R; Lana, Nerina B; Martinez, Luis D; Altamirano, Jorgelina C

    2010-06-30

    Ultrasound-assisted leaching-dispersive solid-phase extraction followed by dispersive liquid-liquid microextraction (USAL-DSPE-DLLME) technique has been developed as a new analytical approach for extracting, cleaning up and preconcentrating polybrominated diphenyl ethers (PBDEs) from sediment samples prior gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis. In the first place, PBDEs were leached from sediment samples by using acetone. This extract was cleaned-up by DSPE using activated silica gel as sorbent material. After clean-up, PBDEs were preconcentrated by using DLLME technique. Thus, 1 mL acetone extract (disperser solvent) and 60 microL carbon tetrachloride (extraction solvent) were added to 5 mL ultrapure water and a DLLME technique was applied. Several variables that govern the proposed technique were studied and optimized. Under optimum conditions, the method detection limits (MDLs) of PBDEs calculated as three times the signal-to-noise ratio (S/N) were within the range 0.02-0.06 ng g(-1). The relative standard deviations (RSDs) for five replicates were <9.8%. The calibration graphs were linear within the concentration range of 0.07-1000 ng g(-1) for BDE-47, 0.09-1000 ng g(-1) for BDE-100, 0.10-1000 ng g(-1) for BDE-99 and 0.19-1000 ng g(-1) for BDE-153 and the coefficients of estimation were > or =0.9991. Validation of the methodology was carried out by standard addition method at two concentration levels (0.25 and 1 ng g(-1)) and by comparing with a reference Soxhlet technique. Recovery values were > or =80%, which showed a satisfactory robustness of the analytical methodology for determination of low PBDEs concentration in sediment samples.

  19. Preparation of an additive-free sample with a MgH2 phase by planetary ball milling of Mg with10 wt% MgH2

    NASA Astrophysics Data System (ADS)

    Hong, Seong-Hyeon; Song, Myoung Youp

    2016-11-01

    In order to prepare an additive-free sample with a MgH2 phase, 90 wt% Mg+10 wt% MgH2 (named Mg-10MgH2) was milled under hydrogen atmosphere in a planetary ball mill for different durations (2 h, 5 h, and 10 h). The hydrogen absorption and release properties of the prepared samples were investigated and compared with those of purchased pure MgH2 samples. Mg-10MgH2 milled for 5 h had the largest quantity of hydrogen released at 648 K for 100 min of 5.96 wt%. Mg-10MgH2 milled for 5 h released 0.11 wt% H for 10 min, 4.85 wt% H for 30 min, and 5.83 wt% H for 60 min at 648 K at the first cycle. Mg-10MgH2 milled for 5 h absorbed 5.39 wt% H for 5 min and 5.92 wt% H for 60 min at 648 K at the second cycle. Dehydriding curves were also obtained at the first cycle of Mg-10MgH2 samples milled for 5 h using Mg powder with or without sieving (200 mesh). The dehydriding curve at 648 K of a Mg-10MgH2 sample milled for 5 h in the planetary ball mill was compared with that of the sample milled for 24 h in a horizontal ball mill.

  20. Deriving site-specific clean-up criteria to protect ecological receptors (plants and soil invertebrates) exposed to metal or metalloid soil contaminants via the direct contact exposure pathway

    PubMed Central

    Checkai, Ron; Van Genderen, Eric; Sousa, José Paulo; Stephenson, Gladys; Smolders, Erik

    2014-01-01

    Soil contaminant concentration limits for the protection of terrestrial plants and soil invertebrates are commonly based on thresholds derived using data from laboratory ecotoxicity tests. A comprehensive assessment has been made for the derivation of ecological soil screening levels (Eco-SSL) in the United States; however, these limits are conservative because of their focus on high bioavailability scenarios. Here, we explain and evaluate approaches to soil limit derivation taken by 4 jurisdictions, 2 of which allow for correction of data for factors affecting bioavailability among soils, and between spiked and field-contaminated soils (Registration Evaluation Authorisation and Restriction of Chemicals [REACH] Regulation, European Union [EU], and the National Environment Protection Council [NEPC], Australia). Scientifically advanced features from these methods have been integrated into a newly developed method for deriving soil clean-up values (SCVs) within the context of site-specific baseline ecological risk assessment. Resulting site-specific SCVs that account for bioavailability may permit a greater residual concentration in soil when compared to generic screening limit concentrations (e.g., Eco-SSL), while still affording acceptable protection. Two choices for selecting the level of protection are compared (i.e., allowing higher effect levels per species, or allowing a higher percentile of species that are potentially unprotected). Implementation of this new method is presented for the jurisdiction of the United States, with a focus on metal and metalloid contaminants; however, the new method can be used in any jurisdiction. A case study for molybdate shows the large effect of bioavailability corrections and smaller effects of protection level choices when deriving SCVs. Integr Environ Assess Manag 2014;10:346–357. PMID:24470189

  1. Deriving site-specific clean-up criteria to protect ecological receptors (plants and soil invertebrates) exposed to metal or metalloid soil contaminants via the direct contact exposure pathway.

    PubMed

    Checkai, Ron; Van Genderen, Eric; Sousa, José Paulo; Stephenson, Gladys; Smolders, Erik

    2014-07-01

    Soil contaminant concentration limits for the protection of terrestrial plants and soil invertebrates are commonly based on thresholds derived using data from laboratory ecotoxicity tests. A comprehensive assessment has been made for the derivation of ecological soil screening levels (Eco-SSL) in the United States; however, these limits are conservative because of their focus on high bioavailability scenarios. Here, we explain and evaluate approaches to soil limit derivation taken by 4 jurisdictions, 2 of which allow for correction of data for factors affecting bioavailability among soils, and between spiked and field-contaminated soils (Registration Evaluation Authorisation and Restriction of Chemicals [REACH] Regulation, European Union [EU], and the National Environment Protection Council [NEPC], Australia). Scientifically advanced features from these methods have been integrated into a newly developed method for deriving soil clean-up values (SCVs) within the context of site-specific baseline ecological risk assessment. Resulting site-specific SCVs that account for bioavailability may permit a greater residual concentration in soil when compared to generic screening limit concentrations (e.g., Eco-SSL), while still affording acceptable protection. Two choices for selecting the level of protection are compared (i.e., allowing higher effect levels per species, or allowing a higher percentile of species that are potentially unprotected). Implementation of this new method is presented for the jurisdiction of the United States, with a focus on metal and metalloid contaminants; however, the new method can be used in any jurisdiction. A case study for molybdate shows the large effect of bioavailability corrections and smaller effects of protection level choices when deriving SCVs.

  2. Determination of the rodenticides warfarin, diphenadione and chlorophacinone in soil samples by HPLC-DAD.

    PubMed

    Medvedovici, A; David, F; Sandra, P

    1997-09-01

    A HPLC-DAD method is described for the analysis of the rodenticides warfarin, diphenadione and chlorophacinone, together with the phenylurea herbicides isoproturon and diuron, in soil samples. The HPLC parameters have been optimised to provide baseline separation with symmetrical peakshapes in short analysis times. The sample preparation consists of Soxhlet extraction followed by SPE clean-up on cyanopropyl silica.

  3. Stochastic sampled-data control for synchronization of complex dynamical networks with control packet loss and additive time-varying delays.

    PubMed

    Rakkiyappan, R; Sakthivel, N; Cao, Jinde

    2015-06-01

    This study examines the exponential synchronization of complex dynamical networks with control packet loss and additive time-varying delays. Additionally, sampled-data controller with time-varying sampling period is considered and is assumed to switch between m different values in a random way with given probability. Then, a novel Lyapunov-Krasovskii functional (LKF) with triple integral terms is constructed and by using Jensen's inequality and reciprocally convex approach, sufficient conditions under which the dynamical network is exponentially mean-square stable are derived. When applying Jensen's inequality to partition double integral terms in the derivation of linear matrix inequality (LMI) conditions, a new kind of linear combination of positive functions weighted by the inverses of squared convex parameters appears. In order to handle such a combination, an effective method is introduced by extending the lower bound lemma. To design the sampled-data controller, the synchronization error system is represented as a switched system. Based on the derived LMI conditions and average dwell-time method, sufficient conditions for the synchronization of switched error system are derived in terms of LMIs. Finally, numerical example is employed to show the effectiveness of the proposed methods.

  4. Synchrotron-based FTIR microspectroscopy for the mapping of photo-oxidation and additives in acrylonitrile-butadiene-styrene model samples and historical objects.

    PubMed

    Saviello, Daniela; Pouyet, Emeline; Toniolo, Lucia; Cotte, Marine; Nevin, Austin

    2014-09-16

    Synchrotron-based Fourier transform infrared micro-spectroscopy (SR-μFTIR) was used to map photo-oxidative degradation of acrylonitrile-butadiene-styrene (ABS) and to investigate the presence and the migration of additives in historical samples from important Italian design objects. High resolution (3×3 μm(2)) molecular maps were obtained by FTIR microspectroscopy in transmission mode, using a new method for the preparation of polymer thin sections. The depth of photo-oxidation in samples was evaluated and accompanied by the formation of ketones, aldehydes, esters, and unsaturated carbonyl compounds. This study demonstrates selective surface oxidation and a probable passivation of material against further degradation. In polymer fragments from design objects made of ABS from the 1960s, UV-stabilizers were detected and mapped, and microscopic inclusions of proteinaceous material were identified and mapped for the first time.

  5. Additional evidence for morpho-dimensional tooth crown variation in a New Indonesian H. erectus sample from the Sangiran Dome (Central Java).

    PubMed

    Zanolli, Clément

    2013-01-01

    This contribution reports fifteen human fossil dental remains found during the last two decades in the Sangiran Dome area, in Central Java, Indonesia. Among this sample, only one of the specimens had already been briefly described, with the other fourteen remaining unreported. Seven of the fifteen isolated teeth were found in a secured stratigraphic context in the late Lower-early Middle Pleistocene Kabuh Formation. The remaining elements were surface finds which, based on coincidental sources of information, were inferred as coming from the Kabuh Formation. Mainly constituted of permanent molars, but also including one upper incisor and one upper premolar, this dental sample brings additional evidence for a marked degree of size variation and time-related structural reduction in Javanese H. erectus. This is notably expressed by a significant decrease of the mesiodistal diameter, frequently associated to the reduction or even loss of the lower molar distal cusp (hypoconulid) and to a more square occlusal outline. In addition to the hypoconulid reduction or loss, this new sample also exhibits a low frequency of the occlusal Y-groove pattern, with a dominance of the X and, to a lesser extent, of the+patterns. This combination is rare in the Lower and early Middle Pleistocene paleoanthropological record, including in the early Javanese dental assemblage from the Sangiran Dome. On the other hand, similar dental features are found in Chinese H. erectus and in H. heidelbergensis. As a whole, this new record confirms the complex nature of the intermittent exchanges that occurred between continental and insular Southeast Asia through the Pleistocene.

  6. Additional Evidence for Morpho-Dimensional Tooth Crown Variation in a New Indonesian H. erectus Sample from the Sangiran Dome (Central Java)

    PubMed Central

    Zanolli, Clément

    2013-01-01

    This contribution reports fifteen human fossil dental remains found during the last two decades in the Sangiran Dome area, in Central Java, Indonesia. Among this sample, only one of the specimens had already been briefly described, with the other fourteen remaining unreported. Seven of the fifteen isolated teeth were found in a secured stratigraphic context in the late Lower-early Middle Pleistocene Kabuh Formation. The remaining elements were surface finds which, based on coincidental sources of information, were inferred as coming from the Kabuh Formation. Mainly constituted of permanent molars, but also including one upper incisor and one upper premolar, this dental sample brings additional evidence for a marked degree of size variation and time-related structural reduction in Javanese H. erectus. This is notably expressed by a significant decrease of the mesiodistal diameter, frequently associated to the reduction or even loss of the lower molar distal cusp (hypoconulid) and to a more square occlusal outline. In addition to the hypoconulid reduction or loss, this new sample also exhibits a low frequency of the occlusal Y-groove pattern, with a dominance of the X and, to a lesser extent, of the+patterns. This combination is rare in the Lower and early Middle Pleistocene paleoanthropological record, including in the early Javanese dental assemblage from the Sangiran Dome. On the other hand, similar dental features are found in Chinese H. erectus and in H. heidelbergensis. As a whole, this new record confirms the complex nature of the intermittent exchanges that occurred between continental and insular Southeast Asia through the Pleistocene. PMID:23843996

  7. Effect of surfactant addition on ultrasonic leaching of trace elements from plant samples in inductively coupled plasma-atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Borkowska-Burnecka, Jolanta; Jankowiak, Urszula; Zyrnicki, Wieslaw; Anna Wilk, Kazimiera

    2004-04-01

    The applicability of surfactants in sample preparation of plant materials followed by analysis by inductively coupled plasma atomic emission spectrometry has been examined. Reference materials (INCT-MPH-2-Mixed Polish Herbs, INCT-TL-1 black tea leaves and CTA-VTL-2 -Virginia tobacco leaves) and commercially available tea leaves were analyzed. Effects of addition surfactants (Triton X-100, didodecyldimethylammonium bromide and cetyltrimethylammonium bromide) on efficiency of ultrasonic leaching of elements from the plant samples and on plasma parameters were investigated. Low concentrations of the surfactants in solutions did not affect, in practice, analytical line intensities and the nebulization process. Quantitative recovery of some elements could be obtained by ultrasonic diluted acid leaching with the aid of surfactants. However, the element recovery depended on type of surfactant, as well as element and sample material. Plasma parameters, i.e. the excitation temperatures of Ar I, Fe II and Ca II as well as the electron number density and the Mg II/Mg I intensity ratio did not vary significantly due to the surfactants in solutions.

  8. Features and machine learning classification of connected speech samples from patients with autopsy proven Alzheimer's disease with and without additional vascular pathology.

    PubMed

    Rentoumi, Vassiliki; Raoufian, Ladan; Ahmed, Samrah; de Jager, Celeste A; Garrard, Peter

    2014-01-01

    Mixed vascular and Alzheimer-type dementia and pure Alzheimer's disease are both associated with changes in spoken language. These changes have, however, seldom been subjected to systematic comparison. In the present study, we analyzed language samples obtained during the course of a longitudinal clinical study from patients in whom one or other pathology was verified at post mortem. The aims of the study were twofold: first, to confirm the presence of differences in language produced by members of the two groups using quantitative methods of evaluation; and secondly to ascertain the most informative sources of variation between the groups. We adopted a computational approach to evaluate digitized transcripts of connected speech along a range of language-related dimensions. We then used machine learning text classification to assign the samples to one of the two pathological groups on the basis of these features. The classifiers' accuracies were tested using simple lexical features, syntactic features, and more complex statistical and information theory characteristics. Maximum accuracy was achieved when word occurrences and frequencies alone were used. Features based on syntactic and lexical complexity yielded lower discrimination scores, but all combinations of features showed significantly better performance than a baseline condition in which every transcript was assigned randomly to one of the two classes. The classification results illustrate the word content specific differences in the spoken language of the two groups. In addition, those with mixed pathology were found to exhibit a marked reduction in lexical variation and complexity compared to their pure AD counterparts.

  9. Analysis of sequences from field samples reveals the presence of the recently described pepper vein yellows virus (genus Polerovirus) in six additional countries.

    PubMed

    Knierim, Dennis; Tsai, Wen-Shi; Kenyon, Lawrence

    2013-06-01

    Polerovirus infection was detected by reverse transcription polymerase chain reaction (RT-PCR) in 29 pepper plants (Capsicum spp.) and one black nightshade plant (Solanum nigrum) sample collected from fields in India, Indonesia, Mali, Philippines, Thailand and Taiwan. At least two representative samples for each country were selected to generate a general polerovirus RT-PCR product of 1.4 kb length for sequencing. Sequence analysis of the partial genome sequences revealed the presence of pepper vein yellows virus (PeVYV) in all 13 samples. A 1990 Australian herbarium sample of pepper described by serological means as infected with capsicum yellows virus (CYV) was identified by sequence analysis of a partial CP sequence as probably infected with a potato leaf roll virus (PLRV) isolate.

  10. FT-Raman and chemometric tools for rapid determination of quality parameters in milk powder: Classification of samples for the presence of lactose and fraud detection by addition of maltodextrin.

    PubMed

    Rodrigues Júnior, Paulo Henrique; de Sá Oliveira, Kamila; de Almeida, Carlos Eduardo Rocha; De Oliveira, Luiz Fernando Cappa; Stephani, Rodrigo; Pinto, Michele da Silva; de Carvalho, Antônio Fernandes; Perrone, Ítalo Tuler

    2016-04-01

    FT-Raman spectroscopy has been explored as a quick screening method to evaluate the presence of lactose and identify milk powder samples adulterated with maltodextrin (2.5-50% w/w). Raman measurements can easily differentiate samples of milk powder, without the need for sample preparation, while traditional quality control methods, including high performance liquid chromatography, are cumbersome and slow. FT-Raman spectra were obtained from samples of whole lactose and low-lactose milk powder, both without and with addition of maltodextrin. Differences were observed between the spectra involved in identifying samples with low lactose content, as well as adulterated samples. Exploratory data analysis using Raman spectroscopy and multivariate analysis was also developed to classify samples with PCA and PLS-DA. The PLS-DA models obtained allowed to correctly classify all samples. These results demonstrate the utility of FT-Raman spectroscopy in combination with chemometrics to infer about the quality of milk powder.

  11. Arsenic Remediation Enhancement Through Chemical Additions to Pump and Treat Operations

    NASA Astrophysics Data System (ADS)

    Wovkulich, K.; Mailloux, B. J.; Stute, M.; Simpson, H. J.; Keimowitz, A. R.; Powell, A.; Lacko, A.; Chillrud, S. N.

    2008-12-01

    Arsenic is a contaminant found at more than 500 US Superfund sites. Since pump and treat technologies are widely used for remediation of contaminated groundwater, increasing the efficiency of contaminant removal at such sites should allow limited financial resources to clean up more sites. The Vineland Chemical Company Superfund site is extensively contaminated with arsenic after waste arsenic salts were stored and disposed of improperly for much of the company's 44 year manufacturing lifetime. Despite approximately eight years of pump and treat remediation, arsenic concentrations in the recovery wells can still be greater than 1000 ppb. The arsenic concentrations in the groundwater remain high because of slow desorption of arsenic from contaminated aquifer solids. Extrapolation of laboratory column experiments suggest that continuing the current groundwater remediation practice based on flushing ambient groundwater through the system may require on the order of hundreds of years to clean the site. However, chemical additions of phosphate or oxalic acid into the aquifer could decrease the remediation time scale substantially. Laboratory results from a soil column experiment using input of 10 mM oxalic acid suggest that site clean up of groundwater could be decreased to as little as four years. Pilot scale forced gradient field experiments will help establish whether chemical additions can be effective for increasing arsenic mobilization from aquifer solids and thus substantially decrease pump and treat clean up time.

  12. Maps showing mines, quarries, oil and gas activity, and sample localities in and near the Sipsey Wilderness and additions, Lawrence and Winston Counties, Alabama

    SciTech Connect

    Mory, P.C.; Behum, P.T.; Ross, R.B. Jr.

    1982-01-01

    This report presents the results of a mineral survey of the Sipsey Wilderness and additions, William B. Bankhead National Forest, Lawrence and Winston Counties, Alabama. The survey includes: limestone quarrying, coal mining, and oil and gas activity. 7 references, 5 figures, 2 tables.

  13. Capillary electrophoretic separation of humic substances using hydroxyethyl cellulose as a buffer additive and its application to characterization of humic substances in a river water sample.

    PubMed

    Takahashi, Toru; Kawana, Jun; Hoshino, Hitoshi

    2009-01-01

    We have developed a concise tool for the investigation of the transition of humic substances in environmental water. The separation of water-soluble humic substances was achieved rapidly and effectively by capillary electrophoresis using a polyacrylamide-coated capillary and a phosphate electrophoretic buffer solution (pH 7.0) containing hydroxyethyl cellulose. The separation mechanism was assessed using the ultrafiltration technique. The effect of the complexation of humic substances with metal ions was studied by using the proposed method. When Fe(III) ions or EDTA was added to the sample solution of fulvic acid, a distinct change in the electropherogram pattern based on the conformational change of fulvic acid was observed. The successful application of the proposed method to the characterization of humic substances in a river water sample was also demonstrated.

  14. Additional notes on clinical repeated-dose pharmacokinetic trials applying a peak-and-trough sampling design to estimate oral clearance.

    PubMed

    Takaai, Mari; Kayano, Yuichiro; Shimizu, Takako; Taguchi, Masato; Hashimoto, Yukiya

    2008-01-01

    In the previous study, we performed a simulation of a clinical pharmacokinetic trial, in which blood was sampled at two time points corresponding to the peak concentration (C(peak)) and trough concentration (C(trough)) following repetitive oral administration at the dose, D, and dosing interval, tau. The approximate oral clearance (CL/F(approx)), estimated as 2 x D/(C(peak) x tau+C(trough) x tau), is accurate for drugs with an elimination half-life comparative to or longer than tau; however, it was suggested that we might not use CL/F(approx) for drugs with a considerably short elimination half-life relative to tau. In the present study, we evaluated the accuracy of the alternative oral clearance (CL/F(exp)) estimated by the simple monoexponential model. In contrast to CL/F(approx), CL/F(exp) was accurate for drugs with a short elimination half-life relative to tau. The present finding in conjunction with our previous study suggested that the peak-and-trough sampling design is promising for the clinical repeated-dose pharmacokinetic trial for drugs with not only slow but also rapid elimination from the body. We think that the accuracy and precision of the two analysis methods to estimate oral clearance (CL/F(approx) and CL/F(exp)) for a target drug should be evaluated carefully before and after a real clinical trial.

  15. Application of HPLC-DAD after SPE/QuEChERS with ZrO2-based sorbent in d-SPE clean-up step for pesticide analysis in edible oils.

    PubMed

    Tuzimski, Tomasz; Rejczak, Tomasz

    2016-01-01

    In this study, the solid-phase extraction/quick, easy, cheap, effective, rugged and safe (SPE/QuEChERS) technique was adapted to develop a simple sample treatment for multi-residue pesticide analysis of edible oils. The proposed method is based on liquid-liquid partitioning with acetonitrile followed by dispersive solid phase extraction using zirconia-coated silica particles for extract purification. To evaluate the described method, 21 pesticides belonging to different chemical classes were analysed using high performance liquid chromatography with diode-array detection (HPLC-DAD). For validation purposes, recovery studies were performed at 75 ng g(-1), 125 ng g(-1), 250 ng g(-1), 500 ng g(-1) and 1000 ng g(-1) levels. Recoveries were over the range of 50-130% for most of the analytes, with relative standard deviations less than 15% being observed. HPLC-DAD provided suitable linearity, precision and accuracy. The validated method was successfully applied to the analysis of edible oil samples selected from the market.

  16. Rapid optimized separation of bromide in serum samples with capillary zone electrophoresis by using glycerol as additive to the background electrolyte.

    PubMed

    Pascali, Jennifer P; Liotta, Eloisa; Gottardo, Rossella; Bortolotti, Federica; Tagliaro, Franco

    2009-04-10

    After decades of neglect, bromide has recently been re-introduced in therapy as an effective anti-epileptic drug. The present paper describes the methodological optimization and validation of a method based on capillary zone electrophoresis for the rapid determination of bromide in serum using a high-viscosity buffer and a short capillary (10 cm). The optimized running buffer was composed of 90 mM sodium tetraborate, 10mM sodium chloride, pH 9.24 and 25% glycerol. The separation was carried out at 25 kV at a temperature of 20 degrees C. Detection was by direct UV absorption at 200 nm wavelength. The limit of detection (signal-to-noise ratio=5) in serum was 0.017 mM. The precision of the method was verified in blank serum samples spiked with bromide, obtaining intra-day and day-to-day tests, relative standard deviation values

  17. Optimisation of a sample preparation method for the determination of fumonisin B(1) in rice.

    PubMed

    Petrarca, Mateus Henrique; Rodrigues, Maria Isabel; Rossi, Elizeu Antonio; de Sylos, Célia Maria

    2014-09-01

    A simple, rapid and cost-effective sample preparation method for the determination of fumonisin B1 in rice was optimised using a strategy of sequential experimental designs. Initially, a Plackett-Burman design was applied to select the statistically significant variables for the determination of fumonisin B1, and then, a central composite rotatable design was used to define the optimal conditions of these variables. The method involves extraction with a 50% acetonitrile aqueous solution and glacial acetic acid, liquid-liquid partitioning with addition of anhydrous sodium sulphate and sodium chloride, followed by dispersive SPE clean-up with diatomaceous earth. The final extract was analysed by HPLC-FLD after precolumn derivatisation with ortho-phthaldialdehyde. The optimised method was validated for selectivity, linearity, matrix effect, limits of detection and quantification, trueness, and precision, and then applied to commercial samples of polished rice. This is the first report of the occurrence of fumonisin B1 in commercial samples of polished rice from the Southeast region of Brazil.

  18. A new liquid chromatography-tandem mass spectrometry method for determination of parabens in human placental tissue samples.

    PubMed

    Jiménez-Díaz, I; Vela-Soria, F; Zafra-Gómez, A; Navalón, A; Ballesteros, O; Navea, N; Fernández, M F; Olea, N; Vílchez, J L

    2011-05-15

    Endocrine disruptors are a group of organic compounds widely used, which are ubiquitous in the environment and in biological samples. The main effect of these compounds is associated with their ability to mimic or block the action of natural hormones in living organisms, including humans. Parabens (esters of p-hydroxybenzoic acid) belong to this group of compounds. In this work, we propose a new liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to asses the presence of parabens most commonly used in industrial applications (methyl-, ethyl-, propyl- and butyl-paraben) in samples of human placental tissue. The method involves the extraction of the analytes from the samples using ethyl acetate, followed by a clean-up step using centrifugation prior to their quantification by LC-MS/MS using an atmospheric pressure chemical ionization (APCI) interface in the negative mode. Deuterated bisphenol A (BPA-d(16)) was used as surrogate. Found detection limits (LOD) ranged from 0.03 to 0.06 ng g(-1) and quantification limits (LOQ) from 0.1 to 0.2 ng g(-1), while inter- and intra-day variability was under 13.8%. The method was validated using standard addition calibration and a spike recovery assay. Recovery rates for spiked samples ranged from 82% to 108%. This method was satisfactorily applied for the determination of parabens in 50 placental tissue samples collected from women who live in the province of Granada (Spain).

  19. Food additives

    PubMed Central

    Spencer, Michael

    1974-01-01

    Food additives are discussed from the food technology point of view. The reasons for their use are summarized: (1) to protect food from chemical and microbiological attack; (2) to even out seasonal supplies; (3) to improve their eating quality; (4) to improve their nutritional value. The various types of food additives are considered, e.g. colours, flavours, emulsifiers, bread and flour additives, preservatives, and nutritional additives. The paper concludes with consideration of those circumstances in which the use of additives is (a) justified and (b) unjustified. PMID:4467857

  20. Cleaning up: Colleges Do Their Part to Revitalize the Gulf

    ERIC Educational Resources Information Center

    Violino, Bob

    2011-01-01

    When the deepwater horizon offshore oil drilling rig exploded in the Gulf of Mexico in April 2010, 11 crewmen were killed; the accident led to the largest oil spill in U.S. history. Forty workers on the rig managed to escape the catastrophe, thanks largely to a safety-training program they had taken at community colleges in the Louisiana Community…

  1. 48 CFR 52.236-12 - Cleaning Up.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... shall at all times keep the work area, including storage areas, free from accumulations of waste materials. Before completing the work, the Contractor shall remove from the work and premises any rubbish... completing the work, the Contractor shall leave the work area in a clean, neat, and orderly...

  2. 75 FR 62923 - WRC-07 Table Clean-up Order

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-10-13

    ... prelude to a rulemaking proceeding that the Commission anticipates initiating in the near future to... Federal use of certain mobile-satellite service (MSS) allocations to earth stations operating with non... changes that, in order to become effective in the United States, would need to be adopted in a...

  3. Cleaning up Trumpet Sound: Some Paths to Better Tone

    ERIC Educational Resources Information Center

    Zingara, James J.

    2004-01-01

    Of all the factors used to assess trumpet players, the one that distinguishes the established professional from the student is sound quality. While a good sound may be called "full," "rich," or "dark," poor sound is often described as "constricted," "tight," "thin," or "fuzzy." Although students' concept of good sound is important, many times…

  4. Bioenergy residues as novel sorbents to clean up pesticide pollution

    NASA Astrophysics Data System (ADS)

    Mukherjee, Santanu

    2016-04-01

    Worldwide, water contamination from agricultural use of pesticides has received increasing attention within the last decades. In general, sources of pesticide water pollution are categorized into diffuse (stemming from treated fields) and point sources (stemming from farmyards and spillages). Research has demonstrated that 40 to 90% of surface water pesticide contamination is due to point source pollution. To reduce point pollution from farm yards, where the spray equipment is washed, biobed or biofilter systems are used to treat the washing water. The organic material usually used in these systems is often not environmentally sustainable (e.g. peat) and incorporated organic material such as straw leads to a highly heterogeneous water flow, with negative effects on the retention and degradation behavior of the pesticides. Therefore, the objective of this study was to assess the suitability of alternative materials based on bioenergy residues (biochar and digestate) for use in biofilters. To this aim the sorption-desorption potential of three contrasting pesticides (bentazone, boscalid, and pyrimethanil) on mixtures of soil with digestate and/or biochar were investigated in laboratory batch equilibrium experiments. The results indicate that the mixture of digestate and biochar increased pesticide sorption potential, whereby in all cases, the Kd des / Kf des values were lower than the Kd ads / Kf ads values indicating that the retention of the pesticides was weak. Thus, as Kf des were lower than the Kf ads values and H values were below 1, it can be concluded that the biomixtures presented negative desorption (higher hysteresis) in those cases. A higher Kd (>78 L kg-1), Kf (>400 μM1-1/nf L1/nfkg-1) and KL (>40 L kg-1) was obtained for all pesticides for the digestate and biochar based mixtures, which had a higher organic matter content. However, lower sorption of the pesticides was observed in blank soil compared to the other biomixtures, which was attributed to the lower organic carbon content of the blank soil. Our results showed that boscalid and pyrimethanil are highly sorbed to the mixture of digestate and biochar. SUVA254 values justified the aromatic character of digestate (5%) and biochar (5%) mixture which showed highest Koc values among all mixtures for all pesticides. This mixture was found to be the most promising substrate amongst the tested ones for a biobed setup and can be used as an effective and alternative adsorbent for removing pesticides, because of its higher adsorption capacity.

  5. Training Workers for Environmental Clean-Up Jobs.

    ERIC Educational Resources Information Center

    Baldwin, Fred

    1993-01-01

    Describes the International Union of Operating Engineers (IUOE) Hazmat Training Program (Beckley, WV). It is the largest program in the nation for training skilled workers to safely handle toxic and hazardous wastes. This program has produced more than 450 certified instructors, who, in turn, have trained more than 18,000 workers. (LP)

  6. Renewable Natural Gas Clean-up Challenges and Applications

    DTIC Science & Technology

    2011-01-13

    produced from digesters ─ Animal manure (dairy cows, swine) ─ Waste water treatment facilities > Methane from Landfills > RNG produced from...AGR used in process • Two stage + trim methanation reactor • Dehydration to achieve gas pipeline specifications ~ 70% conversion efficiency 21... digestion of agricultural waste for on-site electricity generation ─Altamont Landfill—Landfill gas (LFG) cleanup for production of liquefied natural gas

  7. Working with Communities on Cleaning Up Abandoned Uranium Mines

    EPA Pesticide Factsheets

    This site provides information about the EPA's work to inform and include communities in the cleanup of abandoned mines, including health impacts, major enforcement and removal milestones, and community actions.

  8. MSO spent salt clean-up recovery process

    SciTech Connect

    Adamson, M G; Brummond, W A; Hipple, D L; Hsu, P C; Summers, L J; Von Holtz, E H; Wang, F T

    1997-02-01

    An effective process has been developed to separate metals, mineral residues, and radionuclides from spent salt, a secondary waste generated by Molten Salt Oxidation (MSO). This process includes salt dissolution, pH adjustment, chemical reduction and/or sulfiding, filtration, ion exchange, and drying. The process uses dithionite to reduce soluble chromate and/or sulfiding agent to suppress solubilities of metal compounds in water. This process is capable of reducing the secondary waste to less than 5% of its original weight. It is a low temperature, aqueous process and has been demonstrated in the laboratory [1].

  9. Colorado court involvement in chemical spill clean-up activities.

    PubMed Central

    Rice, D

    1981-01-01

    Judicial involvement was utilized to force the owners of a pesticide formulation plant to decontaminate property that had been covered with toxic pesticides having the potential to contaminate both surface and groundwater supplies in the East Denver metropolitan area. This case represented the first use of the Colorado state court system in dealing with a hazardous waste "spill." In this case, judicial intervention was unsatisfactory because of the delays involved. Other courses of action will be considered in future cases of a similar nature. PMID:7270771

  10. Cleaning up contaminated wood-treating sites. Background paper

    SciTech Connect

    1995-09-01

    This report identifies technologies available for organic hazardous waste cleanup at woodtreating sites throughout the country. OTA has identified a range of such technologies that have been selected in the past and could be applied to other sites in the future. The applicability of a technology to a particular Superfund site has to be based on many site-specific factors. Nevertheless, it is clear that a number of the approaches identified by OTA may be appropriate and could prove useful if more detailed site-specific studies and tests were done. Although this study focused on the Texarkana site, decisionmakers and the public could benefit from this analysis in selecting future cleanup strategies for other sites.

  11. News from Online: Cleaning Up--Soap, Detergent, and More.

    ERIC Educational Resources Information Center

    Judd, Carolyn Sweeney

    2002-01-01

    Provides a guide to web resources on cleaning and hygiene. Answers the questions, What do you want to clean--your hair? your carpet? your rusty lawn furniture? Develops special products for different tasks. Focuses on products to use and the environmental impact of our choices. (MM)

  12. With Awards and Recognition, Our Custodians Really Clean Up.

    ERIC Educational Resources Information Center

    Holayter, Marlene C.

    1990-01-01

    Describes a motivational program in the Fairfax County (Virginia) Public Schools that caused a dramatic improvement in custodial staff professionalism and school building cleanliness. The plan emphasized the importance of clean schools, teamwork, and accepting responsibility for one's work. (MLH)

  13. Wet-air oxidation cleans up black wastewater

    SciTech Connect

    Not Available

    1993-09-01

    Sterling Organics produces the analgesic paracetamol (acetaminophen) at its Dudley, England, plant. The wastewater from the batch process contains intermediates such as para-aminophenol (PAP) and byproducts such as thiosulfates, sulfites and sulfides. To stay ahead of increasingly strict environmental legislation, Sterling Organics installed a wet-air oxidation system at the Dudley facility in August 1992. The system is made by Zimpro Environmental Inc. (Rothschild, Wis.). Zimpro's wet-air oxidation system finds a way around the limitations of purely chemical or physical processes. In the process, compressed air at elevated temperature and pressure oxidizes the process intermediates and byproducts and removes the color from the wastewater.

  14. Colorado court involvement in chemical spill clean-up activities.

    PubMed

    Rice, D

    1981-09-01

    Judicial involvement was utilized to force the owners of a pesticide formulation plant to decontaminate property that had been covered with toxic pesticides having the potential to contaminate both surface and groundwater supplies in the East Denver metropolitan area. This case represented the first use of the Colorado state court system in dealing with a hazardous waste "spill." In this case, judicial intervention was unsatisfactory because of the delays involved. Other courses of action will be considered in future cases of a similar nature.

  15. Technical Support Project for Cleaning Up Contaminated Sites - Expertise Directory

    EPA Pesticide Factsheets

    This directory is searchable and provides a snapshot of the various types of expertise possessed by the current members of the three Technical Support Project forums. It is based on input provided by the members themselves.

  16. Cleaning Up the Seas. UNEP Environment Brief No. 5.

    ERIC Educational Resources Information Center

    United Nations Environment Programme, Nairobi (Kenya).

    While the open oceans remain relatively unpolluted, many coastal areas are suffering from oil, sewage, industrial wastes, and agricultural run-off. This document presents some of the key facts related to these kinds of water pollution. It focuses on the major sources of contamination in the world's seas, and provides an overview of how these…

  17. Beyond Symbiosis: Cleaner Shrimp Clean Up in Culture

    PubMed Central

    Militz, Thane A.; Hutson, Kate S.

    2015-01-01

    Cleaner organisms exhibit a remarkable natural behaviour where they consume ectoparasites attached to “client” organisms. While this behaviour can be utilized as a natural method of parasitic disease control (or biocontrol), it is not known whether cleaner organisms can also limit reinfection from parasite eggs and larvae within the environment. Here we show that cleaner shrimp, Lysmata amboinensis, consume eggs and larvae of a harmful monogenean parasite, Neobenedenia sp., in aquaculture. Shrimp consumed parasite eggs under diurnal (63%) and nocturnal (14%) conditions as well as infectious larvae (oncomiracidia) diurnally (26%). Furthermore, we trialled the inclusion of cleaner shrimp for preventative parasite management of ornamental fish, Pseudanthias squamipinnis, and found shrimp reduced oncomiracidia infection success of host fish by half compared to controls (held without shrimp). Fish held without cleaner shrimp exhibited pigmentation changes as a result of infection, possibly indicative of a stress response. These results provide the first empirical evidence that cleaner organisms reduce parasite loads in the environment through non-symbiotic cleaning activities. Our research findings have relevance to aquaculture and the marine ornamental trade, where cleaner shrimp could be applied for prophylaxis and control of ectoparasite infections. PMID:25706952

  18. Let's Stop Talking Medicine and Clean Up the Water.

    ERIC Educational Resources Information Center

    Webster, William

    1987-01-01

    Although California ranked sixth in 1983 per capita income, the state ranks 23rd in 1984-85 public school expenditures per pupil and 50th in student-teacher ratios. To address underfunding and class size problems, a Trust Fund for School Improvement is needed to coordinate fragmented funding sources for well-planned local projects. Included are 10…

  19. Cleaning up That Mess: A Framework for Classifying Educational Apps

    ERIC Educational Resources Information Center

    Cherner, Todd; Dix , Judy; Lee, Corey

    2014-01-01

    As tablet technologies continue to evolve, the emergence of educational applications (apps) is impacting the work of teacher educators. Beyond online lists of best apps for education and recommendations from colleagues, teacher educators have few resources available to support their teaching of how to select educational apps. In response, this…

  20. The 7% Solution - Cleaning Up After Fred Vine's Outstanding Successes

    NASA Astrophysics Data System (ADS)

    Hey, R. N.

    2013-12-01

    Fred Vine was the first & greatest of the wiggle pickers, founding the marine magnetic anomaly field with his 1963 Vine & Matthews paper. Two of his classic study areas were Juan de Fuca & the Reykjanes Ridge. In Juan de Fuca, he recognized the axial symmetry in the Raff & Mason data that had shown the existence of magnetic stripes on the seafloor, demonstrating the seafloor spreading there that Tuzo Wilson had predicted. Fred's iconic color figure of these anomalies perfectly correlated with the magnetic reversal time scale (after the discovery of the Jaramillo event) became the striking cover illustration of 'The History of the Earth's Crust', the symposium volume of the influential 1966 Goddard meeting that confirmed the reality of seafloor spreading & continental drift. Everything Fred did in Juan de Fuca was correct, but fortunately for me he didn't do everything. Some of the linear magnetic anomaly offsets there became a major puzzle in 1967 when Jason Morgan & Dan McKenzie discovered plate tectonics, because those offsets were oblique to the ridges & transforms & thus were incompatible with simple plate tectonics. Although the oblique anomaly offsets look like faults, they instead turned out to be propagating rift pseudofault wakes with no relative motion along them, an interpretation resulting from my analysis of Galapagos magnetic anomalies. Fred's other iconic color figure was his correlation of the Heirtzler et al. Reykjanes Ridge aeromagnetic data with the reversal timescale. This figure, showing the symmetry predicted by seafloor spreading & field reversals, was another key step in the scientific revolution. At the Goddard Symposium Fred was asked if he'd tested the symmetry statistically & he replied "I never touch statistics. I just deal with the facts'. Fred was trying to have a scientific revolution, & of course on that scale pretty symmetric seafloor spreading is a reality. However, fine-scale asymmetric spreading can be seen in his figure (the asymmetry increases towards Iceland where we had the great advantage of working), & contrary to conventional wisdom the V-shaped ridges, scarps & troughs (VSRs) discovered by Peter Vogt are not symmetric about the Reykjanes Ridge axis. Analysis of magnetic anomaly data from our 2007 expedition by Benediktsdóttir et al. shows these asymmetries were created by rift propagation both away from & towards Iceland, suggesting a tectonic alternative to the magmatic pulsing plume explanation for the VSRs. These results further suggest that the massive transform-eliminating North Atlantic plate boundary reorganization that created the linear obliquely-spreading Reykjanes Ridge might also be a propagating rift phenomenon instead of a thermal phenomenon as generally assumed, & we hope to present results from a new Reykjanes Ridge expedition later this summer designed to determine exactly how this reorganization is occurring. That so much research for several decades has resulted from the small (the 7% number in the title is made up - inspired by Fred I never did learn statistics) modification of Fred's results is a tribute to the overwhelming success of seafloor spreading & plate tectonics. Unfortunately for Vine, Morgan & McKenzie, this scientific revolution appears to have been too profound for Nobel Prizes.

  1. Making Use of Manure for a Clean-Up Job

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Wastes should no longer be wasted. This article describes how animal manure can be utilized by converting it into activated carbons. These activated carbons are then utilized to adsorb unwanted pollutants because of their high porosity. The animal manure will eventually help to remove odors from dr...

  2. Novel Sorbent to Clean Up Biogas for CHPs

    SciTech Connect

    Alptekin, Gökhan O.; Jayataman, Ambalavanan; Schaefer, Matthew; Ware, Michael; Hunt, Jennifer; Dobek, Frank

    2015-05-30

    In this project, TDA Research Inc. (TDA) has developed low-cost (on a per unit volume of gas processed basis), high-capacity expendable sorbents that can remove both the H2S and organic sulfur species in biogas to the ppb levels. The proposed sorbents will operate downstream of a bulk desulfurization system as a polishing bed to provide an essentially sulfur-free gas to a fuel cell (or any other application that needs a completely sulfur-free feed). Our sorbents use a highly dispersed mixed metal oxides active phase with desired modifiers prepared over on a mesoporous support. The support structure allows the large organic sulfur compounds (such as the diethyl sulfide and dipropyl sulfide phases with a large kinetic diameter) to enter the sorbent pores so that they can be adsorbed and removed from the gas stream.

  3. Beyond symbiosis: cleaner shrimp clean up in culture.

    PubMed

    Militz, Thane A; Hutson, Kate S

    2015-01-01

    Cleaner organisms exhibit a remarkable natural behaviour where they consume ectoparasites attached to "client" organisms. While this behaviour can be utilized as a natural method of parasitic disease control (or biocontrol), it is not known whether cleaner organisms can also limit reinfection from parasite eggs and larvae within the environment. Here we show that cleaner shrimp, Lysmata amboinensis, consume eggs and larvae of a harmful monogenean parasite, Neobenedenia sp., in aquaculture. Shrimp consumed parasite eggs under diurnal (63%) and nocturnal (14%) conditions as well as infectious larvae (oncomiracidia) diurnally (26%). Furthermore, we trialled the inclusion of cleaner shrimp for preventative parasite management of ornamental fish, Pseudanthias squamipinnis, and found shrimp reduced oncomiracidia infection success of host fish by half compared to controls (held without shrimp). Fish held without cleaner shrimp exhibited pigmentation changes as a result of infection, possibly indicative of a stress response. These results provide the first empirical evidence that cleaner organisms reduce parasite loads in the environment through non-symbiotic cleaning activities. Our research findings have relevance to aquaculture and the marine ornamental trade, where cleaner shrimp could be applied for prophylaxis and control of ectoparasite infections.

  4. Simultaneous determination of methyl tert-butyl ether, its degradation products and other gasoline additives in soil samples by closed-system purge-and-trap gas chromatography-mass spectrometry.

    PubMed

    Rosell, Mònica; Lacorte, Sílvia; Barceló, Damià

    2006-11-03

    A new protocol for the simultaneous determination of methyl tert-butyl ether (MTBE); its main degradation products: tert-butyl alcohol (TBA) and tert-butyl formate (TBF); other gasoline additives, oxygenate dialkyl ethers: ethyl tert-butyl ether (ETBE), tert-amyl methyl ether (TAME) and diisopropyl ether (DIPE); aromatics: benzene, toluene, ethylbenzene and xylenes (BTEX) and other compounds causing odour events such as dicyclopentadiene (DCPD) and trichloroethylene (TCE) in soils has been developed. On the basis of US Environmental Protection Agency (EPA) method 5035A, a fully automated closed-system purge-and-trap coupled to gas chromatography/mass spectrometry (P&T-GC/MS) was optimised and permitted to detect microg/kg concentrations in solid matrices avoiding losses of volatile compounds during operation processes. Parameters optimised were the sampling procedure, sample preservation and storage, purging temperature, matrix effects and quantification mode. Using 5 g of sample, detection limits were between 0.02 and 1.63 microg/kg and acceptable method precision and accuracy was obtained provided quantification was performed using adequate internal standards. Soil samples should be analysed as soon as possible after collection, stored under -15 degrees C for not longer than 7 days if degradation products have to be analysed. The non-preservative alternative (empty vial) provided good recoveries of the most analytes when freezing the samples up to 7 day holding time, however, if biologically active soil are analysed the preservation with trisodium phosphate dodecahydrate (Na(3)PO(4).12H(2)O or TSP) is strongly recommended more than sodium bisulphate (NaHSO(4)). The method was finally applied to provide threshold and background levels of several gasoline additives in a point source and in sites not influenced by gasoline spills. The proposed method provides the directions for the future application on real samples in current monitoring programs at gasoline

  5. Combining Electrochemical Sensors with Miniaturized Sample Preparation for Rapid Detection in Clinical Samples

    PubMed Central

    Bunyakul, Natinan; Baeumner, Antje J.

    2015-01-01

    Clinical analyses benefit world-wide from rapid and reliable diagnostics tests. New tests are sought with greatest demand not only for new analytes, but also to reduce costs, complexity and lengthy analysis times of current techniques. Among the myriad of possibilities available today to develop new test systems, amperometric biosensors are prominent players—best represented by the ubiquitous amperometric-based glucose sensors. Electrochemical approaches in general require little and often enough only simple hardware components, are rugged and yet provide low limits of detection. They thus offer many of the desirable attributes for point-of-care/point-of-need tests. This review focuses on investigating the important integration of sample preparation with (primarily electrochemical) biosensors. Sample clean up requirements, miniaturized sample preparation strategies, and their potential integration with sensors will be discussed, focusing on clinical sample analyses. PMID:25558994

  6. Food additives

    MedlinePlus

    ... or natural. Natural food additives include: Herbs or spices to add flavor to foods Vinegar for pickling ... Certain colors improve the appearance of foods. Many spices, as well as natural and man-made flavors, ...

  7. Direct sampling MS for environmental screening

    SciTech Connect

    Wise, M.B.; Guerin, M.R.

    1997-01-01

    Decades of improper storage and disposal of hazardous materials by government and industry have resulted in =40,000 contaminated sites that will require cleanup by state and federal agencies. Almost 1,300 of these sites are classified as especially serious threats and are listed on the Superfund National Priorities List (NPL) for accelerated remediation; by 2020, it is estimated that the number of NPL sites will exceed 3,000. Given that an average of 10 years is required to clean up a superfund site, remediation of known hazardous sites will continue well into the next century. Cost projections for environmental restoration range from nearly $200 billion to more than $2 trillion. DSMS is a simple technique that provides real-time response, high sample throughput, and ppb detection limits at low cost. This paper discusses screening methods and direct sampling MS (DSMS) for more cost-effective and efficient environmental characterization. 18 refs., 2 figs., 1 tab.

  8. Non-PBDE halogenated flame retardants in Canadian indoor house dust: sampling, analysis, and occurrence.

    PubMed

    Fan, Xinghua; Kubwabo, Cariton; Rasmussen, Pat E; Wu, Fang

    2016-04-01

    An analytical method was developed for the measurement of 18 novel halogenated flame retardants in house dust. Sample preparation was based on ultrasound-assisted solvent extraction and clean up with solid phase extraction (SPE). Sample extracts were analyzed by gas chromatography-mass spectrometry (GC/MS) operated in electron capture negative ion (ECNI) chemical ionization mode. Baseline data from 351 fresh (active) dust samples collected under the Canadian House Dust Study (CHDS) revealed that five out of 18 target chemicals were present with detection frequencies higher than 90 %. Median (range) concentrations for these five compounds were as follows: 104 (<1.5-13,000) ng/g for 2-ethylhexyl-2,3,4,5-tetrabromobenzoate (EHTBB), 8.5 (<1.7-2390) ng/g for 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE), 10.2 (<1.7-430) ng/g for hexabromobenzene (HBB), 2.9 (<1.2-1410) ng/g for syn-dechlorane plus (syn-DP) and 5.6 (<1.9-1570) ng/g for anti-dechlorane plus (anti-DP). A comparison of two sampling methods in a subset of 40 homes showed significant positive correlations between samples of "active" dust and samples taken directly from the household vacuum cleaner for all target compounds having median values above their corresponding method detection limits (MDLs). In addition, the method was also applied to the analysis of the targeted compounds in National Institute of Standards and Technology (NIST) standard reference material (SRM 2585, organic contaminants in house dust). Results from the current study could contribute to the potential certification of target chemicals in SRM 2585.

  9. RECOMMENDATIONS FOR SAMPLING OF TANK 18 IN F TANK FARM

    SciTech Connect

    Shine, G.

    2009-12-14

    Representative sampling is required for characterization of the residual floor material in Tank 18 prior to operational closure. Tank 18 is an 85-foot diameter, 34-foot high carbon steel tank with nominal operating volume of 1,300,000 gallons. It is a Type IV tank, and has been in service storing radioactive materials since 1959. Recent mechanical cleaning of the tank removed all mounds of material. Anticipating a low level of solids in the residual material, Huff and Thaxton [2009] developed a plan to sample the material during the final clean-up process while it would still be resident in sufficient quantities to support analytical determinations in four quadrants of the tank. Execution of the plan produced fewer solids than expected to support analytical determinations in all four quadrants. Huff and Thaxton [2009] then restructured the plan to characterize the residual floor material separately in the North and the South regions: two 'hemispheres.' This document provides sampling recommendations to complete the characterization of the residual material on the tank bottom following the guidance in Huff and Thaxton [2009] to split the tank floor into a North and a South hemisphere. The number of samples is determined from a modification of the formula previously published in Edwards [2001] and the sample characterization data for previous sampling of Tank 18 described by Oji [2009]. The uncertainty is quantified by an upper 95% confidence limit (UCL95%) on each analyte's mean concentration in Tank 18. The procedure computes the uncertainty in analyte concentration as a function of the number of samples, and the final number of samples is determined when the reduction in the uncertainty from an additional sample no longer has a practical impact on results. The characterization of the full suite of analytes in the North hemisphere is currently supported by a single Mantis rover sample obtained from a compact region near the center riser. A floor scrape sample was

  10. Sources of Technical Variability in Quantitative LC-MS Proteomics: Human Brain Tissue Sample Analysis.

    SciTech Connect

    Piehowski, Paul D.; Petyuk, Vladislav A.; Orton, Daniel J.; Xie, Fang; Moore, Ronald J.; Ramirez Restrepo, Manuel; Engel, Anzhelika; Lieberman, Andrew P.; Albin, Roger L.; Camp, David G.; Smith, Richard D.; Myers, Amanda J.

    2013-05-03

    To design a robust quantitative proteomics study, an understanding of both the inherent heterogeneity of the biological samples being studied as well as the technical variability of the proteomics methods and platform is needed. Additionally, accurately identifying the technical steps associated with the largest variability would provide valuable information for the improvement and design of future processing pipelines. We present an experimental strategy that allows for a detailed examination of the variability of the quantitative LC-MS proteomics measurements. By replicating analyses at different stages of processing, various technical components can be estimated and their individual contribution to technical variability can be dissected. This design can be easily adapted to other quantitative proteomics pipelines. Herein, we applied this methodology to our label-free workflow for the processing of human brain tissue. For this application, the pipeline was divided into four critical components: Tissue dissection and homogenization (extraction), protein denaturation followed by trypsin digestion and SPE clean-up (digestion), short-term run-to-run instrumental response fluctuation (instrumental variance), and long-term drift of the quantitative response of the LC-MS/MS platform over the 2 week period of continuous analysis (instrumental stability). From this analysis, we found the following contributions to variability: extraction (72%) >> instrumental variance (16%) > instrumental stability (8.4%) > digestion (3.1%). Furthermore, the stability of the platform and its’ suitability for discovery proteomics studies is demonstrated.

  11. Comparison of UV absorption and electrospray mass spectrometry for the high-performance liquid chromatographic determination of domoic acid in shellfish and biological samples.

    PubMed

    Lawrence, J F; Lau, B P; Cleroux, C; Lewis, D

    1994-01-21

    Domoic acid, a neurotoxic amino acid produced by the marine diatom Nitchia pungens multiseries, was determined in samples of anchovies, razor clams, mussels, crab, rat serum, urine and feces by HPLC with UV absorption and electrospray (ESI) mass spectrometric (MS) detection. Shellfish samples were extracted with methanol-water followed by clean-up of the extracts with solid-phase extraction cartridges (strong anion or strong cation exchange). An aliquot of the fraction containing the domoic acid was analysed by HPLC. HPLC column size, mobile phase composition and flow-rate were selected so that essentially the same conditions could be used for both HPLC-UV and HPLC-ESI-MS with selected ion monitoring (SIM) determinations. These included the use of acetonitrile-water-formic acid as the mobile phase, at a flow-rate of 0.2 ml/min (split 13:1 for HPLC-ESI-MS-SIM, 10 microliters/min to the mass spectrometer). The results indicated that extracts found positive by the HPLC-UV method could be readily confirmed directly by HPLC-ESI-MS-SIM without additional sample treatment down to levels of 0.1 micrograms/g of domoic acid. This study demonstrates the use of HPLC-ESI-MS-SIM for the routine confirmation of domoic acid in a wide variety of samples.

  12. Comparison of sample preparation strategies for target analysis of total thyroid hormones levels in serum by liquid chromatography-quadrupole time-of-flight-mass spectrometry.

    PubMed

    Álvarez, E; Madrid, Y; Marazuela, M D

    2017-03-01

    This paper describes a novel method based on liquid chromatography quadrupole time-of-flight-mass spectrometry (LC-QTOF-MS) for target analysis of total THs in serum. Several sample preparation strategies have been evaluated to reduce matrix effect (namely, HybridSPE cartridges, supported liquid extraction, SLE and solid phase extraction, SPE). Deproteinization and further clean-up with mixed-mode SPE was selected as the best strategy for sample preparation, since achieved the cleanest extracts and reduced ionization suppression effects (between -11 and -24%). Method validation was performed by the analysis of control human serum samples. Criteria for confirming THs identity in serum extracts were based on retention times, accurate masses, isotopic pattern and MS/MS fragmentation pattern. Moreover, the quantitation capabilities of the LC-QTOF-MS method were also evaluated in terms of linearity, precision, accuracy and sensitivity by the application of matrix-matched calibration. Additionally, the developed LC-QTOF-MS method successfully provides qualitative information on endogenous components responsible of ion suppression (e.g. lysophosphatidylcholines), via post acquisition data analysis. This demonstrates the significant advantage of using LC-QTOF-MS, as it allows retrospective querying of the acquired data without the need of re-injecting/re-processing the samples.

  13. Potlining Additives

    SciTech Connect

    Rudolf Keller

    2004-08-10

    In this project, a concept to improve the performance of aluminum production cells by introducing potlining additives was examined and tested. Boron oxide was added to cathode blocks, and titanium was dissolved in the metal pool; this resulted in the formation of titanium diboride and caused the molten aluminum to wet the carbonaceous cathode surface. Such wetting reportedly leads to operational improvements and extended cell life. In addition, boron oxide suppresses cyanide formation. This final report presents and discusses the results of this project. Substantial economic benefits for the practical implementation of the technology are projected, especially for modern cells with graphitized blocks. For example, with an energy savings of about 5% and an increase in pot life from 1500 to 2500 days, a cost savings of $ 0.023 per pound of aluminum produced is projected for a 200 kA pot.

  14. Phosphazene additives

    DOEpatents

    Harrup, Mason K; Rollins, Harry W

    2013-11-26

    An additive comprising a phosphazene compound that has at least two reactive functional groups and at least one capping functional group bonded to phosphorus atoms of the phosphazene compound. One of the at least two reactive functional groups is configured to react with cellulose and the other of the at least two reactive functional groups is configured to react with a resin, such as an amine resin of a polycarboxylic acid resin. The at least one capping functional group is selected from the group consisting of a short chain ether group, an alkoxy group, or an aryloxy group. Also disclosed are an additive-resin admixture, a method of treating a wood product, and a wood product.

  15. Gas-liquid chromatographic and gas-liquid-mass spectometric determination of fenvalerate and permethrin residues in grasshoppers and duck tissue samples

    USGS Publications Warehouse

    Reichel, W.L.; Kolbe, E.J.; Stafford, C.J.

    1981-01-01

    A procedure is described for determining fenvalerate and permethrin residues in grasshoppers and duck tissues. Samples are Soxhlet-extracted with hexane and cleaned up by gel permeation chromatography with an in-line alumina column. Samples are analyzed by gas-liquid chromatography with electron capture detection, and confirmed by gas-liquid chromatography-mass spectrometry. The average recovery from fortified tissues was 97%.

  16. Rapid extraction and reverse phase-liquid chromatographic separation of mercury(II) and methylmercury in fish samples with inductively coupled plasma mass spectrometric detection applying oxygen addition into plasma.

    PubMed

    Döker, Serhat; Boşgelmez, İffet İpek

    2015-10-01

    A simple and sensitive procedure was developed for extraction and speciation of mercury in fish. Species separation was accomplished with reverse phase-high performance liquid chromatography (HPLC) hyphenated to inductively coupled plasma mass spectrometry (ICP-MS). Oxygen addition into plasma allowed use of organic-rich mobile phase, achieving species separation in 4 min. Mercury species extraction was achieved by microwave exposure for 2 min at mild conditions (60°C, pH 2.0), avoiding necessity of neutralizing sample prior to injection in HPLC, and reducing number of sample preparation steps, analytical source of errors and inter conversion of species. Limit of detection for entire procedure was found to be 0.2 and 0.1 ng g(-1) for mercuric ion and methylmercury, respectively. The method was applied to certified reference materials (TORT-2 and DORM-2) and commercialized fish samples (Mullus barbatus, Sparus aurata, Trachurus mediterraneus, Mugil soiuy, Dicentrarchus labrax, and Pomatomus saltatrix) from Black Sea.

  17. 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.

    PubMed

    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 C18 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.

  18. RECOMMENDATIONS FOR SAMPLING OF TANK 19 IN F TANK FARM

    SciTech Connect

    Harris, S.; Shine, G.

    2009-12-14

    Representative sampling is required for characterization of the residual material in Tank 19 prior to operational closure. Tank 19 is a Type IV underground waste storage tank located in the F-Tank Farm. It is a cylindrical-shaped, carbon steel tank with a diameter of 85 feet, a height of 34.25 feet, and a working capacity of 1.3 million gallons. Tank 19 was placed in service in 1961 and initially received a small amount of low heat waste from Tank 17. It then served as an evaporator concentrate (saltcake) receiver from February 1962 to September 1976. Tank 19 also received the spent zeolite ion exchange media from a cesium removal column that once operated in the Northeast riser of the tank to remove cesium from the evaporator overheads. Recent mechanical cleaning of the tank removed all mounds of material. Anticipating a low level of solids in the residual waste, Huff and Thaxton [2009] developed a plan to sample the waste during the final clean-up process while it would still be resident in sufficient quantities to support analytical determinations in four quadrants of the tank. Execution of the plan produced fewer solids than expected to support analytical determinations in all four quadrants. Huff and Thaxton [2009] then restructured the plan to characterize the residual separately in the North and the South regions: two 'hemispheres.' This document provides sampling recommendations to complete the characterization of the residual material on the tank bottom following the guidance in Huff and Thaxton [2009] to split the tank floor into a North and a South hemisphere. The number of samples is determined from a modification of the formula previously published in Edwards [2001] and the sample characterization data for previous sampling of Tank 19 described by Oji [2009]. The uncertainty is quantified by an upper 95% confidence limit (UCL95%) on each analyte's mean concentration in Tank 19. The procedure computes the uncertainty in analyte concentration as a

  19. An electrochemical magneto immunosensor (EMIS) for the determination of paraquat residues in potato samples.

    PubMed

    Garcia-Febrero, Raul; Valera, Enrique; Muriano, Alejandro; Pividori, M-Isabel; Sanchez-Baeza, Francisco; Marco, M-Pilar

    2013-09-01

    An electrochemical magneto immunosensor for the detection of low concentrations of paraquat (PQ) in food samples has been developed and its performance evaluated in a complex sample such as potato extracts. The immunosensor presented uses immunoreagents specifically developed for the recognition of paraquat, a magnetic graphite-epoxy composite (m-GEC) electrode and biofunctionalized magnetic micro-particles (PQ1-BSAMP) that allow reduction of the potential interferences caused by the matrix components. The amperometric signal is provided by an enzymatic probe prepared by covalently linking an enzyme to the specific antibodies (Ab198-cc-HRP). The use of hydroquinone, as mediator, allows recording of the signal at a low potential, which also contributes to reducing the background noise potentially caused by the sample matrix. The immunocomplexes formed on top of the modified MP are easily captured by the m-GEC, which acts simultaneously as transducer. PQ can be detected at concentrations as low as 0.18 ± 0.09 μg L(-1). Combined with an efficient extraction procedure, PQ residues can be directly detected and accurately quantified in potato extracts without additional clean-up or purification steps, with a limit of detection (90% of the maximum signal) of 2.18 ± 2.08 μg kg(-1), far below the maximum residue level (20 μg kg(-1)) established by the EC. The immunosensor presented here is suitable for on-site analysis. Combined with the use of magnetic racks, multiple samples can be run simultaneously in a reasonable time.

  20. Risk-based approach to developing a national residue sampling plan for testing under European Union regulation for veterinary medicinal products and coccidiostat feed additives in domestic animal production.

    PubMed

    Danaher, Martin; Shanahan, Conor; Butler, Francis; Evans, Rhodri; O'Sullivan, Dan; Glynn, Denise; Camon, Tim; Lawlor, Peadar; O'Keeffe, Michael

    2016-07-01

    A ranking system for veterinary medicinal products and coccidiostat feed additives has been developed as a tool to be applied in a risk-based approach to the residue testing programme for foods of animal origin in the Irish National Residue Control Plan (NRCP). Three characteristics of substances that may occur as residues in food are included in the developed risk ranking system: Potency, as measured by the acceptable daily intake assigned by the European Medicines Agency Committee for Medicinal Products for Veterinary Use, to each substance; Usage, as measured by the three factors of Number of Doses, use on Individual animals or for Group treatment, and Withdrawal Period; and Residue Occurrence, as measured by the number of Non-Compliant Samples in the NRCP. For both Number of Doses and Non-Compliant Samples, data for the 5-year period 2008-12 have been used. The risk ranking system for substances was developed for beef cattle, sheep and goats, pigs, chickens and dairy cattle using a scoring system applied to the various parameters described above to give an overall score based on the following equation: Potency × Usage (Number of Doses + Individual/Group Use + Withdrawal Period) × Residue Occurrence. Applying this risk ranking system, the following substances are ranked very highly: antimicrobials such as amoxicillin (for all species except pigs), marbofloxacillin (for beef cattle), oxytetracycline (for all species except chickens), sulfadiazine with trimethoprim (for pigs and chickens) and tilmicosin (for chickens); antiparasitic drugs, such as the benzimidazoles triclabendazole (for beef and dairy cattle), fenbendazole/oxfendazole (for sheep/goats and dairy cattle) and albendazole (for dairy cattle), the avermectin ivermectin (for beef cattle), and anti-fluke drugs closantel and rafoxanide (for sheep/goats); the anticoccidials monensin, narasin, nicarbazin and toltrazuril (for chickens). The risk ranking system described is a relatively simple system

  1. Simultaneous determination of nickel and copper by H-point standard addition method-first-order derivative spectrophotometry in plant samples after separation and preconcentration on modified natural clinoptilolite as a new sorbent.

    PubMed

    Roohparvar, Rasool; Taher, Mohammad Ali; Mohadesi, Alireza

    2008-01-01

    For the simultaneous determination of nickel(ll) and copper(ll) in plant samples, a rapid and accurate method was developed. In this method, solid-phase extraction (SPE) and first-order derivative spectrophotometry (FDS) are combined, and the result is coupled with the H-point standard addition method (HPSAM). Compared with normal spectrophotometry, derivative spectrophotometry offers the advantages of increased selectivity and sensitivity. As there is no need for carrying out any pretreatment of the sample, the spectrophotometry method is easy, but because of a high detection limit, it is not so practical. In order to decrease the detection limit, it is suggested to combine spectrophotometry with a preconcentration method such as SPE. In the present work, after separation and preconcentration of Ni(ll) and Cu(ll) on modified clinoptilolite zeolite that is loaded with 2-[1-(2-hydroxy-5-sulforphenyl)-3-phenyl-5-formaza-no]-benzoic acid monosodium salt (zincon) as a selective chromogenic reagent, FDS-HPSAM, which is a simple and selective spectrophotometric method, has been applied for simultaneous determination of these ions. With optimum conditions, the detection limit in original solutions is 0.7 and 0.5 ng/mL, respectively, for nickel and copper. The linear concentration ranges in the proposed method for nickel and copper ions in original solutions are 1.1 to 3.0 x 10(3) and 0.9 to 2.0 x 10(3) ng/mL, respectively. The recommended procedure is applied to successful determination of Cu(ll) and Ni(ll) in standard and real samples.

  2. Optimization for Peptide Sample Preparation for Urine Peptidomics

    SciTech Connect

    Sigdel, Tara K.; Nicora, Carrie D.; Hsieh, Szu-Chuan; Dai, Hong; Qian, Weijun; Camp, David G.; Sarwal, Minnie M.

    2014-02-25

    when utilizing the conventional SPE method. In conclusion, the mSPE method was found to be superior to the conventional, standard SPE method for urine peptide sample preparation when applying LC-MS peptidomics analysis due to the optimized sample clean up that provided improved experimental inference from the confidently identified peptides.

  3. A novel pretreatment approach for fast determination of organochlorine pesticides in biotic samples.

    PubMed

    Yang, Dai B; Wang, Ya Q; Liu, Wen X; Tao, Shu

    2008-05-01

    Recent studies have focused on enantiomeric behaviors of chiral organochlorine pesticides (OCPs) in biotic matrix because they provide insights into the biotransformation processes of chiral OCPs. In the present paper, a double in-line column chromatographic method was developed to effectively remove the lipid impurity in different biotic samples for clean-up of OCPs. After an initial Soxhlet extraction of OCPs from the biotic samples by a mixture of acetone and dichloromethane (DCM), dimethyl sulfoxide (DMSO) was directly added to the extract, and low boiling point solvents (acetone and DCM) were then evaporated. OCPs remained in DMSO were eluted via column 1 filled with silicon gel, and subsequently passed through column 2 packed with 15% deactivated florisil. This novel method was characterized by significant time and solvent savings. The recovery rates of alpha-HCH (hexachlorocyclohexane), beta-HCH, gamma-HCH and delta-HCH were 78.5+/-3.1%, 72.4+/-7.7%, 72+/-4.0% and 70.0+/-8.7%, respectively, and 92.5+/-3.8%, 79.7+/-6.7% and 83.4+/-6.5% for 1,1-dichloro-2-(2-chlorophenyl)-2-(4- chlorophenyl) ethylene (o,p'-DDE), 1,1-dichloro-2-(2-chlorophenyl)-2-(4-chloro phenyl)ethane (o,p'-DDD) and 1,1,1-trichloro-2-(2-chlorophenyl)-2-(4-chlorophenyl) ethane (o,p'-DDT), separately. In addition, the separation efficiencies of the target compounds by both achiral and chiral gas chromatographic columns were satisfactory using the established method. Therefore, the double in-line column chromatography was a useful alternative method for pretreatment of OCPs in different biotic samples.

  4. Fast RPLC-UV method on short sub-two microns particles packed column for the assay of tenoxicam in plasma samples.

    PubMed

    Sora, Iulia; Galaon, Toma; Udrescu, Stefan; Negru, Jean; David, Victor; Medvedovici, Andrei

    2007-03-12

    An extraction-less sample preparation technique followed by a RPLC-UV method on sub-two microns particles packed short column were used for the assay of tenoxicam in plasma samples. Protein precipitation was made by means of trichloroacetic acid addition. Supernatant was injected to the chromatographic column without any further pH adjustment. The mobile phase consisted in a mixture of acetonitrile and aqueous 0.1% phosphoric acid, at 2 mL/min flow rate and gradient elution. The Zorbax SB-C18 column (50 mm length, 4.6 mm internal diameter and 1.8 microm particle size) was thermostated at 60 degrees C. The mobile phase gradient composition program allowed separation of tenoxicam and piroxicam (internal standard), column clean-up and re-equilibration within 4 min. UV detection was achieved at 368+/-10 nm. The method is characterized by a low limit of quantitation of 25 ng/mL for tenoxicam, with a linearity interval up to 5500 ng/mL. The use of a low volume detection cell and detector high frequency data acquisition rate produced high precision and accuracy through a whole bioequivalence study of tenoxicam in two commercially available tablet formulations, after a single oral administration dose. Full method validation is presented. The high throughput characteristic of the proposed method allowed full validation and bioanalytical study completion within a 96 h period.

  5. Rapid determination of actinides in asphalt samples

    SciTech Connect

    Maxwell, Sherrod L.; Culligan, Brian K.; Hutchison, Jay B.

    2014-01-12

    A new rapid method for the determination of actinides in asphalt samples has been developed that can be used in emergency response situations or for routine analysis If a radiological dispersive device (RDD), Improvised Nuclear Device (IND) or a nuclear accident such as the accident at the Fukushima Nuclear Power Plant in March, 2011 occurs, there will be an urgent need for rapid analyses of many different environmental matrices, including asphalt materials, to support dose mitigation and environmental clean up. The new method for the determination of actinides in asphalt utilizes a rapid furnace step to destroy bitumen and organics present in the asphalt and sodium hydroxide fusion to digest the remaining sample. Sample preconcentration steps are used to collect the actinides and a new stacked TRU Resin + DGA Resin column method is employed to separate the actinide isotopes in the asphalt samples. The TRU Resin plus DGA Resin separation approach, which allows sequential separation of plutonium, uranium, americium and curium isotopes in asphalt samples, can be applied to soil samples as well.

  6. Rapid determination of actinides in asphalt samples

    DOE PAGES

    Maxwell, Sherrod L.; Culligan, Brian K.; Hutchison, Jay B.

    2014-01-12

    A new rapid method for the determination of actinides in asphalt samples has been developed that can be used in emergency response situations or for routine analysis If a radiological dispersive device (RDD), Improvised Nuclear Device (IND) or a nuclear accident such as the accident at the Fukushima Nuclear Power Plant in March, 2011 occurs, there will be an urgent need for rapid analyses of many different environmental matrices, including asphalt materials, to support dose mitigation and environmental clean up. The new method for the determination of actinides in asphalt utilizes a rapid furnace step to destroy bitumen and organicsmore » present in the asphalt and sodium hydroxide fusion to digest the remaining sample. Sample preconcentration steps are used to collect the actinides and a new stacked TRU Resin + DGA Resin column method is employed to separate the actinide isotopes in the asphalt samples. The TRU Resin plus DGA Resin separation approach, which allows sequential separation of plutonium, uranium, americium and curium isotopes in asphalt samples, can be applied to soil samples as well.« less

  7. Rapid On-Site Environmental Sampling and Analysis of Propellant Stabilizers and their Decomposition Products by Portable Sampling and Thin-Layer Chromotography Kits

    SciTech Connect

    Haas, J S; Gonzalez, M A

    2003-08-04

    Sustainable future use of land containing unexploded ordnance requires extensive field assessments, cleanup, and restoration. The ordnance is generally semi-exposed or buried in pits and, because of aging, needs to be handled with caution. Being able to characterize the ordnance in the field to minimize handling, as well as to distinguish it from inert mock material, greatly facilitates assessments and clean-up. We have developed unique sample preparation methodologies and a portable thin-layer chromatography (TLC) kit technology for rapid field screening and quantitative assessment of stabilizer content in propellants and, energetic materials (explosives) in environmental scenarios. Major advantages of this technology include simultaneous chromatography of multiple samples and standards for high sample throughput, high resolution, very low detection limits, and ease of operation. The TLC kit technology, sponsored by the Defense Ammunition Center (DAC) of the U.S. Army, is now patented and has been completely transitioned to our commercial partners, Ho'olana Technologies, located in Hilo, Hawaii. Once fully deployed in the field, the new technology will demonstrate a cost-effective and efficient means for determining the percent of effective stabilizer that is remaining on-site and at munitions clean-up sites, as well as munitions storage facilities. The TLC kit technology is also readily applicable for analysis at military or commercial facilities, for a variety of emergency and non-emergency scenarios, and for situations where public concern is high.

  8. Ochratoxin A in cocoa and chocolate sampled in Canada

    PubMed Central

    Turcotte, A.-M.; Scott, P.M.

    2011-01-01

    In order to determine the levels of ochratoxin A (OTA) in cocoa and cocoa products available in Canada, a previously published analytical method, with minor modifications to the extraction and immunoaffinity clean-up and inclusion of an evaporation step, was initially used (Method I). To improve the low method recoveries (46–61%), 40% methanol was then included in the aqueous sodium bicarbonate extraction solvent (pH 7.8) (Method II). Clean-up was on an Ochratest™ immunoaffinity column and OTA was determined by liquid chromatography (LC) with fluorescence detection. Recoveries of OTA from spiked cocoa powder (0.5 and 5 ng g−1) were 75–84%; while recoveries from chocolate were 93–94%. The optimized method was sensitive (limit of quantification (LOQ) = 0.07–0.08 ng g−1), accurate (recovery = 75–94%) and precise (coefficient of variation (CV) < 5%). It is applicable to cocoa and chocolate. Analysis of 32 samples of cocoa powder (16 alkalized and 16 natural) for OTA showed an incidence of 100%, with concentrations ranging from 0.25 to 7.8 ng g−1; in six samples the OTA level exceeded 2 ng g−1, the previously considered European Union limit for cocoa. The frequency of detection of OTA in 28 chocolate samples (21 dark or baking chocolate and seven milk chocolate) was also 100% with concentrations ranging from 0.05 to 1.4 ng g−1; one sample had a level higher than the previously considered European Union limit for chocolate (1 ng g−1). PMID:21623500

  9. Ochratoxin A in cocoa and chocolate sampled in Canada.

    PubMed

    Turcotte, A-M; Scott, P M

    2011-06-01

    In order to determine the levels of ochratoxin A (OTA) in cocoa and cocoa products available in Canada, a previously published analytical method, with minor modifications to the extraction and immunoaffinity clean-up and inclusion of an evaporation step, was initially used (Method I). To improve the low method recoveries (46-61%), 40% methanol was then included in the aqueous sodium bicarbonate extraction solvent (pH 7.8) (Method II). Clean-up was on an Ochratest™ immunoaffinity column and OTA was determined by liquid chromatography (LC) with fluorescence detection. Recoveries of OTA from spiked cocoa powder (0.5 and 5 ng g(-1)) were 75-84%; while recoveries from chocolate were 93-94%. The optimized method was sensitive (limit of quantification (LOQ) = 0.07-0.08 ng g(-1)), accurate (recovery = 75-94%) and precise (coefficient of variation (CV) < 5%). It is applicable to cocoa and chocolate. Analysis of 32 samples of cocoa powder (16 alkalized and 16 natural) for OTA showed an incidence of 100%, with concentrations ranging from 0.25 to 7.8 ng g(-1); in six samples the OTA level exceeded 2 ng g(-1), the previously considered European Union limit for cocoa. The frequency of detection of OTA in 28 chocolate samples (21 dark or baking chocolate and seven milk chocolate) was also 100% with concentrations ranging from 0.05 to 1.4 ng g(-1); one sample had a level higher than the previously considered European Union limit for chocolate (1 ng g(-1)).

  10. Analytical performance of two miniaturised extraction methods for triclosan and methyltriclosan, in fish roe and surimi samples.

    PubMed

    Gonzalo-Lumbreras, R; Sanz-Landaluze, J; Cámara, C

    2014-03-01

    A new and reliable miniaturised QuEChERS-based extraction method combined with a dispersive SPE cleanup procedure for extracting triclosan and methyltriclosan from fish roe and surimi samples was proposed. The effectiveness of different extraction/partition conditions for QuEChERS method was systematically investigated, and the use of acetonitrile extraction solvent and MgSO4, PSA, C18 and Florisil as cleanup reagents was recommended in the final method. Other method based on ultrasonic extraction with ethylacetate and clean-up with SPE was also evaluated for these samples. Different polymeric and silica sorbents for clean up were tested and the combination of Florisil and PSA was finally selected. The performance of these miniaturised sample preparation methods combined with GC-MS with quadrupole detection were compared. Extraction efficiency as well as cleaning effectiveness, laboriousness and speed were taken as criteria for method evaluation. Satisfactory validation parameters, such as linearity, recovery, precision and LODs and LOQs for both developed analytical methods were obtained from fish roe and surimi samples. Finally, both methods were applied to real samples. The sensitivity of the proposed methods was good enough to ensure reliable determination of target analytes at concentration levels commonly found in this kind of samples.

  11. Supercritical fluid extraction of polyhalogenated pollutants from aquaculture and marine environmental samples: a review.

    PubMed

    García-Rodríguez, Diego; Carro-Díaz, Antonia María; Lorenzo-Ferreira, Rosa Antonia

    2008-05-01

    This article focuses on the state-of-the-art in sample preparation using supercritical fluid extraction (SFE), to monitor the content of polyhalogenated pollutants in aquaculture and marine environmental samples. Marine sediments and biological applications, including several types of samples matrices (fish, shellfish, seaweed and fish feed) and analyte groups (polychlorinated biphenyls (PCBs), polybrominated biphenyls (PBBs), polybrominated diphenylethers (PBDEs), polychlorinated dibenzo-p-dioxin (PCDD)/Fs and organochlorinated pesticide (OCPs)) are discussed with respect to SFE use and optimisation of conditions. We also discuss the great analytical potential of SFE, the integration of the extraction and clean-up steps for rapid sample processing justifying its use for routine work. The most recent SFE applications to the determination of these pollutants in marine environmental (biota and sediment) samples, published in the last 15 years, are reviewed.

  12. Middlesex Sampling Plant environmental report for calendar year 1992, 239 Mountain Avenue, Middlesex, New Jersey. Formerly Utilized Sites Remedial Action Program (FUSRAP)

    SciTech Connect

    Not Available

    1993-05-01

    This report describes the environmental surveillance program at the Middlesex Sampling Plant (MSP) and provides the results for 1992. The site, in the Borough of Middlesex, New Jersey, is a fenced area and includes four buildings and two storage piles that contain 50,800 m{sup 3} of radioactive and mixed hazardous waste. More than 70 percent of the MSP site is paved with asphalt. The MSP facility was established in 1943 by the Manhattan Engineer District (MED) to sample, store, and/or ship uranium, thorium, and beryllium ores. In 1955 the Atomic Energy Commission (AEC), successor to MED, terminated the operation and later used the site for storage and limited sampling of thorium residues. In 1967 AEC activities ceased, onsite structures were decontaminated, and the site was certified for unrestricted use under criteria applicable at that time. In 1980 the US Department of Energy (DOE) initiated a multiphase remedial action project to clean up several vicinity properties onto which contamination from the plant had migrated. Material from these properties was consolidated into the storage piles onsite. Environmental surveillance of MSP began in 1980 when Congress added the site to DOE`s Formerly Utilized Sites Remedial Action Program. The environmental surveillance program at MSP includes sampling networks for radon and thoron in air; external gamma radiation exposure; and radium-226, radium-228, thorium-230, thorium-232, and total uranium in surface water, sediment, and groundwater. Additionally, chemical analyses are performed to detect metals and organic compounds in surface water and groundwater and metals in sediments. This program assists in fulfilling th DOE policy of measuring and monitoring effluents from DOE activities and calculating hypothetical doses.

  13. Determination of insoluble soap in agricultural soil and sewage sludge samples by liquid chromatography with ultraviolet detection.

    PubMed

    Cantarero, Samuel; Zafra-Gómez, Alberto; Ballesteros, Oscar; Navalón, Alberto; Vílchez, José L; Crovetto, Guillermo; Verge, Coral; de Ferrer, Juan A

    2010-11-01

    We have developed a new analytical procedure for determining insoluble Ca and Mg fatty acid salts (soaps) in agricultural soil and sewage sludge samples. The number of analytical methodologies that focus in the determination of insoluble soap salts in different environmental compartments is very limited. In this work, we propose a methodology that involves a sample clean-up step with petroleum ether to remove soluble salts and a conversion of Ca and Mg insoluble salts into soluble potassium salts using tripotassium ethylenediaminetetraacetate salt and potassium carbonate, followed by the extraction of analytes from the samples using microwave-assisted extraction with methanol. An improved esterification procedure using 2,4-dibromoacetophenone before the liquid chromatography with ultraviolet detection analysis also has been developed. The absence of matrix effect was demonstrated with two fatty acid Ca salts that are not commercial and are never detected in natural samples (C₁₃:₀ and C₁₇:₀). Therefore, it was possible to evaluate the matrix effect because both standards have similar environmental behavior (adsorption and precipitation) to commercial soaps (C₁₀:₀) to C₁₈:₀). We also studied the effect of the different variables on the clean-up, the conversion of Ca soap, and the extraction and derivatization procedures. The quantification limits found ranged from 0.4 to 0.8 mg/kg. The proposed method was satisfactorily applied for the development of a study on soap behavior in agricultural soil and sewage sludge samples.

  14. Cyanovanadate(III) complexes as novel additives for efficient generation of volatile cadmium species in complex samples prior to determinations by inductively coupled plasma mass spectrometry (ICP-MS).

    PubMed

    Yilmaz, Vedat; Arslan, Zikri; Rose, LaKeysha; Little, Maria D

    2013-10-15

    A new method has been described for generation of volatile species of Cd using vanadium(III) cyanide complex. Aqueous solutions of 0.04 mol L(-1) vanadium chloride (VCl3) and 0.12 mol L(-1) potassium cyanide (KCN) were reacted on-line yielding a suspension of vanadium hydroxide, V(OH)3. This suspension was dissolved along the stream of sample solution in dilute HCl to form heptacyanovanadate(III) complex, [V(CN)7]4-. Volatile Cd species were generated by reacting the stream of sample solution and cyanovanadate(III) complex with sodium borohydride (NaBH4). Feasibility of off-line and on-online approaches was investigated for quantitative determinations. Better precision and daily stability were achieved with on-line settings. Optimum signals were obtained from sample solutions within a range of 3 to 5% v/v HCl. A concentration of 2% m/v NaBH4 was adequate to achieve an enhancement of 20-fold in the presence of cyanovanadate(III) complex. The limits of detection were 5.0 and 4.5 ng L(-1) for 110Cd and 111Cd isotopes, respectively. Precision (%RSD) was better than 4.7% for six replicate measurements. The interferences of Cu(II) and Ni(II) were marginal (<10%) at 1.0 µg mL(-1). Depressive effects from Bi, Se and Sn were not significant below 0.1 µg mL(-1). The method was validated by determination of Cd using ICP-MS in certified reference materials of Nearshore seawater (CASS-4), Bone ash (SRM 1400), Dogfish liver (DOLT-4) and Mussel tissue (SRM 2976).

  15. Investigations into the feasibility of routine ultra high performance liquid chromatography-tandem mass spectrometry analysis of equine hair samples for detecting the misuse of anabolic steroids, anabolic steroid esters and related compounds.

    PubMed

    Gray, Bobby P; Viljanto, Marjaana; Bright, Jane; Pearce, Clive; Maynard, Steve

    2013-07-17

    The detection of the abuse of anabolic steroids in equine sport is complicated by the endogenous nature of some of the abused steroids, such as testosterone and nandrolone. These steroids are commonly administered as intramuscular injections of esterified forms of the steroid, which prolongs their effects and improves bioavailability over oral dosing. The successful detection of an intact anabolic steroid ester therefore provides unequivocal proof of an illegal administration, as esterified forms are not found endogenously. Detection of intact anabolic steroid esters is possible in plasma samples but not, to date, in the traditional doping control matrix of urine. The analysis of equine mane hair for the detection of anabolic steroid esters has the potential to greatly extend the time period over which detection of abuse can be monitored. Equine mane hair samples were incubated in 0.1M phosphate buffer (pH 9.5) before anabolic steroids (testosterone, nandrolone, boldenone, trenbolone and stanozolol), anabolic steroid esters (esters of testosterone, nandrolone, boldenone and trenbolone) and associated compounds (fluticasone propionate and esters of hydroxyprogesterone) were extracted by liquid-liquid extraction with a mix of hexane and ethyl acetate (7:3, v:v). Further sample clean up by solid phase extraction was followed by derivatisation with methoxylamine HCL and analysis by UHPLC-MS/MS. Initial method development was performed on a representative suite of four testosterone esters (propionate, phenylpropionate, isocaproate and decanoate) and the method was later extended to include a further 18 compounds. The applicability of the method was demonstrated by the analysis of mane hair samples collected following the intramuscular administration of 500 mg of Durateston(®) (mixed testosterone esters) to a Thoroughbred mare (560 kg). The method was subsequently used to successfully detect boldenone undecylenate and stanozolol in hair samples collected following

  16. Preservation of samples for dissolved mercury

    USGS Publications Warehouse

    Hamlin, S.N.

    1989-01-01

    Water samples for dissolved mercury requires special treatment because of the high chemical mobility and volatility of this element. Widespread use of mercury and its compounds has provided many avenues for contamination of water. Two laboratory tests were done to determine the relative permeabilities of glass and plastic sample bottles to mercury vapor. Plastic containers were confirmed to be quite permeable to airborne mercury, glass containers were virtually impermeable. Methods of preservation include the use of various combinations of acids, oxidants, and complexing agents. The combination of nitric acid and potassium dichromate successfully preserved mercury in a large variety of concentrations and dissolved forms. Because this acid-oxidant preservative acts as a sink for airborne mercury and plastic containers are permeable to mercury vapor, glass bottles are preferred for sample collection. To maintain a healthy work environment and minimize the potential for contamination of water samples, mercury and its compounds are isolated from the atmosphere while in storage. Concurrently, a program to monitor environmental levels of mercury vapor in areas of potential contamination is needed to define the extent of mercury contamination and to assess the effectiveness of mercury clean-up procedures.Water samples for dissolved mercury require special treatment because of the high chemical mobility and volatility of this element. Widespread use of mercury and its compounds has provided many avenues for contamination of water. Two laboratory tests were done to determine the relative permeabilities of glass and plastic sample bottles to mercury vapor. Plastic containers were confirmed to be quite permeable to airborne mercury, glass containers were virtually impermeable. Methods of preservation include the use of various combinations of acids, oxidants, and complexing agents. The combination of nitric acid and potassium dichromate successfully preserved mercury in a

  17. Simultaneous qualitative and quantitative analysis of 21 mycotoxins in Radix Paeoniae Alba by ultra-high performance liquid chromatography quadrupole linear ion trap mass spectrometry and QuEChERS for sample preparation.

    PubMed

    Xing, Yanyan; Meng, Wenting; Sun, Wanyang; Li, Dongxiang; Yu, Zhiguo; Tong, Ling; Zhao, Yunli

    2016-09-15

    A high-throughput method for simultaneous qualitative and quantitative analysis of 21 mycotoxins in Radix Paeoniae Alba (RPA) was developed by coupling the modified QuEChERS method with ultra-high performance liquid chromatography quadrupole linear ion trap mass spectrometry (UHPLC-QqLIT-MS). The 21 mycotoxins were extracted and cleaned up using QuEChERS-based procedure, then further separated on a C18 column and detected by a hybrid triple quadrupole linear ion trap mass spectrometer equipped with electrospray ionization source in the multiple reaction monitoring-information dependent acquisition-enhanced product ion (MRM-IDA-EPI) mode. Under this technique, 13 mycotoxins were detected using acetonitrile and water containing 0.1% formic acid as the mobile phase in positive mode while the other 8 mycotoxins were detected using acetonitrile and water containing 0.1% ammonia as the mobile phase in negative mode. The calibration curves of all analytes showed good linearity (r(2)>0.995) within test ranges. The limits of detection and quantification ranged from 0.031 to 5.4μg/kg and 0.20 to 22μg/kg, respectively. Additionally, recoveries were all above 75.3% with relative standard deviations within 15%. The method proposed herein with significant advantages including simple pretreatment, rapid determination as well as high sensitivity, accuracy and throughput would be a preferred candidate for the determination and quantification of multi-class mycotoxin contaminants in real samples.

  18. New addition curing polyimides

    NASA Technical Reports Server (NTRS)

    Frimer, Aryeh A.; Cavano, Paul

    1991-01-01

    In an attempt to improve the thermal-oxidative stability (TOS) of PMR-type polymers, the use of 1,4-phenylenebis (phenylmaleic anhydride) PPMA, was evaluated. Two series of nadic end-capped addition curing polyimides were prepared by imidizing PPMA with either 4,4'-methylene dianiline or p-phenylenediamine. The first resulted in improved solubility and increased resin flow while the latter yielded a compression molded neat resin sample with a T(sub g) of 408 C, close to 70 C higher than PME-15. The performance of these materials in long term weight loss studies was below that of PMR-15, independent of post-cure conditions. These results can be rationalized in terms of the thermal lability of the pendant phenyl groups and the incomplete imidization of the sterically congested PPMA. The preparation of model compounds as well as future research directions are discussed.

  19. Different formats of imprinted polymers for determining organotin compounds in environmental samples.

    PubMed

    Gallego-Gallegos, Mercedes; Muñoz-Olivas, Riansares; Cámara, Carmen

    2009-02-01

    Organotin compounds and their degradation products enter the environment mainly as a result of their use as biocides and antifouling paints. Analysis of these compounds in environmental samples has to be very sensitive and selective so that their concentrations corresponding to the low environmental target values can also be detected. Generally, analysis of a complex matrix leads to high interferences during the different process steps; clean-up procedures are recommended to overcome this problem. For the past many years, solid phase extraction by employing imprinted materials has been extensively used for many organic substances that are used for pre-concentration and clean-up purposes with excellent results. Here, we present three different imprinted polymers prepared via bulk, precipitation, and emulsion polymerization methods that use similar compositions. The synthesized polymer particles were characterized morphologically by employing scanning electron microscopy and Brunauer-Emmett-Teller analysis. Binding properties were calculated using the Langmuir-Freundlich isotherm. Depending on the properties of the materials, different analytical applications for complex matrices are proposed. These applications are mainly used on tributyltin and its degradation products for environmental analysis.

  20. Occurrence of ochratoxin A in wine and beer samples from China.

    PubMed

    Wu, Jianwei; Tan, Yinfeng; Wang, Yuqi; Xu, Rong

    2011-01-01

    A total of 125 wine and beer samples, including 42 white, 63 red wine and 20 beer samples, originating from several areas of China were analyzed for ochratoxin A (OTA). An analytical method based on immunoaffinity column (IAC) for clean-up and high performance liquid chromatography with fluorescence detection (HPLC-FD) was used to determine OTA. Positive results were further confirmed by LC-MS-MS. OTA was detected in 22 (17.6%) samples at levels of 0.02-1.18 ng/ml, which were below the EU maximum limit. The mean OTA concentration in red wine was slightly higher than in white wine. This study showed that OTA occurs in wine and beer in China but at levels that pose no danger of significant human exposure to OTA from this source.

  1. Capillary sample

    MedlinePlus

    ... repeat the test with blood drawn from a vein. Alternative Names Blood sample - capillary; Fingerstick; Heelstick Images Phenylketonuria test Phenylketonuria test Capillary sample References Garza ...

  2. A sensitive and efficient method for routine pesticide multiresidue analysis in bee pollen samples using gas and liquid chromatography coupled to tandem mass spectrometry.

    PubMed

    Vázquez, P Parrilla; Lozano, A; Uclés, S; Ramos, M M Gómez; Fernández-Alba, A R

    2015-12-24

    Several clean-up methods were evaluated for 253 pesticides in pollen samples concentrating on efficient clean-up and the highest number of pesticides satisfying the recovery and precision criteria. These were: (a) modified QuEChERS using dSPE with PSA+C18; (b) freeze-out prior to QuEChERS using dSPE with PSA+C18; (c) freeze-out prior to QuEChERS using dSPE with PSA+C18+Z-Sep; and (d) freeze-out followed by QuEChERS using dSPE with PSA+C18 and SPE with Z-Sep. Determinations were made using LC-MS/MS and GC-MS/MS. The modified QuEChERS protocol applying a freeze-out followed by dSPE with PSA+C18 and SPE clean-up with Z-Sep was selected because it provided the highest number of pesticides with mean recoveries in the 70-120% range, as well as relative standard deviations (RSDs) typically below 20% (12.2% on average) and ensured much better removal of co-extracted matrix compounds of paramount importance in routine analysis. Limits of quantification at levels as low as 5μgkg(-1) were obtained for the majority of the pesticides. The proposed methodology was applied to the analysis of 41 pollen bee samples from different areas in Spain. Pesticides considered potentially toxic to bees (DL50<2μg/bee) were detected in some samples with concentrations up to 72.7μgkg(-1), which could negatively affect honeybee health.

  3. Injection-port derivatization coupled to GC-MS/MS for the analysis of glycosylated and non-glycosylated polyphenols in fruit samples.

    PubMed

    Marsol-Vall, Alexis; Balcells, Mercè; Eras, Jordi; Canela-Garayoa, Ramon

    2016-08-01

    Polyphenols, including glycosylated polyphenols, were analyzed via a procedure based on injection-port derivatization coupled to gas chromatography-tandem mass spectrometry (GC-MS/MS). The polyphenols in lyophilized fruit samples were extracted with an acidified MeOH mixture assisted by ultrasound. Samples were dried under vacuum, and carbonyl groups were protected with methoxylamine. Free hydroxyl groups were subsequently silylated in-port. Mass fragmentations of 17 polyphenol and glycosylated polyphenol standards were examined using Multiple Reaction Monitoring (MRM) as the acquisition mode. Furthermore, in-port derivatization was optimized in terms of optimal injection port temperature, derivatization time and sample: N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) volume ratio. A C18 solid-phase-extraction clean-up method was used to reduce matrix effects and injection liner degradation. Using this clean-up method, recoveries for samples spiked at 1 and 10μg/g ranged from 52% to 98%, depending on the chemical compound. Finally, the method was applied to real fruit samples containing the target compounds. The complete chromatographic runtime was 15min, which is faster than reported for recent HPLC methods able to analyze similar compounds.

  4. Determining the extragalactic extinction law with SALT - II. Additional sample

    NASA Astrophysics Data System (ADS)

    Finkelman, Ido; Brosch, Noah; Kniazev, Alexei Y.; Väisänen, Petri; Buckley, David A. H.; O'Donoghue, Darragh; Gulbis, Amanda; Hashimoto, Yas; Loaring, Nicola; Romero-Colmenero, Encarni; Sefako, Ramotholo

    2010-12-01

    We present new results from an ongoing programme to study the dust extragalactic extinction law in E/S0 galaxies with dust lanes with the Southern African Large Telescope (SALT) during its performance verification phase. The wavelength dependence of the dust extinction for seven galaxies is derived in six spectral bands ranging from the near-ultraviolet atmospheric cut-off to the near-infrared. The derivation of an extinction law is performed by fitting model galaxies to the unextinguished parts of the image in each spectral band, and subtracting from these the actual images. We compare our results with the derived extinction law in the Galaxy and find them to run parallel to the Galactic extinction curve with a mean total-to-selective extinction value of RV = 2.71 +/- 0.43. We use total optical extinction values to estimate the dust mass for each galaxy, compare these with dust masses derived from IRAS measurements, and find them to range from 104 to 107 Msolar. We study the case of the well-known dust-lane galaxy NGC2685 for which Hubble Space Telescope/Wide Field Planetary Camera 2 (HST/WFPC2) data are available to test the dust distribution on different scales. Our results imply a scale-free dust distribution across the dust lanes, at least within ~1arcsec (~60 pc) regions. Based on observations made with the Southern African Large Telescope (SALT). E-mail: ido@wise.tau.ac.il (IF); noah@wise.tau.ac.il (NB); akniazev@saao.ac.za (AYK); petri@saao.ac.za (PV); dibnob@saao.ac.za (DAHB); dod@saao.ac.za (DO); amanda@saao.ac.za (AG); hashimot@ntnu.edu.tw (YH); nsl@saao.ac.za (NL); erc@saao.ac.za (ER-C); rrs@saao.ac.za (RS)

  5. Rapid cleanup of bacterial DNA from samples containing aerosol contaminants

    NASA Astrophysics Data System (ADS)

    Menking, Darrell E.; Kracke, Suzanne K.; Emanuel, Peter A.; Valdes, James J.

    1999-01-01

    Polymerase Chain Reaction (PCR) is an in vitro enzymatic, synthetic method used to amplify specific DNA sequences from organisms. Detection of DNA using gene probes allows for absolute identification not only of specific organisms, but also of genetic material in recombinant organisms. PCR is an exquisite biological method for detecting bacteria in aerosol samples. A major challenge facing detection of DNA from field samples is that they are almost sure to contain impurities, especially impurities that inhibit amplification through PCR. DNA is being extracted from air, sewage/stool samples, food, sputum, a water and sediment; however, multi- step, time consuming methods are required to isolate the DNA from the surrounding contamination. This research focuses on developing a method for rapid cleanup of DNA which combines extraction and purification of DNA while, at the same time, removing inhibitors from 'dirty samples' to produce purified, PCR-ready DNA. GeneReleaser produces PCR-ready DNA in a rapid five-minute protocol. GeneReleaser resin was able to clean up sample contain micrograms of typical aerosol and water contaminants. The advantages of using GR are that it is rapid, inexpensive, requires one-step, uses no hazardous material and produces PCR-ready DNA.

  6. Quantitation of yeast total proteins in sodium dodecyl sulfate-polyacrylamide gel electrophoresis sample buffer for uniform loading.

    PubMed

    Sheen, Hyukho

    2016-04-01

    Proteins in sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) sample buffer are difficult to quantitate due to SDS and reducing agents being in the buffer. Although acetone precipitation has long been used to clean up proteins from detergents and salts, previous studies showed that protein recovery from acetone precipitation varies from 50 to 100% depending on the samples tested. Here, this article shows that acetone precipitates proteins highly efficiently from SDS-PAGE sample buffer and that quantitative recovery is achieved in 5 min at room temperature. Moreover, precipitated proteins are resolubilized with urea/guanidine, rather than with SDS. Thus, the resolubilized samples are readily quantifiable with Bradford reagent without using SDS-compatible assays.

  7. Pyrolysis-capillary gas chromatography-mass spectrometry for the determination of polyvinyl chloride traces in solid environmental samples.

    PubMed

    Tienpont, B; David, F; Vanwalleghem, F; Sandra, P

    2001-03-16

    A novel method based on pyrolysis-capillary gas chromatography-mass spectrometry (CGC-MS) was developed for the quantitative analysis of polyvinylchloride (PVC) in solid environmental samples like sludge and dust. The samples are extracted and the extract is fractionated by solid-phase extraction (SPE). Possibly interfering biological and frequently occuring synthetic polymers are removed by this clean-up. The final extract is analyzed by pyrolysis-CGC-MS. Selective detection of PVC is performed by using specific markers in the pyrogram. Quantitation is done on naphthalene. Good linearity was obtained in a range from 0.5 to 100 microg applied to the pyrolyser. The limit of quantitation (LOQ) in sludge and dust samples is 10 mg/kg dry mass. A correlation between PVC and phthalates was made for sewage sludge samples.

  8. Venous Sampling

    MedlinePlus

    ... parts of the body, including: Adrenal venous sampling (AVS) , in which blood samples are taken from the ... for a few days before the procedure. For AVS, you will be asked to stop taking certain ...

  9. A simple and selective method for determination of phthalate biomarkers in vegetable samples by high pressure liquid chromatography-electrospray ionization-tandem mass spectrometry.

    PubMed

    Zhou, Xi; Cui, Kunyan; Zeng, Feng; Li, Shoucong; Zeng, Zunxiang

    2016-06-01

    In the present study, solid-phase extraction cartridges including silica reversed-phase Isolute C18, polymeric reversed-phase Oasis HLB and mixed-mode anion-exchange Oasis MAX, and liquid-liquid extractions with ethyl acetate, n-hexane, dichloromethane and its mixtures were compared for clean-up of phthalate monoesters from vegetable samples. Best recoveries and minimised matrix effects were achieved using ethyl acetate/n-hexane liquid-liquid extraction for these target compounds. A simple and selective method, based on sample preparation by ultrasonic extraction and liquid-liquid extraction clean-up, for the determination of phthalate monoesters in vegetable samples by liquid chromatography/electrospray ionisation-tandem mass spectrometry was developed. The method detection limits for phthalate monoesters ranged from 0.013 to 0.120 ng g(-1). Good linearity (r(2)>0.991) between MQLs and 1000× MQLs was achieved. The intra- and inter-day relative standard deviation values were less than 11.8%. The method was successfully used to determine phthalate monoester metabolites in the vegetable samples.

  10. Laser sampling

    NASA Astrophysics Data System (ADS)

    Gorbatenko, A. A.; Revina, E. I.

    2015-10-01

    The review is devoted to the major advances in laser sampling. The advantages and drawbacks of the technique are considered. Specific features of combinations of laser sampling with various instrumental analytical methods, primarily inductively coupled plasma mass spectrometry, are discussed. Examples of practical implementation of hybrid methods involving laser sampling as well as corresponding analytical characteristics are presented. The bibliography includes 78 references.

  11. Additive Similarity Trees

    ERIC Educational Resources Information Center

    Sattath, Shmuel; Tversky, Amos

    1977-01-01

    Tree representations of similarity data are investigated. Hierarchical clustering is critically examined, and a more general procedure, called the additive tree, is presented. The additive tree representation is then compared to multidimensional scaling. (Author/JKS)

  12. Lunar Sample Quarantine & Sample Curation

    NASA Technical Reports Server (NTRS)

    Allton, Judith H.

    2000-01-01

    The main goal of this presentation is to discuss some of the responsibility of the lunar sample quarantine project. The responsibilities are: flying the mission safely, and on schedule, protect the Earth from biohazard, and preserve scientific integrity of samples.

  13. Polyimide processing additives

    NASA Technical Reports Server (NTRS)

    Pratt, J. R.; St. Clair, T. L.; Burks, H. D.; Stoakley, D. M.

    1987-01-01

    A method has been found for enhancing the melt flow of thermoplastic polyimides during processing. A high molecular weight 422 copoly(amic acid) or copolyimide was fused with approximately 0.05 to 5 pct by weight of a low molecular weight amic acid or imide additive, and this melt was studied by capillary rheometry. Excellent flow and improved composite properties on graphite resulted from the addition of a PMDA-aniline additive to LARC-TPI. Solution viscosity studies imply that amic acid additives temporarily lower molecular weight and, hence, enlarge the processing window. Thus, compositions containing the additive have a lower melt viscosity for a longer time than those unmodified.

  14. [Food additives and healthiness].

    PubMed

    Heinonen, Marina

    2014-01-01

    Additives are used for improving food structure or preventing its spoilage, for example. Many substances used as additives are also naturally present in food. The safety of additives is evaluated according to commonly agreed principles. If high concentrations of an additive cause adverse health effects for humans, a limit of acceptable daily intake (ADI) is set for it. An additive is a risk only when ADI is exceeded. The healthiness of food is measured on the basis of nutrient density and scientifically proven effects.

  15. Shale JP-4 Additive Evaluation

    DTIC Science & Technology

    1986-10-01

    8217. •% . , ’ ,,,r ,% . -- - ,.-. ’ ’ 4,w% %’. " - ,’ . . . * ’, .* . TABLE OF CONTENTS .4q ,4 . * SECTION PAGE I. INTRODUCTION 1 II. TEST PARAMETERS 2 1...42 PRECEDING PAGE BLANK TABLE OF CONTENTS (CON’T) SECT ION PAGE V. CONCLUSIONS 44 REFERENCES 46 APPENDIX A Drum to Test Sample Relationship 47 APPENDIX...B.O.C.L.E. Results 40 vii LIST OF TABLES TABLE PAGE 1 Antioxidants 3 2 Raw Shale/Petroleum Fuel Properties 10 3 Drum Sample Additive Content 13 4

  16. Sampling Development

    PubMed Central

    Adolph, Karen E.; Robinson, Scott R.

    2011-01-01

    Research in developmental psychology requires sampling at different time points. Accurate depictions of developmental change provide a foundation for further empirical studies and theories about developmental mechanisms. However, overreliance on widely spaced sampling intervals in cross-sectional and longitudinal designs threatens the validity of the enterprise. This article discusses how to sample development in order to accurately discern the shape of developmental change. The ideal solution is daunting: to summarize behavior over 24-hour intervals and collect daily samples over the critical periods of change. We discuss the magnitude of errors due to undersampling, and the risks associated with oversampling. When daily sampling is not feasible, we offer suggestions for sampling methods that can provide preliminary reference points and provisional sketches of the general shape of a developmental trajectory. Denser sampling then can be applied strategically during periods of enhanced variability, inflections in the rate of developmental change, or in relation to key events or processes that may affect the course of change. Despite the challenges of dense repeated sampling, researchers must take seriously the problem of sampling on a developmental time scale if we are to know the true shape of developmental change. PMID:22140355

  17. Quantification of polycyclic aromatic hydrocarbons in tea and coffee samples of Mumbai City (India) by high performance liquid chromatography.

    PubMed

    Bishnoi, Narsi R; Mehta, Urvashi; Sain, Umashanker; Pandit, G G

    2005-08-01

    This paper describes a method for quantification of sixteen polycyclic aromatic hydrocarbons (PAHs) in tea and coffee samples of Mumbai City with the help of reversed phase high performance liquid chromatography with UV-VIS detector. This method is based on liquid-liquid extraction followed by clean up with C-18 cartridge. Concentration of total PAHs in different brands of tea and coffee samples varied from 18.79 to 31.37 microg/L and from 16.47 to 18.24 microg/L, respectively. Mean concentration of total PAHs was 27.56 microg/L in tea and 17.20 microg/L in coffee. Recoveries at different concentration levels were higher than 68% in samples of tea and coffee. Detection limit was found to be low (0.0006 ng) for anthracene and highest (0.174 ng) for naphthalene with relative standard deviation between 0.4%-7%.

  18. Nanoengineered Additives for Active Coatings

    DTIC Science & Technology

    2007-04-01

    commercial ad bial activ component from the coating, leading to eventual depletion of the film. Small TPU samples were evaluated using a Kirby - Bauer ...7 Table 5. Summary of 24-hr ASTM E 2180 tests with 1 weight-percent additive in PUr (solvent dispersible) based on 6-log loading of...Noveon X-1150). The ASTM E 2180 test is run in triplicate (Note that alternative ro 1° amines) was suspended in dry tetrahydrofuran (THF) (150 mL) in

  19. Sampling Development

    ERIC Educational Resources Information Center

    Adolph, Karen E.; Robinson, Scott R.

    2011-01-01

    Research in developmental psychology requires sampling at different time points. Accurate depictions of developmental change provide a foundation for further empirical studies and theories about developmental mechanisms. However, overreliance on widely spaced sampling intervals in cross-sectional and longitudinal designs threatens the validity of…

  20. Long-term Effects of Nutrient Addition and Phytoremediation on Diesel and Crude Oil Contaminated Soils in subarctic Alaska.

    PubMed

    Leewis, Mary-Cathrine; Reynolds, Charles M; Leigh, Mary Beth

    2013-12-01

    Phytoremediation is a potentially inexpensive method of detoxifying contaminated soils using plants and associated soil microorganisms. The remote locations and cold climate of Alaska provide unique challenges associated with phytoremediation such as finding effective plant species that can achieve successful site clean-up despite the extreme environmental conditions and with minimal site management. A long-term assessment of phytoremediation was performed which capitalized on a study established in Fairbanks in 1995. The original study sought to determine how the introduction of plants (Festuca rubra, Lolium multiflorum), nutrients (fertilizer), or their combination would affect degradation of petroleum hydrocarbon (TPH) contaminated soils (crude oil or diesel) over time. Within the year following initial treatments, the plots subjected to both planting and/or fertilization showed greater overall decreases in TPH concentrations in both the diesel and crude oil contaminated soils relative to untreated plots. We re-examined this field site after 15 years with no active site management to assess the long-term effects of phytoremediation on colonization by native and non-native plants, their rhizosphere microbial communities and on petroleum removal from soil. Native and non-native vegetation had extensively colonized the site, with more abundant vegetation found on the diesel contaminated soils than the more nutrient-poor, more coarse, and acidic crude oil contaminated soils. TPH concentrations achieved regulatory clean up levels in all treatment groups, with lower TPH concentrations correlating with higher amounts of woody vegetation (trees & shrubs). In addition, original treatment type has affected vegetation recruitment to each plot with woody vegetation and more native plants in unfertilized plots. Bacterial community structure also varies according to the originally applied treatments. This study suggests that initial treatment with native tree species in

  1. Long-term Effects of Nutrient Addition and Phytoremediation on Diesel and Crude Oil Contaminated Soils in subarctic Alaska

    PubMed Central

    Leewis, Mary-Cathrine; Reynolds, Charles M.; Leigh, Mary Beth

    2014-01-01

    Phytoremediation is a potentially inexpensive method of detoxifying contaminated soils using plants and associated soil microorganisms. The remote locations and cold climate of Alaska provide unique challenges associated with phytoremediation such as finding effective plant species that can achieve successful site clean-up despite the extreme environmental conditions and with minimal site management. A long-term assessment of phytoremediation was performed which capitalized on a study established in Fairbanks in 1995. The original study sought to determine how the introduction of plants (Festuca rubra, Lolium multiflorum), nutrients (fertilizer), or their combination would affect degradation of petroleum hydrocarbon (TPH) contaminated soils (crude oil or diesel) over time. Within the year following initial treatments, the plots subjected to both planting and/or fertilization showed greater overall decreases in TPH concentrations in both the diesel and crude oil contaminated soils relative to untreated plots. We re-examined this field site after 15 years with no active site management to assess the long-term effects of phytoremediation on colonization by native and non-native plants, their rhizosphere microbial communities and on petroleum removal from soil. Native and non-native vegetation had extensively colonized the site, with more abundant vegetation found on the diesel contaminated soils than the more nutrient-poor, more coarse, and acidic crude oil contaminated soils. TPH concentrations achieved regulatory clean up levels in all treatment groups, with lower TPH concentrations correlating with higher amounts of woody vegetation (trees & shrubs). In addition, original treatment type has affected vegetation recruitment to each plot with woody vegetation and more native plants in unfertilized plots. Bacterial community structure also varies according to the originally applied treatments. This study suggests that initial treatment with native tree species in

  2. Polylactides in additive biomanufacturing.

    PubMed

    Poh, Patrina S P; Chhaya, Mohit P; Wunner, Felix M; De-Juan-Pardo, Elena M; Schilling, Arndt F; Schantz, Jan-Thorsten; van Griensven, Martijn; Hutmacher, Dietmar W

    2016-12-15

    New advanced manufacturing technologies under the alias of additive biomanufacturing allow the design and fabrication of a range of products from pre-operative models, cutting guides and medical devices to scaffolds. The process of printing in 3 dimensions of cells, extracellular matrix (ECM) and biomaterials (bioinks, powders, etc.) to generate in vitro and/or in vivo tissue analogue structures has been termed bioprinting. To further advance in additive biomanufacturing, there are many aspects that we can learn from the wider additive manufacturing (AM) industry, which have progressed tremendously since its introduction into the manufacturing sector. First, this review gives an overview of additive manufacturing and both industry and academia efforts in addressing specific challenges in the AM technologies to drive toward AM-enabled industrial revolution. After which, considerations of poly(lactides) as a biomaterial in additive biomanufacturing are discussed. Challenges in wider additive biomanufacturing field are discussed in terms of (a) biomaterials; (b) computer-aided design, engineering and manufacturing; (c) AM and additive biomanufacturing printers hardware; and (d) system integration. Finally, the outlook for additive biomanufacturing was discussed.

  3. Additive Manufactured Product Integrity

    NASA Technical Reports Server (NTRS)

    Waller, Jess; Wells, Doug; James, Steve; Nichols, Charles

    2017-01-01

    NASA is providing key leadership in an international effort linking NASA and non-NASA resources to speed adoption of additive manufacturing (AM) to meet NASA's mission goals. Participants include industry, NASA's space partners, other government agencies, standards organizations and academia. Nondestructive Evaluation (NDE) is identified as a universal need for all aspects of additive manufacturing.

  4. Pesticide residues in chicken eggs - A sample preparation methodology for analysis by gas and liquid chromatography/tandem mass spectrometry.

    PubMed

    Hildmann, Fanny; Gottert, Christina; Frenzel, Thomas; Kempe, Guenther; Speer, Karl

    2015-07-17

    A sample preparation method was developed for the analysis of chicken eggs to determine 97 GC and 81 LC amenable residues, including organophosphates, organochlorines, pyrethroids, triazoles, carboxyl-containing compounds, and the indicator PCBs. Hereby, considerations were given to the recoveries of the analytes, the method's suitability for routine analysis, and the assessment of the clean-up effect, for which a simple thin layer chromatography was implemented to visualize the most important lipid classes. The procedure consisted of (I) the extraction by matrix solid phase dispersion, and the clean-up by means of (II) small-scale gel permeation chromatography (GPC) and (III) two different solid phase extractions (SPE) for GC and LC amenable analytes, as well as (IV) the quantification using GC-MS/MS and LC-MS/MS. Cyclohexane/ethyl acetate was chosen as extraction solvent due to its suitability for extracting strong non-polar but also more polar analytes. The classical GPC was scaled down to ensure a 50% lower solvent consumption. The comprehensive investigation of conventional and modern zirconium-oxide-coated SPE materials resulted in the selection of octadecyl-modified silica (C18) combined with primary secondary amine using acetonitrile as elution solvent for GC amenable analytes and pure C18 in combination with acidified methanol for LC amenable pesticides. Compared to the currently established EN 1528 method the sample preparation proposed offered a higher sample throughput and a lower solvent consumption. Furthermore, for the first time the clean-up effectiveness of the sample preparation steps was documented as shown by means of thin-layer chromatography. The validation of chicken eggs proved the fulfillment of the quality control criteria for 164 of the 178 analytes tested, mostly at the lowest validated level of 5μg/kg for pesticides and 0.5μg/kg for the single indicator PCBs. However, the analysis of strongly polar analytes was still problematic

  5. Lunar Sample Compendium

    NASA Technical Reports Server (NTRS)

    Meyer, C.

    2009-01-01

    The Lunar Sample Compendium is a succinct summary of what has been learned from the study of Apollo and Luna samples of the Moon. Basic information is compiled, sample-by-sample, in the form of an advanced catalog in order to provide a basic description of each sample. Information presented is carefully attributed to the original source publication, thus the Compendium also serves as a ready access to the now vast scientific literature pertaining to lunar smples. The Lunar Sample Compendium is a work in progress (and may always be). Future plans include: adding sections on additional samples, adding new thin section photomicrographs, replacing the faded photographs with newly digitized photos from the original negatives, attempting to correct the age data using modern decay constants, adding references to each section, and adding an internal search engine.

  6. Recent developments in sample preparation techniques for chromatography analysis of traditional Chinese medicines.

    PubMed

    Deng, Chunhui; Liu, Ning; Gao, Mingxia; Zhang, Xiangmin

    2007-06-15

    Traditional Chinese medicines (TCMs) have a long history dating back thousands of years. Recently, there has been increasing interest worldwide in the use of TCMs for the prevention and treatment of various illnesses. In China, a large number of analytical tools, especially chromatographic techniques have been used to analyze the constituents of TCMs in order to control their quality and discover new bioactive compounds. In this paper, recent developments in sample preparation techniques for the extraction, clean-up, and concentration of analytes from TCMs are compared. These techniques include headspace solid-phase microextraction (HS-SPME), headspace liquid-phase microextraction (HS-LPME), microwave-assisted extraction (MAE), supercritical-fluid extraction (SFE), pressurized-liquid extraction (PLE), and microwave distillation (MD).

  7. Elevating sampling

    PubMed Central

    Labuz, Joseph M.; Takayama, Shuichi

    2014-01-01

    Sampling – the process of collecting, preparing, and introducing an appropriate volume element (voxel) into a system – is often under appreciated and pushed behind the scenes in lab-on-a-chip research. What often stands in the way between proof-of-principle demonstrations of potentially exciting technology and its broader dissemination and actual use, however, is the effectiveness of sample collection and preparation. The power of micro- and nanofluidics to improve reactions, sensing, separation, and cell culture cannot be accessed if sampling is not equally efficient and reliable. This perspective will highlight recent successes as well as assess current challenges and opportunities in this area. PMID:24781100

  8. Cleaning up after ICH: the role of Nrf2 in modulating microglia function and hematoma clearance

    PubMed Central

    Zhao, Xiurong; Sun, Guanghua; Ting, Shun-Ming; Song, Shen; Zhang, Jie; Edwards, Nancy J; Aronowski, Jaroslaw

    2014-01-01

    As a consequence of intracerebral hemorrhage (ICH), blood components enter brain parenchyma causing progressive damage to the surrounding brain. Unless hematoma is cleared, the reservoirs of blood continue to inflict injury to neurovascular structures and blunt the brain repair processes. Microglia/macrophages (MM Φ) represent the primary phagocytic system that mediates the cleanup of hematoma. Thus the efficacy of phagocytic function by MM Φ is an essential step in limiting ICH-mediated damage. By using primary microglia to model red blood cell (main component of hematoma) clearance, we studied the role of transcription factor Nrf2, a master-regulator of anti-oxidative defense, in the hematoma clearance process. We showed that in cultured microglia, activators of Nrf2 1) induce anti-oxidative defense components, 2) reduce peroxide formation, 3) upregulate phagocytosis-mediating scavenger receptor CD36, and 4) enhance RBC phagocytosis. Through inhibiting Nrf2 or CD36 in microglia, by DNA-decoy or neutralizing antibody, we documented the important role of Nrf2 and CD36 in RBC phagocytosis. Using autologous blood injection ICH model to measure hematoma resolution, we showed that Nrf2 activator, sulforaphane, injected to animals after the onset of ICH, induced CD36 expression in ICH-affected brain and improved hematoma clearance in rats and wild-type mice, but expectedly not in Nrf2-knockout-(KO) mice. Normal hematoma clearance was impaired in Nrf2-KO mice. Our experiments suggest that Nrf2 in microglia play an important role in augmenting the anti-oxidative capacity, phagocytosis and hematoma clearance after ICH. PMID:25328080

  9. ACCESSING FEDERAL DATA BASES FOR CONTAMINATED SITE CLEAN-UP TECHNOLOGIES

    EPA Science Inventory

    The Federal Remediation Technologies Roundtable (Roundtable) eveloped this publication to provide information on accessing Federal data bases that contain data on innovative remediation technologies. The Roundtable includes representatives from the Department of Defense (DoD), En...

  10. Final Report, University Research Program in Robotics (URPR), Nuclear Facilities Clean-up

    SciTech Connect

    Tesar, Delbert; Kapoor, Chetan; Pryor, Mitch

    2005-03-31

    This final report describes the research activity at the University of Texas at Austin with application to EM needs at DOE. This research activity is divided in to two major thrusts and contributes to the overall University Research Program in Robotics (URPR) thrust by providing mechanically oriented robotic solutions based on modularity and generalized software. These thrusts are also the core strengths of the UTA program that has a 40-year history in machine development, 30 years specifically devoted to robotics. Since 1975, much of this effort has been to establish the general analytical and design infrastructure for an open (modular) architecture of systems with many degrees of freedom that are able to satisfy a broad range of applications for future production machines. This work has coalesced from two principal areas: standardized actuators and generalized software.

  11. Code regenerative clean-up loop transponder for a mu-type ranging system

    NASA Technical Reports Server (NTRS)

    Hurd, W. J. (Inventor)

    1973-01-01

    A loop transponder for regenerating the code of a mu type ranging system is disclosed. It includes a phase locked loop, a code generator, and a loop detector. The function of the phase locked loop is to provide phase lock between a received component wk of the range signal and a replica rafter wk of the received component, provided by the code generator. The code generator also provides a replica of the next component rafter w(w+1). The loop detector responds to wk rafler wk and rafter w(k+1) to determine when the next component w(k+1) is received and controls the code generator to supply w(k+1) to the phase locked loop and to generate a replica rafter w(k+2) of the next component.

  12. Phytoremediation: using green plants to clean up contaminate soil, groundwater, and wastewater

    SciTech Connect

    Negri, M.C.; Hinchman, R.R.; Gatliff, E.G.

    1996-07-01

    Phytoremediation, an emerging cleanup technology for contaminated soils, groundwater, and wastewater that is both low-tech and low-cost, is defined as the engineered use of green plants (including grasses, forbs, and woody species) to remove, contain, or render harmless such environmental contaminants as heavy metals, trace elements, organic compounds and radioactive compounds in soil or water. Our research includes a successful field demonstration of a plant bioreactor for processing the salty wastewater from petroleum wells; the demonstration is currently under way at a natural gas well site in Oklahoma, in cooperation with Devon Energy Corporation. A greenhouse experiment on zinc uptake in hybrid poplar (Populus sp.) was initiated in 1995. These experiments are being conducted to confirm and extend field data indicating high levels of zinc (4,200 ppm) in leaves of hybrid poplar growing as a cleanup system at a site with zinc contamination in the root zone of some of the trees. Analyses of soil water from experimental pots that had received several doses of zinc indicated that the zinc was totally sequestered by the plants in about 4 hours during a single pass through the root system. The data also showed concentrations of sequestered metal of >38,000 ppm Zn in the dry root tissue. These levels of sequestered zinc exceed the levels found in either roots or tops of many of the known ``hyperaccumulator`` species. Because the roots sequester most of the contaminant taken up in most plants, a major objective of this program is to determine the feasibility of root harvesting as a method to maximize the removal of contaminants from soils. Available techniques and equipment for harvesting plant roots, including young tree roots, are being evaluated and modified as necessary for use with phytoremediation plants.

  13. Battelle Research Outlook, Volume 2 Number 3. Cleaning Up the Atmosphere.

    ERIC Educational Resources Information Center

    Westerman, Arthur B., Ed.

    "Outlook" publications focus on areas of science and technology in which research can be valuable to industry, government, and society as a whole. This issue deals with the problems of air pullution and air quality control. The first of six essays,". . . This Most Excellent Canopy, the Air," prognosticates the surge in atmospheric pollution and…

  14. Multiple rate digital command detection system with range clean-up capability

    NASA Technical Reports Server (NTRS)

    Lesh, J. R.; Butman, S. A. (Inventor)

    1977-01-01

    A multi-rate digital command system is disclosed which uses the composite signal of a mu-type ranging system as a subcarrier to transmit range codes and data from a station to a receiver where the range codes are sequentially phase modulated on a subcarrier of frequency by one of its own subharmonics and data is phase modulated on a selected ranging component. A range cleanup loop in a spacecraft locks the phase of a locally generated reference component to a received ranging component and retransmits the component to a ground station. When the inverse phase of a ranging component is received and detected, the cleanup loop is modified to demodulate phase modulated command symbols while continuing tracking the same ranging component. The command symbol rate is coherently related to the ranging signal component bit rate.

  15. Cleaning up Water? Or Building Rural Community? Community Watershed Organizations in Pennsylvania

    ERIC Educational Resources Information Center

    Stedman, Richard; Lee, Brian; Brasier, Kathryn; Weigle, Jason L.; Higdon, Francis

    2009-01-01

    Recent initiatives from state and federal government agencies have helped foster the formation of community-based watershed organizations. Although there is a great deal of enthusiasm about the potential of these organizations to enhance water quality, relatively little attention has been paid to the impacts these organizations may have on the…

  16. Colleges Must Clean up Their Athletics Programs or Face Professionalization, NCAA President Says.

    ERIC Educational Resources Information Center

    Farrell, Charles S.

    1987-01-01

    Wilford S. Bailey of Auburn University is heading the National Collegiate Athletic Association as it struggles to cope with several controversial issues: testing athletes for drug abuse, new academic standards for freshman athletes, the role of college presidents in governing sports, and the integrity of college athletics. (MLW)

  17. Synthesis and characterization of low viscosity carbon dioxide binding organic liquids for flue gas clean up

    SciTech Connect

    Koech, Phillip K.; Malhotra, Deepika; Heldebrant, David J.; Cantu Cantu, David; Glezakou, Vassiliki Alexandra; Rousseau, Roger J.

    2015-01-01

    Climate change is partly attributed to global anthropogenic carbon dioxide (CO2) emission to the atmosphere. These environmental effects can be mitigated by CO2 capture, utilization and storage. Alkanolamine solvents, such as monoethanolamine (MEA), which bind CO2 as carbamates or bicarbonate salts are used for CO2 capture in niche applications. These solvents consist of approximately 30 wt% of MEA in water, exhibiting a low, CO2-rich viscosity, fast kinetics and favorable thermodynamics. However, these solvents have low CO2 capacity and high heat capacity of water, resulting in prohibitively high costs of thermal solvent regeneration. Effective capture of the enormous amounts of CO2 produced by coal-fired plants requires a material with high CO2 capacity and low regeneration energy requirements. To this end, several water-lean transformational solvents systems have been developed in order to reduce these energy penalties. These technologies include nano-material organic hybrids (NOHMs), task-specific, protic and conventional ionic liquids, phase change solvents. As part of an ongoing program in our group, we have developed new water lean transformational solvents known as CO2 binding organic liquids (CO2BOLs) which have the potential to be energy efficient CO2 capture solvents. These solvents, also known as switchable ionic liquids meaning, are organic solvents that can reversibly transform from non- ionic to ionic form and back. The zwitterionic state in these liquids is formed when low polarity non-ionic alkanolguanidines or alkanolamidines react with CO2 or SO2 to form ionic liquids with high polarity. These polar ionic liquids can be thermally converted to the less polar non-ionic solvent by releasing CO2.

  18. CUTBA (Cleaning Up the Tower of Babel of Acronyms) in IBA

    NASA Astrophysics Data System (ADS)

    Amsel, G.

    1996-09-01

    The various techniques used in ion beam analysis (IBA) are referred to by names that are often abbreviated into acronyms. While some contractions like RBS, NRA or PIXE are well established, one observes in recent literature an increasing trend to introduce new ad hoc acronyms for specific applications or techniques, although names already exist that may be adapted to correspond rather accurately to the concept. In the present situation even people well informed of this field have more and more difficulties to understand what is meant by, for example, ESS, PES, HIRBS, CERDA, CCM or CSTIM. This is especially true when the acronyms are used in titles or abstracts, without definition. To deal with this situation a list of acronyms encountered in recent literature was submitted by electronic mail consultation to a large panel of physicists active in the IBA field. The outcome of this electronic forum was discussed at a workshop held at the IBA-12 conference. Useful recommendations have been worked out to facilitate understanding of IBA-related acronyms, a consensus having been reached to lay down some not overly rigid guidelines.

  19. Reusing Cleaned Up Superfund Sites: Ecological Use Where Waste is Left on Site

    EPA Pesticide Factsheets

    The report draws from experiences at completedand current reuse projects, EPA technical guidance, and other sources to describe ecosystem characteristics and remediation approaches that have been used to accommodate ecological usesat Superfund sites wher

  20. Phytoremediation: Using green plants to clean up contaminated soil, groundwater, and wastewater

    SciTech Connect

    Negri, M.C.; Hinchman, R.R.

    1996-05-01

    Phytoremediation, an emerging cleanup technology for contaminated soils, groundwater, and wastewater that is both low-tech and low-cost, is defined as the engineered use of green plants (including grasses, forbs, and woody species) to remove, contain, or render harmless such environmental contaminants as heavy metals, trace elements, organic compounds ({open_quotes}organics{close_quotes}), and radioactive compounds in soil or water. Current research at Argonne National Laboratory includes a successful field demonstration of a plant bioreactor for processing the salty wastewater from petroleum wells; the demonstration is currently under way at a natural gas well site in Oklahoma, in cooperation with Devon Energy Corporation. A greenhouse experiment on zinc uptake in hybrid poplar (Populus sp.) was initiated in 1995. These experiments are being conducted to confirm and extend field data from Applied Natural Sciences, Inc. (our CRADA partner), indicating high levels of zinc (4,200 ppm) in leaves of hybrid poplar growing as a cleanup system at a site with zinc contamination in the root zone of some of the trees. Analyses of soil water from experimental pots that had received several doses of zinc indicated that the zinc was totally sequestered by the plants in about 4 hours during a single pass through the root system. The data also showed concentrations of sequestered metal of >38,000 ppm Zn in the dry root tissue. These levels of sequestered zinc exceed the levels found in either roots or tops of many of the known {open_quotes}hyperaccumulator{close_quotes} species. Because the roots sequester most of the contaminant taken up in most plants, a major objective of this program is to determine the feasibility of root harvesting as a method to maximize the removal of contaminants from soils. Available techniques and equipment for harvesting plant roots, including young tree roots, are being evaluated and modified as necessary for use with phytoremediation plants.

  1. ASSESSMENT OF LIQUID EMULSION MEMBRANE FOR CLEAN UP OF AQUEOUS WASTE EFFLUENTS FROM HAZARDOUS ELEMENTS

    SciTech Connect

    El-Reefy, Sohair A.; Selim, Y.T.; Hassan, M.A.; Aly, H.F.

    2003-02-27

    Four liquid emulsion membrane (LEM) systems are given to remove different hazardous elements such as uranium, thorium, cobalt, copper, lead, and cadmium from different aqueous waste effluents. The optimum conditions for use of these systems are deduced. The potentiality of LEM for removal of hazardous pollutants from aqueous waste solutions is given.

  2. Comments on Hanford 2012 Accelerating Clean Up and Shrinking the Site

    SciTech Connect

    SHERMAN, Y.T.

    2001-01-01

    In the late summer of 2000, the Department of Energy Richland Operations Office (RL) Manager, Keith Klein, announced his approach to cleanup of the Hanford Site in a document called ''Done in a Decade.'' He asked for comments and suggestions to improve the plan from employees and stakeholders. We received over 300 individual comments. Several of the comments and the Hanford Advisory Board objected to the title of the plan, leading us to change it to ''Hanford 2012 Accelerating Cleanup and Shrinking the Site.'' We addressed virtually all substantive comments, i.e. those that recommended a change in the text, better understanding of an Issue, or consideration of a new Mea, and incorporated editorial comments where appropriate. We thank all those who took time to comment. The new plan, ''Hanford 2012'', is a much better document because you did so. You will notice some things about the table: Comments are not quoted verbatim--most were paraphrased to conserve space; Comments were separated into one of four sections: general, the River, the Plateau, the Future; Commenters are not identified by name or organization; Comments are generally listed in the order in which they were received, several comments were repetitive, but differed slightly so we made an effort to respond to each one, despite apparent repetition; There are many acronyms used at the Hanford Site, most of which can be found on the Web at http:/Ewww.hanford.gov/acronyml. We have attempted to spell out each acronym the first time it's used in a comment/response with the following exceptions: DOE--Department of Energy; RL--Department of Energy, Richland Operations Office; and ORP--Department of Energy, Office of River Protection.

  3. Environmental remediation 1991: ``Cleaning up the environment for the 21st Century``. Proceedings

    SciTech Connect

    Wood, D.E.

    1991-12-31

    This report presents discussions given at a conference on environmental remediation, September 8--11, Pasco, Washington. Topics include: public confidence; education; in-situ remediation; Hanford tank operations; risk assessments; field experiences; standards; site characterization and monitoring; technology discussions; regulatory issues; compliance; and the UMTRA project. Individual projects are processed separately for the data bases.

  4. Cleaning up our act: Alternatives for hazardous solvents used in cleaning

    SciTech Connect

    Shoemaker, J.D.; Meltzer, M.; Miscovich, D.; Montoya, D.; Goodrich, P.; Blycker, G.

    1994-01-01

    Lawrence Livermore National Laboratory (LLNL) has studied more than 70 alternative cleaners as potential replacements for chlorofluorocarbons (CFCs), halogenated hydrocarbons (e.g., trichloroethylene and trichloroethane), hydrocarbons (e.g., toluene and Stoddard Solvent), and volatile organic compounds (e.g., acetone, alcohols). This report summarizes LLNL`s findings after testing more than 45 proprietary formulations on bench-scale testing equipment and in more than 60 actual shops and laboratories. Cleaning applications included electronics fabrication, machine shops, optical lenses and hardware, and general cleaning. Most of the alternative cleaners are safer than the solvents previously used and many are nonhazardous, according to regulatory criteria.

  5. TECHNICAL APPROACHES TO CHARACTERIZING AND CLEANING UP AUTOMOTIVE REPAIR SITES UNDER THE BROWNFIELDS INITIATIVE

    EPA Science Inventory

    The document provides brownfields planners with an overview of the technical methods that can be used to achieve successful site assessment and cleanup which are two key components of the brownfields redevelopment process. No two brownfields sites are identical and planners will...

  6. TECHNICAL APPROACHES TO CHARACTERIZING AND CLEANING UP METAL FINISHING SITES UNDER THE BROWNFIELDS INITIATIVE

    EPA Science Inventory

    The document provides brownfields planners with an overview of the technical methods that can be used to achieve successful site assessment and cleanup which are two key components of the brownfields redevelopment process. No two brownfields sites are identical and planners will...

  7. SOx-NOx-Rox Box{trademark} flue gas clean-up demonstration. Final report

    SciTech Connect

    1995-09-01

    Babcock and Wilcox`s (B and W) SOx-NOx-Rox Box{trademark} process effectively removes SOx, NOx and particulate (Rox) from flue gas generated from coal-fired boilers in a single unit operation, a high temperature baghouse. The SNRB technology utilizes dry sorbent injection upstream of the baghouse for removal of SOx and ammonia injection upstream of a zeolitic selective catalytic reduction (SCR) catalyst incorporated in the baghouse to reduce NOx emissions. Because the SOx and NOx removal processes require operation at elevated gas temperatures (800--900 F) for high removal efficiency, high-temperature fabric filter bags are used in the baghouse. The SNRB technology evolved from the bench and laboratory pilot scale to be successfully demonstrated at the 5-MWe field scale. This report represents the completion of Milestone M14 as specified in the Work Plan. B and W tested the SNRB pollution control system at a 5-MWe demonstration facility at Ohio Edison`s R.E. Burger Plant located near Shadyside, Ohio. The design and operation were influenced by the results from laboratory pilot testing at B and W`s Alliance Research Center. The intent was to demonstrate the commercial feasibility of the SNRB process. The SNRB facility treated a 30,000 ACFM flue gas slipstream from Boiler No. 8. Operation of the facility began in May 1992 and was completed in May 1993. About 2,300 hours of high-temperature operation were achieved. The main emissions control performance goals of: greater than 70% SO{sub 2} removal using a calcium-based sorbent; greater than 90% NOx removal with minimal ammonia slip; and particulate emissions in compliance with the New Source Performance Standards (NSPS) of 0.03 lb/million Btu were exceeded simultaneously in the demonstration program when the facility was operated at optimal conditions. Testing also showed significant reductions in emissions of some hazardous air pollutants.

  8. TECHNICAL APPROACHES TO CHARACTERIZING AND CLEANING UP BROWNFIELDS SITES: PULP AND PAPER MILLS

    EPA Science Inventory

    This guidance document gives assistance to communities, decision-makers, states and municipalities, academia, and the private sector to address issues related to the redevelopment of Brownfields sites, specifically pulp and paper mills sites. The document helps users to understan...

  9. TECHNICAL APPROACHES TO CHARACTERIZING AND CLEANING UP BROWNFIELDS SITES: RAILROAD YARDS

    EPA Science Inventory

    This guidance document gives assistance to communities, decision-makers, states and municipalities, academia, and the private sector to address issues related to the redevelopment of Brownfields sites, specifically railroad yards. The document helps users to understand the proble...

  10. EPA Signs Two Clean Up Decisions in a Continued Effort to Protect Cape Cod Drinking Water

    EPA Pesticide Factsheets

    In its ongoing efforts to protect the Cape Cod aquifer from contamination from historical military training activities, the U.S. Environmental Protection Agency (EPA) has issued final cleanup strategies for two contaminated areas at Camp Edwards.

  11. Integrating Sediment Clean Up and Watershed Management for Sinclair and Dyes Inlets, WA USA

    DTIC Science & Technology

    2005-01-01

    Naval Research 2004 Annual Report. KCHD (Kitsap County Health District). 2002. Water Quality Program 2000-2001 WATER QUALITY MONITORING REPORT...Sherrell, R.K. Johnston, F. Meriwether , T. Determan, W. Kendra, S. Magoon, S. Whitford, and J. Zimney. 2003. Assessment of Bacterial Contamination in...Bay, BC, SSWM (Kitsap County Public Works Surface and Stormwater Management). 2003. Annual Report 2003. US EPA 2000. EPA Superfund Record of

  12. High intensity magnetic separation for the clean-up of a site polluted by lead metallurgy.

    PubMed

    Sierra, C; Martínez, J; Menéndez-Aguado, J M; Afif, E; Gallego, J R

    2013-03-15

    The industrial history in the district of Linares (Spain) has had a severe impact on soil quality. Here we examined soil contaminated by lead and other heavy metals in "La Cruz" site, a brownfield affected by metallurgical residues. Initially, the presence of contaminants mainly associated with the presence of lead slag fragments mixed with the soil was evaluated. The subsequent analysis showed a quasi-uniform distribution of the pollution irrespective of the grain-size fractions. This study was accompanied by a characterization of the lead slag behavior under the presence of a magnetic field. Two main magnetic components were detected: first a ferromagnetic and/or ferrimagnetic contribution, second a paramagnetic and/or antiferromagnetic one. It was also established that the slag was composed mainly of lead spherules and iron oxides embedded in a silicate matrix. Under these conditions, the capacity of magnetic separation to remove pollutants was examined. Therefore, two high intensity magnetic separators (dry and wet devices, respectively) were used. Dry separation proved to be successful at decontaminating soil in the first stages of a soil washing plant. In contrast, wet separation was found effective as a post-process for the finer fractions.

  13. EPA Awards Pulaski County $350,000 to Clean up Contaminated Brownfields Sites

    EPA Pesticide Factsheets

    DALLAS - (Sept. 23, 2015) The U.S. Environmental Protection Agency (EPA) is awarding $350,000 in supplemental funding to clean contaminated sites in Pulaski County, Ark. The county plans to use the funding to clean Full Counsel and Sterling building

  14. Relevance of Nuclear Weapons Clean-Up Experience to Dirty Bomb Response

    SciTech Connect

    Vantine, H C; Crites, T R

    2002-08-19

    During the past 50 years, the United States has experienced 32 major nuclear weapons accidents, nine of which released special nuclear material to the environment. Response to these accidents, coupled with recovery experience following the Russian satellite reentry and weapons test site cleanup, form the basis for determining actions that might be required following a nuclear terrorist event involving the release of radioactive material. Though valuable information has been gained following the recovery from various commercial accidents, most notably the Chernobyl nuclear power plant failure and the dismantled radiography source in the Brazilian city of Goi nia, this paper will focus on the lessons learned from the U.S. nuclear weapons program.

  15. Reaching Part Per Trillion Clean-Up Criteria for Mercury in Water

    SciTech Connect

    Klasson, K. T.; Kosny, K.; Drescher, S. R.; Southworth, G. R.; Hensley, J. F.

    2003-02-24

    In the last couple of years, emphasis on environmental mercury contamination and elimination of mercury use has increased. The U.S. Department of Energy has for many decades maintained a stockpile of elemental mercury for operations and, as a consequence of its routine use, spills have occurred. These historical spills have resulted in some contamination of water streams and soils. In this work we examine a newly developed technique for removal of mercury from contaminated groundwater. In this application the mercury concentration was approximately 2.3 parts per billion and the treatment criterion was 200 parts per trillion. Several forms of mercury species contributed to the contamination. The treatment technique developed for this water was to convert all forms of mercury, through a series of fast chemical reactions, to elemental mercury, which was air-stripped from the water. This paper presents preliminary laboratory work on the method.

  16. Use of magnetic carbon composites from renewable resource materials for oil spill clean up and recovery

    DOEpatents

    Viswanathan, Tito

    2014-02-11

    A method for separating a liquid hydrocarbon material from a body of water. In one embodiment, the method includes the steps of mixing a plurality of magnetic carbon-metal nanocomposites with a liquid hydrocarbon material dispersed in a body of water to allow the plurality of magnetic carbon-metal nanocomposites each to be adhered by an amount of the liquid hydrocarbon material to form a mixture, applying a magnetic force to the mixture to attract the plurality of magnetic carbon-metal nanocomposites each adhered by an amount of the liquid hydrocarbon material, and removing said plurality of magnetic carbon-metal nanocomposites each adhered by an amount of the liquid hydrocarbon material from said body of water while maintaining the applied magnetic force, wherein the plurality of magnetic carbon-metal nanocomposites is formed by subjecting one or more metal lignosulfonates or metal salts to microwave radiation, in presence of lignin/derivatives either in presence of alkali or a microwave absorbing material.

  17. From cleaning up to helping out: parental socialization and children's early prosocial behavior.

    PubMed

    Pettygrove, Dana M; Hammond, Stuart I; Karahuta, Erin L; Waugh, Whitney E; Brownell, Celia A

    2013-12-01

    Relations between parental socialization and infants' prosocial behavior were investigated in sixty three 18- and 30-month old children. Parents' socialization techniques (e.g., directives, negotiation, reasoning) differed for the two age groups, as did relations between socialization and different forms of emerging prosocial behavior (helping; sharing).

  18. WhoKnows? Evaluating Linked Data Heuristics with a Quiz that Cleans up DBpedia

    ERIC Educational Resources Information Center

    Waitelonis, Jorg; Ludwig, Nadine; Knuth, Magnus; Sack, Harald

    2011-01-01

    Purpose: Linking Open Data (LOD) provides a vast amount of well structured semantic information, but many inconsistencies may occur, especially if the data are generated with the help of automated methods. Data cleansing approaches enable detection of inconsistencies and overhauling of affected data sets, but they are difficult to apply…

  19. Ground truth and detection threshold from WWII naval clean-up in Denmark

    NASA Astrophysics Data System (ADS)

    Larsen, Tine B.; Dahl-Jensen, Trine; Voss, Peter

    2013-04-01

    The sea bed below the Danish territorial waters is still littered with unexploded mines and other ammunition from World War II. The mines were air dropped by the RAF and the positions of the mines are unknown. As the mines still pose a potential threat to fishery and other marine activities, the Admiral Danish Fleet under the Danish Navy searches for the mines and destroy them by detonation, where they are found. The largest mines destroyed in this manner in 2012 are equivalent to 800 kg TNT each. The Seismological Service at the National Geological Survey of Denmark and Greenland is notified by the navy when ammunition in excess of 100 kg TNT is detonated. The notifications include information about position, detonation time and the estimated amount of explosives. The larger explosions are clearly registered not only on the Danish seismographs, but also on seismographs in the neighbouring countries. This includes the large seismograph arrays in Norway, Sweden, and Finland. Until recently the information from the Danish navy was only utilized to rid the Danish earthquake catalogue of explosions. But the high quality information provided by the navy enables us to use these ground truth events to assess the quality of our earthquake catalogue. The mines are scattered though out the Danish territorial waters, thus we can use the explosions to test the accuracy of the determined epicentres in all parts of the country. E.g. a detonation of 135 kg in Begstrup Vig in the central part of Denmark was located using Danish, Norwegian and Swedish stations with an accuracy of less than 2 km from ground truth. A systematic study of the explosions will sharpen our understanding of the seismicity in Denmark, and result in a more detailed understanding of the detection threshold. Furthermore the study will shed light on the sensitivity of the network to various seismograph outages.

  20. Clean-up of lead in household carpet and floor dust.

    PubMed

    Ewers, L; Clark, S; Menrath, W; Succop, P; Bornschein, R

    1994-07-01

    Methods to remove lead-containing dust were tested on carpets from homes of children with high blood lead and on new carpets artificially contaminated in the laboratory. The household carpets could not be cleaned effectively by repetitive vacuuming with HEPA-filtered cleaners. The lead concentration in the removed dust remained about the same from the initial cleaning (1 min/m2) to the final cleaning (total cleaning time of 10 min/m2). The lead loading on the surface of the carpets often increased during cleaning because vacuuming brought lead from deeper in the carpet to the surface. Over 95% of the total dust was removed from bare wooden floors by dry vacuuming (5 min/m2). For linoleum, more than 75% was removed by vacuuming for 5 min/m2. However, little was removed in vacuuming after the initial two minutes and about 20% was removed in a final wet-washing step. HEPA-vacuuming of the laboratory-contaminated carpets revealed that two of the commercially available vacuum cleaners tested were essentially equivalent and each removed significantly more dust than a third vacuum during a total cleaning time of 10 min/m2. Cleaning for 6 min/m2 was necessary to remove more than 70% of the embedded dust by the two more efficient vacuums. Cleaning efficiencies were about the same for short pile and sculptured carpets. It was concluded that it may be more practical to replace rather than clean carpets. HEPA-vacuum cleaning of carpets was shown to increase lead dust on the surface under some conditions.

  1. Groundwater Contamination: DOD Uses and Develops a Range of Remediation Technologies to Clean Up Military Sites

    DTIC Science & Technology

    2005-06-01

    barriers X X X X X Phytoremediation X X X X Thermal treatments X X X X Ex-situ Advanced oxidation processes X X X X Air stripping...6 Figure 2: Selected Phases and Milestones in DOD’s Environmental Cleanup Process 8 Figure 3: Example of a Conventional Pump-and-Treat System 12Page...biological, chemical, or physical processes to treat the contaminated groundwater underground (in-situ). 2The Navy oversees environmental restoration

  2. Cockroach Clean-Up Tour . Urban Pest Management. Teaching Environmental Living Skills to Elementary Students.

    ERIC Educational Resources Information Center

    Cowles, Kathleen Letcher

    Integrated Pest Management (IPM), a decision-making approach to pest control, is designed to help individuals decide if pest suppression treatments are necessary, when they should be initiated, where they should be applied, and what strategy/mix of tatics to use. IPM combines a variety of approaches with which to manage pests, including human…

  3. EPA Science Matters Newsletter: Advancing Ways to Clean Up Drinking Water Systems (Published November 2013)

    EPA Pesticide Factsheets

    To advance the science and engineering of decontaminating pipe systems and safely disposing of high-volumes of contaminated water, Agency homeland security researchers are developing a Water Security Test Bed (WSTB).

  4. Report: Environmental Justice Concerns and Communication Problems Complicated Cleaning Up Ringwood Mines/Landfill Site

    EPA Pesticide Factsheets

    Report #2007-P-00016, April 2, 2007. We did not find evidence to indicate that the EPA's decision making to investigate environmental conditions at the Ringwood Mines/Landfill site were affected by the area’s racial, cultural, or socioeconomic status.

  5. Social and psychological state of the Chornobyl clean up workers. Risk factors for negative changes.

    PubMed

    Buzunov, V O; Loganovsky, K N; Krasnikova, L I; Bomko, M O; Belyaev, Yu M; Yaroshenko, Zh S; Domashevska, T Ye

    2016-12-01

    It is generally recognized that the Chornobyl nuclear accident caused strong psychosocial stress affecting the entire population of Ukraine, primarily people involved in recovery operations. But what are the reasons? What is the struc ture of stressors? What are their social, medical and biological consequences, what are strategy and preventive meas ures? Issues that require special research and development.

  6. Beam Clean-Up and Combining via Stimulated Scattering in Liquid Crystals

    DTIC Science & Technology

    2007-11-02

    3 High-power CW solid-state and fiber lasers are here ! They have the power more...Experiment.) d kα 14 Observation of Stimulated Grating Orientational Scattering in NLC λ = 1.08 mkm, Yb-doped IPG fiber laser , output power 100 W...1.08 mkm, Yb-doped IPG fiber laser , output power 100 W, power to the cell 3.2 W. Lens F = 20 cm, beam ∅ = 5 mm (FWe-2M) at the lens. Cell

  7. Initial operation of the Tidd PFBC hot gas clean up filter

    SciTech Connect

    Mudd, M.J.; Hoffman, J.D.

    1993-09-01

    The objective of this program is to evaluate the design and obtain operating experience for up to two Advanced Particle Filter (APF) systems through long-term testing on a slipstream at Ohio Power Company`s Tidd PFBC Demonstration Plant. Performance and reliability of commercial-scale filter modules will be monitored to aid in an assessment of the readiness and economic viability of this technology for commercial PFBC applications.

  8. Use of magnetic carbon composites from renewable resource materials for oil spill clean up and recovery

    DOEpatents

    Viswanathan, Tito

    2015-10-27

    A method of separating a liquid hydrocarbon material from a body of water, includes: (a) mixing magnetic carbon-metal nanocomposites with a liquid hydrocarbon material dispersed in a body of water to allow the magnetic carbon-metal nanocomposites each to be adhered by the liquid hydrocarbon material to form a mixture; (b) applying a magnetic force to the mixture to attract the magnetic carbon-metal nanocomposites each adhered by the liquid hydrocarbon material; and (c) removing the body of water from the magnetic carbon-metal nanocomposites each adhered by the liquid hydrocarbon material while maintaining the applied magnetic force. The magnetic carbon-metal nanocomposites is formed by subjecting one or more metal lignosulfonates or metal salts to microwave radiation, in presence of lignin/derivatives either in presence of alkali or a microwave absorbing material, for a period of time effective to allow the carbon-metal nanocomposites to be formed.

  9. Mathematical Modeling Groundwater Mercury Pollution, Post Demercuriztion Monitoring And Evaulation of Clean-up Efficiency

    EPA Science Inventory

    The aim of the model was to forecast the groundwater mercury pollution distribution aureole and to discuss the mathematical simulations of the estimated quantity of mercury entering the river Irtysh and the aquifer wells in the village of Pavlodarskoe. During the years of 1975-1...

  10. Spring is a good time to clean up your vendor contracts.

    PubMed

    Daigrepont, Jeffery

    2013-01-01

    Whether it's a new purchase or renewal, every year physicians and hospitals obligate themselves financially to vendor contracts without fully understanding the terms and conditions of their commitments. Some of these contracts renew automatically without permission or approval and come with automatic price increases. In some cases, practices may even be paying for services no longer being used or maintenance fees for support services no longer needed. However, discerning what vendor and system to select or renew, based on the unique objectives of the practice or hospital, can be overwhelming. This article provides many helpful strategies for negotiating a rock-solid contract that is a win for the physician practice or hospital and holds the vendor accountable for delivery of promises.

  11. Vestibular and acustic dysfunctions in clean up workers of Chornobyl accident (30 years of follow up).

    PubMed

    Zabolotnyi, D I; Mishchanchuk, N S

    2016-12-01

    Meta – vyvchyty kliniko elektrofiziologichni porushennia pry vestybuliarniy̆ ta akustychniy̆ dysfunktsiiakh v uchas nykiv likvidatsïï naslidkiv avariï na Chornobyl's'kiy̆ atomniy̆ elektrostantsiï v zalezhnosti vid dozy ta tryvalosti diï ionizuiuchoï radiatsiï, osoblyvosti determinovanykh efektiv vprodovzh 30 rokiv pislia avariï.Material ta metody. U 7812 uchasnykiv likvidatsiï naslidkiv avariï na ChAES (ULNA na ChAES) cholovichoï stati, u to mu chysli u 325 osib, vidibranykh dlia prolongovanykh doslidzhen', u 1986 2015 rr. provedeni standartni kliniko elektrofiziologichni obstezhennia funktsiy̆ vestybuliarnogo ta akustychnogo analizatoriv. Vykonani matematychni metody analizu iz zastosuvanniam programnykh paketiv SYSTAT, EPICURE ta EGRET.Rezul'taty. Vstanovleni vestybuliarna ta akustychna dysfunktsiï za tsentral'nym typom z progresuiuchym rozvyt kom gal'mivnykh protsesiv u stovburomozkovykh, pidkorkovo korkovykh strukturakh vestybuliarnogo ta akustychnogo analizatoriv. Vyznachena zalezhnist' zmin u tsykh strukturakh vid velychyny dozy ta tryvalosti diï ionizuiuchoï radiatsiï. Vstanovleni zakonomirnosti determinovanykh radiatsiy̆nykh efektiv u vzaiemozv'iazku z formuvanniam or ganichnoï tserebrovaskuliarnoï patologiï v ULNA na ChAES u viddaleni pisliaavariy̆ni roky, iaki uzgodzhuiut'sia z ney̆ rofiziologichnymy, MRT ta inshymy obstezhenniamy, shcho pidtverdzheno pry koreliatsiy̆nomu analizi.Vysnovky. Vidznacheno, shcho vestybuliarna ta akustychna dysfunktsiï v ULNA na ChAES proiavliaiut'sia kliniko elekt rofiziologichnymy zminamy na rivni tsentral'nykh struktur doslidzhuvanykh analizatoriv, iaki vkazuiut' na para lelizm spil'nogo mekhanizmu determinovanykh radiatsiy̆nykh efektiv pry dozi 0,20 Gr,a takozh ïkh dozozalezhnist' u dy namitsi 30 pisliaavariy̆nykh rokiv. Vstanovleno, shcho vestybuliarna dysfunktsiia v ULNA na ChAES proiavliaiet'sia klinichno ranishe, a elektroakustychni ta elektrofiziologichni zminy pry normal'nomu slukhu svidchat' pro doklinichni gal'mivni protsesy u stovburomozkovykh ta pidkorkovo korkovykh strukturakh akustychnogo analizatora u ranni pisliaavariy̆ni roky. Vyiavleni osoblyvosti klinichnogo perebigu vestybuliarnoï ta akustychnoï dysfunktsiy̆ pry dovgotryvalomu monitoryngu pry korotkochasniy̆ diï ionizuiuchoï radiatsiï u velykykh dozakh v grupi ULNA na ChA ES, iaki perenesly gostru promenevu khvorobu, a pry analogichnykh malykh dozakh u viddaleni roky proiav zmin bil' shyy̆ ta pryskorenyy̆ u chasi pry tryvaliy̆ diï IR, nizh pry vidnosno korotkochasniy̆. V ULNA na ChAES vyiavleno virogidne zrostannia slukhovykh porushen' za typom peredchasnogo vikovogo znyzhennia (rgesbyacuzis precox) u vidpovidnykh vikovykh kategoriiakh, iake ie odnym iz symptomiv peredchasnogo starinnia ïkhn'ogo organizmu.

  12. Multiple myeloma among Chornobyl accident clean-up workers - state and perspectives of analytical study.

    PubMed

    Bazyka, D A; Gudzenko, N A; Dyagil, I S; Babkina, N G; Chumak, V V; Bakhanova, E V; Paramonov, V V; Romanenko, A Y

    2013-01-01

    Meta: proanalizuvaty zahvorjuvanist' na mnozhynnu mijelomu (MM) sered uchasnykiv likvidacii' naslidkiv Chornobyl's'koi' katastrofy (ULNA) ta pidgotuvaty informacijnu osnovu dlja podal'shogo analitychnogo doslidzhennja dozozalezhnyh ryzykiv cijei' patologii', vrahovujuchy i'i' potencijnu radiacijnu zumovlenist'. Materialy i metody. Dlja identyfikacii' vypadkiv MM u doslidzhuvanij kogorti ULNA chysel'nistju 152 520 osib cholovichoi' stati buv provedenyj linkidzh bazy danyh kogorty z informacijnym masyvom Nacional'nogo kancerrejestru Ukrai'ny. Rezul'taty. Za doslidzhuvanyj period (1987–2012 rr.) bulo identyfikovano 64 vypadky, 58 z jakyh buly vkljucheni do poperedn'ogo analizu zahvorjuvanosti, vrahovujuchy 10-richnyj lag-period. Za rezul'tatamy poperedn'ogo analizu zahvorjuvanist' na MM u doslidzhuvanij kogorti ULNA ne perevyshhuvala harakternyj dlja zagal'nogo naselennja riven' protjagom pershyh 21 rokiv pislja avarii'. Vysnovok. Rozrahunok standartyzovanogo spivvidnoshennja zahvorjuvanosti (SIR) za period 2008–2012 rr., tobto cherez 22–26 rokiv pislja avarii', prodemonstruvav dostovirne perevyshhennja rivnja sered ULNA porivnjano zi spontannym populjacijnym rivnem dlja naselennja Ukrai'ny cholovichoi' stati (SIR 1.61, 95% CI 1.01;2.21). Pislja provedennja nezalezhnoi' diagnostychnoi' ekspertyzy vsih identyfikovanyh vypadkiv, rekonstrukcii' otrymanoi' dozy zovnishn'ogo oprominennja na chervonyj kistkovyj mozok za metodom RADRUE budut' proanalizovani dozozalezhni ryzyky vynyknennja MM z urahuvannjam mozhlyvogo modyfikujuchogo vplyvu inshyh faktoriv.

  13. Gas stream clean-up filter and method for forming same

    DOEpatents

    Mei, Joseph S.; DeVault, James; Halow, John S.

    1993-01-01

    A gas cleaning filter is formed in-situ within a vessel containing a fluidizable bed of granular material of a relatively large size fraction. A filter membrane provided by a porous metal or ceramic body or such a body supported a perforated screen on one side thereof is coated in-situ with a layer of the granular material from the fluidized bed by serially passing a bed-fluidizing gas stream through the bed of granular material and the membrane. The layer of granular material provides the filtering medium for the combined membrane-granular layer filter. The filter is not blinded by the granular material and provides for the removal of virtually all of the particulates from a process gas stream. The granular material can be at least partially provided by a material capable of chemically reacting with and removing sulfur compounds from the process gas stream. Low level radioactive waste containing organic material may be incinerated in a fluidized bed in communication with the described filter for removing particulates from the gaseous combustion products.

  14. Superfund Reauthorization 1994: DoD’s Opportunity to Clean Up Its Hazardous Waste Act

    DTIC Science & Technology

    1994-04-01

    AFB AR x Edwards AFB CA x Eielson AFB AK x Ellsworth AFB SD x Elmendorf AFB AK x England AFB LA x Fairchild AFB WA x F.E. Warren AFB WY x George AFB CA...amount of toxins produced, substances such as PCBs, dioxins , cyanides, heavy metals, pesticides, residues, alkalines, and acids have been emitted into...4 TX x *AFP 144 AZ x AFP PKUS CO x Andersen AFB GU x Bergstrom AFB TX x Carswell AFB TX x Castle AFB

  15. Angiogenesis after stroke is correlated with increased numbers of macrophages: the clean-up hypothesis.

    PubMed

    Manoonkitiwongsa, P S; Jackson-Friedman, C; McMillan, P J; Schultz, R L; Lyden, P D

    2001-10-01

    Brain cells manufacture and secrete angiogenic peptides after focal cerebral ischemia, but the purpose of this angiogenic response is unknown. Because the maximum possible regional cerebral blood flow is determined by the quantity of microvessels in each unit volume, it is possible that angiogenic peptides are secreted to generate new collateral channels; other possibilities include neuroprotection, recovery/regeneration, and removal of necrotic debris. If the brain attempts to create new collaterals, microvessel density should increase significantly after ischemia. Conversely, if angiogenic-signaling molecules serve some other purpose, microvessel densities may increase slightly or not at all. To clarify, the authors measured microvessel densities with quantitative morphometry. Left middle cerebral arteries of adult male Sprague-Dawley rats were occluded with intraluminal nylon suture for 4 hours followed by 7, 14, 19, or 30 days of reperfusion. Controls received no surgery or suture occlusion. Changes in microvessel density and macrophage numbers were measured by light microscopic morphometry using semiautomated stereologic methods. Microvessel density increased only in the ischemic margin adjacent to areas of pannecrosis and was always associated with increased numbers of macrophages. Ischemic brain areas without macrophages displayed no vascularity changes compared with normal animals. These data suggest that ischemia-induced microvessels are formed to facilitate macrophage infiltration and removal of necrotic brain.

  16. CLEANING UP WEST VIRGINIA: WHAT'S IT WORTH? ENVIRONMENTAL AND ECONOMIC PERSPECTIVES

    EPA Science Inventory

    In this presentation I discuss cleanup of AMD impaired waterways in the Cheat River Watershed of West Virginia from an economic standpoint. Appalachian states have an especially large number of contaminated streams and rivers, and the USGS places AMD as the primary source of wat...

  17. Sorption Mechanisms for Mercury Capture in Warm Post-Gasification Gas Clean-Up Systems

    SciTech Connect

    Jost Wendt; Sung Jun Lee; Paul Blowers

    2008-09-30

    The research was directed towards a sorbent injection/particle removal process where a sorbent may be injected upstream of the warm gas cleanup system to scavenge Hg and other trace metals, and removed (with the metals) within the warm gas cleanup process. The specific objectives of this project were to understand and quantify, through fundamentally based models, mechanisms of interaction between mercury vapor compounds and novel paper waste derived (kaolinite + calcium based) sorbents (currently marketed under the trade name MinPlus). The portion of the research described first is the experimental portion, in which sorbent effectiveness to scavenge metallic mercury (Hg{sup 0}) at high temperatures (>600 C) is determined as a function of temperature, sorbent loading, gas composition, and other important parameters. Levels of Hg{sup 0} investigated were in an industrially relevant range ({approx} 25 {micro}g/m{sup 3}) although contaminants were contained in synthetic gases and not in actual flue gases. A later section of this report contains the results of the complementary computational results.

  18. Clean Up Your Image: A Beginner's Guide to Scanning and Photoshop

    ERIC Educational Resources Information Center

    Stitzer, Michael S.

    2005-01-01

    In this article, the author addresses the key steps of scanning and illustrates the process with screen shots taken from a Macintosh G4 Powerbook computer running OSX and Adobe Photoshop 7.0. After reviewing scanning procedures, the author describes how to use Photoshop 7.0 to manipulate a scanned image. This activity gives students a good general…

  19. Clean up standards for decontamination and decommissioning of the West Valley Demonstration Project

    SciTech Connect

    Sullivan, D.; Szalinski, S.; Gramling, J.; Westcott, D.

    1995-12-31

    The purpose of this paper is to describe the process for developing decontamination and decommissioning (D and D) criteria for the West Valley Demonstration Project (WVDP). The WVDP is a project being conducted to demonstrate solidification techniques that can be used for preparing high-level radioactive waste (HLW) for disposal. The D and D criteria for the WVDP is being developed in a unique and evolving regulatory environment. The basis for the development of the D and D criteria for the WVDP is the assumption that NRC will execute its responsibilities for the WVDP in a manner consistent with its rules, regulations, and licensing processes, even though DOE is not subject to NRC licensing requirements. This is a reasonable assumption because upon completion of the WVDP, the DOE will turn over operational responsibility to New York State Energy Research and Development Authority (NYSERDA), the licensee. NYSERDA will then be subject to the NRC license requirements. Within the licensing context there are four options: (1) license termination and unrestricted release of the facility, (2) license conversions (3) amending the existing license, and (4) rulemaking. These options are evaluated to address a means for the DOE to satisfy its commitments in completing the WVDP and to then turn operational responsibility for the site back to NYSERDA.

  20. TECHNICAL APPROACHES TO CHARACTERIZING AND CLEANING UP IRON AND STEEL MILL SITES UNDER THE BROWNFIELDS INITIATIVE

    EPA Science Inventory

    This document provides brownfields planners with an overview of the technical methods that can be used to achieve successful site assessment and cleanup which are two key components of the brownfields redevelopment process. No two brownfields sites are identical and planners will...

  1. EPA Announces Availability of $26 Million to Clean Up Diesel Engines Nationwide

    EPA Pesticide Factsheets

    (Washington, D.C.) - The U.S. Environmental Protection Agency (EPA) today announced the availability of $26 million in grant funding to establish clean diesel projects aimed at reducing emissions from the nation's existing fleet of diesel engines. Di

  2. EPA Announces Availability of $26 Million to Clean Up Diesel Engines Nationwide

    EPA Pesticide Factsheets

    SAN FRANCISCO - The U.S. Environmental Protection Agency today announced the availability of $4.4 million in grant funding to establish clean diesel projects aimed at reducing emissions from the existing fleet of diesel engines in Arizona, California, Haw

  3. Effect of matrix clean-up for aflatoxin analysis in corn and dried distillers grains

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Aflatoxins are a group of highly carcinogenic mycotoxins that contaminate a wide variety of agricultural crops. These toxins have a detrimental economic impact on such industries as corn and ethanol production. They are highly regulated by the FDA and as such, a rapid, reliable method with low det...

  4. PHYTOREMEDIATION: USING PLANTS TO CLEAN UP CONTAMINATED SOIL, GROUNDWATER, AND WASTEWATER

    EPA Science Inventory

    Phytoremediation is an emerging cleanup technology for contaminated soils, groundwater, and wastewater that is both low-tech and low-cost. The cleanup technology is defined as the use of green plants to remove, contain, or render harmless such environmental contaminants as heavy ...

  5. PERFORMANCE OF MTBE CLEAN-UP TECHNOLOGIES IN NEW YORK STATE

    EPA Science Inventory

    The efficiency of cleanup technologies, based on MTBE concentration reduction, was evaluated for 1,012 UST sites from the State of New York. MTBE concentration reduction was calculated by dividing the maximum BTBE concentration by the current MTBE concentrations and the resul...

  6. SAMPLING SYSTEM

    DOEpatents

    Hannaford, B.A.; Rosenberg, R.; Segaser, C.L.; Terry, C.L.

    1961-01-17

    An apparatus is given for the batch sampling of radioactive liquids such as slurries from a system by remote control, while providing shielding for protection of operating personnel from the harmful effects of radiation.

  7. Polyimide processing additives

    NASA Technical Reports Server (NTRS)

    Fletcher, James C. (Inventor); Pratt, J. Richard (Inventor); St.clair, Terry L. (Inventor); Stoakley, Diane M. (Inventor); Burks, Harold D. (Inventor)

    1992-01-01

    A process for preparing polyimides having enhanced melt flow properties is described. The process consists of heating a mixture of a high molecular weight poly-(amic acid) or polyimide with a low molecular weight amic acid or imide additive in the range of 0.05 to 15 percent by weight of additive. The polyimide powders so obtained show improved processability, as evidenced by lower melt viscosity by capillary rheometry. Likewise, films prepared from mixtures of polymers with additives show improved processability with earlier onset of stretching by TMA.

  8. Polyimide processing additives

    NASA Technical Reports Server (NTRS)

    Pratt, J. Richard (Inventor); St.clair, Terry L. (Inventor); Stoakley, Diane M. (Inventor); Burks, Harold D. (Inventor)

    1993-01-01

    A process for preparing polyimides having enhanced melt flow properties is described. The process consists of heating a mixture of a high molecular weight poly-(amic acid) or polyimide with a low molecular weight amic acid or imide additive in the range of 0.05 to 15 percent by weight of the additive. The polyimide powders so obtained show improved processability, as evidenced by lower melt viscosity by capillary rheometry. Likewise, films prepared from mixtures of polymers with additives show improved processability with earlier onset of stretching by TMA.

  9. Large volume sample stacking in capillary zone electrophoresis for the monitoring of the degradation products of metribuzin in environmental samples.

    PubMed

    Quesada-Molina, Carolina; García-Campaña, Ana M; Del Olmo-Iruela, Laura; Del Olmo, Monsalud

    2007-09-14

    A capillary zone electrophoresis (CZE) method with UV-vis detection has been developed for the simultaneous monitoring of the major degradation products of metribuzin, i.e. deaminometribuzin (DA), deaminodiketometribuzin (DADK) and diketometribuzin (DK). The dissociation acid constants have also been estimated by CE and no significant differences have been observed with the values obtained by applying other techniques. Optimum separation has been achieved in less than 9 min in 40 mM sodium tetraborate buffer, pH 9.5 by applying a voltage of 15kV at 25 degrees C and using p-aminobenzoic acid as internal standard. In order to increase sensitivity, large volume sample stacking (LVSS) with polarity switching has been applied as on-line pre-concentration methodology. Detection limits of 10, 10 and 20 ng/mL for DA, DADK and DK, respectively were obtained. The method has been applied to soil samples, after pressurized liquid extraction (PLE). Samples were extracted at high temperature (103 degrees C and 1500 psi) using methanol as extraction solvent and sodium sulphate as drying agent. This PLE procedure was followed by an off-line pre-concentration and sample clean-up procedure by solid-phase extraction (SPE) using a LiChrolut EN sorbent column. These last two procedures were also suitable for the direct treatment of groundwater samples before CE analysis. The combination of both off-line and on-line pre-concentration procedures provided a significant improvement in sensitivity. LVSS provided pre-concentration factors of 4, 36 and 28 for DK, DA and DADK, respectively and with SPE a pre-concentration of 500-fold for the case of water samples and of 2.5-fold in the case of soil samples was obtained. The method is suitable for the monitoring of these residues in environmental samples with high sensitivity, precision and satisfactory recoveries.

  10. Food Additives and Hyperkinesis

    ERIC Educational Resources Information Center

    Wender, Ester H.

    1977-01-01

    The hypothesis that food additives are causally associated with hyperkinesis and learning disabilities in children is reviewed, and available data are summarized. Available from: American Medical Association 535 North Dearborn Street Chicago, Illinois 60610. (JG)

  11. Smog control fuel additives

    SciTech Connect

    Lundby, W.

    1993-06-29

    A method is described of controlling, reducing or eliminating, ozone and related smog resulting from photochemical reactions between ozone and automotive or industrial gases comprising the addition of iodine or compounds of iodine to hydrocarbon-base fuels prior to or during combustion in an amount of about 1 part iodine per 240 to 10,000,000 parts fuel, by weight, to be accomplished by: (a) the addition of these inhibitors during or after the refining or manufacturing process of liquid fuels; (b) the production of these inhibitors for addition into fuel tanks, such as automotive or industrial tanks; or (c) the addition of these inhibitors into combustion chambers of equipment utilizing solid fuels for the purpose of reducing ozone.

  12. Aptamer-based trapping of phytosphingosine in urine samples.

    PubMed

    Fischer, Christin; Klockmann, Sven; Wessels, Hauke; Hünniger, Tim; Schrader, Jil; Paschke-Kratzin, Angelika; Fischer, Markus

    2016-11-20

    Usually, small molecules like single metabolites used in clinical diagnostic can be quantified by instrumental approaches like LC-MS or bioanalytical techniques using antibodies or aptamers as selective receptors. The present work comprises the generation of aptamers with an affinity towards the medically relevant metabolite phytosphingosine via the previously reported just in time-Selection approach (Hünniger et al., 2014). The whole approach could be seen as a proof of concept to extend the existing just in time-Selection protocol for selection towards small molecules with dissociation constants in the low nanomolar range. Moreover it is conceivable that the shown methods could be quickly adapted to further scopes. Aptamers could be applied for clean-up or concentration processes prior to further analysis. As an example, we used the selected aptamers towards phytosphingosine bound to magnetic particles for affinity enrichment in both selection buffer and urine samples. As an outcome, enrichment factors of up to 9-fold (selection buffer)/4-fold (urine samples) were achieved by this approach.

  13. SAMPLING OSCILLOSCOPE

    DOEpatents

    Sugarman, R.M.

    1960-08-30

    An oscilloscope is designed for displaying transient signal waveforms having random time and amplitude distributions. The oscilloscopc is a sampling device that selects for display a portion of only those waveforms having a particular range of amplitudes. For this purpose a pulse-height analyzer is provided to screen the pulses. A variable voltage-level shifter and a time-scale rampvoltage generator take the pulse height relative to the start of the waveform. The variable voltage shifter produces a voltage level raised one step for each sequential signal waveform to be sampled and this results in an unsmeared record of input signal waveforms. Appropriate delay devices permit each sample waveform to pass its peak amplitude before the circuit selects it for display.

  14. Sampling apparatus

    DOEpatents

    Gordon, N.R.; King, L.L.; Jackson, P.O.; Zulich, A.W.

    1989-07-18

    A sampling apparatus is provided for sampling substances from solid surfaces. The apparatus includes first and second elongated tubular bodies which telescopically and sealingly join relative to one another. An absorbent pad is mounted to the end of a rod which is slidably received through a passageway in the end of one of the joined bodies. The rod is preferably slidably and rotatably received through the passageway, yet provides a selective fluid tight seal relative thereto. A recess is formed in the rod. When the recess and passageway are positioned to be coincident, fluid is permitted to flow through the passageway and around the rod. The pad is preferably laterally orientable relative to the rod and foldably retractable to within one of the bodies. A solvent is provided for wetting of the pad and solubilizing or suspending the material being sampled from a particular surface. 15 figs.

  15. Sampling apparatus

    DOEpatents

    Gordon, Norman R.; King, Lloyd L.; Jackson, Peter O.; Zulich, Alan W.

    1989-01-01

    A sampling apparatus is provided for sampling substances from solid surfaces. The apparatus includes first and second elongated tubular bodies which telescopically and sealingly join relative to one another. An absorbent pad is mounted to the end of a rod which is slidably received through a passageway in the end of one of the joined bodies. The rod is preferably slidably and rotatably received through the passageway, yet provides a selective fluid tight seal relative thereto. A recess is formed in the rod. When the recess and passageway are positioned to be coincident, fluid is permitted to flow through the passageway and around the rod. The pad is preferably laterally orientable relative to the rod and foldably retractable to within one of the bodies. A solvent is provided for wetting of the pad and solubilizing or suspending the material being sampled from a particular surface.

  16. Analysis of thyreostatic drugs in thyroid samples by liquid chromatography tandem mass spectrometry: comparison of two sample treatment strategies.

    PubMed

    Abuín, S; Companyó, R; Centrich, F; Rúbies, A; Prat, M D

    2008-10-17

    A method based on ultra-performance liquid chromatography-electrospray ionisation-tandem mass spectrometry (UPLC-MS/MS) for the determination of six thyreostatic drugs in thyroid tissue has been optimised and validated in accordance with Decision 2002/657/EC. Sample extraction was evaluated in methanol and in ethyl acetate, the latter which gave better results. Two clean-up strategies were compared: one based on silica cartridges (SPE), and the other, on gel permeation chromatography (GPC). Recoveries ranged from 40% to 79% for the SPE approach and from 80% to 109% for GPC. Quantification was performed with blank tissue samples spiked with the analytes in the range 50-500microgkg(-1). 5,6-Dimethyl-2-thiouracil and 2-mercaptobenzimidazole-d(4) were used as internal standards. Decision limit (CCalpha) and detection capability (CCbeta) ranged from 1 to 15microgkg(-1) and from 6 to 25microgkg(-1), respectively. The accuracy of the method was calculated as percent error, which was less than 10%. The relative standard deviation in reproducibility conditions ranged between 2% and 14%.

  17. Group Sparse Additive Models

    PubMed Central

    Yin, Junming; Chen, Xi; Xing, Eric P.

    2016-01-01

    We consider the problem of sparse variable selection in nonparametric additive models, with the prior knowledge of the structure among the covariates to encourage those variables within a group to be selected jointly. Previous works either study the group sparsity in the parametric setting (e.g., group lasso), or address the problem in the nonparametric setting without exploiting the structural information (e.g., sparse additive models). In this paper, we present a new method, called group sparse additive models (GroupSpAM), which can handle group sparsity in additive models. We generalize the ℓ1/ℓ2 norm to Hilbert spaces as the sparsity-inducing penalty in GroupSpAM. Moreover, we derive a novel thresholding condition for identifying the functional sparsity at the group level, and propose an efficient block coordinate descent algorithm for constructing the estimate. We demonstrate by simulation that GroupSpAM substantially outperforms the competing methods in terms of support recovery and prediction accuracy in additive models, and also conduct a comparative experiment on a real breast cancer dataset.

  18. Additive Manufacturing Infrared Inspection

    NASA Technical Reports Server (NTRS)

    Gaddy, Darrell

    2014-01-01

    Additive manufacturing is a rapid prototyping technology that allows parts to be built in a series of thin layers from plastic, ceramics, and metallics. Metallic additive manufacturing is an emerging form of rapid prototyping that allows complex structures to be built using various metallic powders. Significant time and cost savings have also been observed using the metallic additive manufacturing compared with traditional techniques. Development of the metallic additive manufacturing technology has advanced significantly over the last decade, although many of the techniques to inspect parts made from these processes have not advanced significantly or have limitations. Several external geometry inspection techniques exist such as Coordinate Measurement Machines (CMM), Laser Scanners, Structured Light Scanning Systems, or even traditional calipers and gages. All of the aforementioned techniques are limited to external geometry and contours or must use a contact probe to inspect limited internal dimensions. This presentation will document the development of a process for real-time dimensional inspection technique and digital quality record of the additive manufacturing process using Infrared camera imaging and processing techniques.

  19. On-line coupled extraction and separation using superheated water for the analysis of triazine herbicides in spiked compost samples.

    PubMed

    Tajuddin, Ruziyati; Smith, Roger M

    2005-08-19

    An on-line method, with a purely aqueous mobile phase, has employed linked superheated water extraction and superheated water separation for the analysis of triazine herbicides in spiked compost samples. After the superheated water extraction, a X-Terra solid-phase trap was used to collect and focus the extracted analytes. The trapped analytes were then released by thermal desorption and passed directly to a superheated water chromatographic separation using a PGC column. Two clean-up steps (prior to extraction and separation) were included to remove most of the interfering matrix components. The effects of the sample matrix and the extraction temperatures on the recovery of the triazines were investigated. Despite some thermal degradation of the chloro-triazines during the SWE, the on-line SWE-SWC method was sensitive and rapid. The coupled method could potentially reduce costs and labour and by using only water in every stage is compatible with the concepts of green chemistry.

  20. Optical waveguide lightmode spectroscopy technique-based immunosensor development for aflatoxin B1 determination in spice paprika samples.

    PubMed

    Majer-Baranyi, Krisztina; Zalán, Zsolt; Mörtl, Mária; Juracsek, Judit; Szendrő, István; Székács, András; Adányi, Nóra

    2016-11-15

    Optical waveguide lightmode spectroscopy (OWLS) technique has been applied to label-free detection of aflatoxin B1 in a competitive immunoassay format, with the aim to compare the analytical goodness of the developed OWLS immunosenor with HPLC and enzyme-linked immunosorbent assay (ELISA) methods for the detection of aflatoxin in spice paprika matrix. We have also assessed applicability of the QuEChERS method prior to ELISA measurements, and the results were compared to those obtained by traditional solvent extraction followed by immunoaffinity clean-up. The AFB1 content of sixty commercial spice paprika samples from different countries were measured with the developed and optimized OWLS immunosensor. Comparing the results from the indirect immunosensor to that obtained by HPLC or ELISA provided excellent correlation (with regression coefficients above 0.94) indicating that the competitive OWLS immunosensor has a potential for quick determination of aflatoxin B1 in paprika samples.

  1. Phenylethynyl Containing Reactive Additives

    NASA Technical Reports Server (NTRS)

    Connell, John W. (Inventor); Smith, Joseph G., Jr. (Inventor); Hergenrother, Paul M. (Inventor)

    2002-01-01

    Phenylethynyl containing reactive additives were prepared from aromatic diamine, containing phenylethvnvl groups and various ratios of phthalic anhydride and 4-phenylethynviphthalic anhydride in glacial acetic acid to form the imide in one step or in N-methyl-2-pvrrolidinone to form the amide acid intermediate. The reactive additives were mixed in various amounts (10% to 90%) with oligomers containing either terminal or pendent phenylethynyl groups (or both) to reduce the melt viscosity and thereby enhance processability. Upon thermal cure, the additives react and become chemically incorporated into the matrix and effect an increase in crosslink density relative to that of the host resin. This resultant increase in crosslink density has advantageous consequences on the cured resin properties such as higher glass transition temperature and higher modulus as compared to that of the host resin.

  2. Fused Lasso Additive Model

    PubMed Central

    Petersen, Ashley; Witten, Daniela; Simon, Noah

    2016-01-01

    We consider the problem of predicting an outcome variable using p covariates that are measured on n independent observations, in a setting in which additive, flexible, and interpretable fits are desired. We propose the fused lasso additive model (FLAM), in which each additive function is estimated to be piecewise constant with a small number of adaptively-chosen knots. FLAM is the solution to a convex optimization problem, for which a simple algorithm with guaranteed convergence to a global optimum is provided. FLAM is shown to be consistent in high dimensions, and an unbiased estimator of its degrees of freedom is proposed. We evaluate the performance of FLAM in a simulation study and on two data sets. Supplemental materials are available online, and the R package flam is available on CRAN. PMID:28239246

  3. Phenylethynyl Containing Reactive Additives

    NASA Technical Reports Server (NTRS)

    Connell, John W. (Inventor); Smith, Joseph G., Jr. (Inventor); Hergenrother, Paul M. (Inventor)

    2002-01-01

    Phenylethynyl containing reactive additives were prepared from aromatic diamines containing phenylethynyl groups and various ratios of phthalic anhydride and 4-phenylethynylphthalic anhydride in glacial acetic acid to form the imide in one step or in N-methyl-2-pyrrolidi none to form the amide acid intermediate. The reactive additives were mixed in various amounts (10% to 90%) with oligomers containing either terminal or pendent phenylethynyl groups (or both) to reduce the melt viscosity and thereby enhance processability. Upon thermal cure, the additives react and become chemically incorporated into the matrix and effect an increase in crosslink density relative to that of the host resin. This resultant increase in crosslink density has advantageous consequences on the cured resin properties such as higher glass transition temperature and higher modulus as compared to that of the host resin.

  4. Additives in plastics.

    PubMed Central

    Deanin, R D

    1975-01-01

    The polymers used in plastics are generally harmless. However, they are rarely used in pure form. In almost all commercial plastics, they are "compounded" with monomeric ingredients to improve their processing and end-use performance. In order of total volume used, these monomeric additives may be classified as follows: reinforcing fibers, fillers, and coupling agents; plasticizers; colorants; stabilizers (halogen stabilizers, antioxidants, ultraviolet absorbers, and biological preservatives); processing aids (lubricants, others, and flow controls); flame retardants, peroxides; and antistats. Some information is already available, and much more is needed, on potential toxicity and safe handling of these additives during processing and manufacture of plastics products. PMID:1175566

  5. Additives in plastics.

    PubMed

    Deanin, R D

    1975-06-01

    The polymers used in plastics are generally harmless. However, they are rarely used in pure form. In almost all commercial plastics, they are "compounded" with monomeric ingredients to improve their processing and end-use performance. In order of total volume used, these monomeric additives may be classified as follows: reinforcing fibers, fillers, and coupling agents; plasticizers; colorants; stabilizers (halogen stabilizers, antioxidants, ultraviolet absorbers, and biological preservatives); processing aids (lubricants, others, and flow controls); flame retardants, peroxides; and antistats. Some information is already available, and much more is needed, on potential toxicity and safe handling of these additives during processing and manufacture of plastics products.

  6. Chain Sampling

    DTIC Science & Technology

    1972-08-01

    35609 Advanced Techniques Branch Plans and Programs Analysis Division Directorate for Product Assurance U. S. Army Missile Command Redstone Arsenal...Ray Heathcock Advanced Techniques Branch Plans and Programs Analysis Division Directorate for Product Assurance U. S. Army Missile Command...for Product Assurance has established a rather unique computer program for handling a variety of chain sampling schemes and is available for

  7. A quadruplex real-time qPCR assay for the simultaneous assessment of total human DNA, human male DNA, DNA degradation and the presence of PCR inhibitors in forensic samples: a diagnostic tool for STR typing.

    PubMed

    Hudlow, William R; Chong, Mavis Date; Swango, Katie L; Timken, Mark D; Buoncristiani, Martin R

    2008-03-01

    A quadruplex real-time qPCR assay was developed to simultaneously assess total human DNA, human male DNA, DNA degradation and PCR inhibitors in forensic samples. Specifically, the assay utilizes a approximately 170-190bp target sequence that spans the TH01 STR locus to quantify total human DNA (nuTH01), a 137 bp target sequence directly adjacent to the SRY gene to quantify human male DNA (nuSRY), a 67 bp target sequence flanking the CSF1PO STR locus (nuCSF) to assess degradation (nuCSF:nuTH01 ratio) and a 77 bp synthetic DNA template used as an internal PCR control target sequence (IPC) for the assessment of PCR inhibition. Validation studies, performed on an ABI 7500 SDS instrument using TaqMan and TaqManMGB detection, indicate each of the targets in the quadruplex assay performs effectively and is informative even when challenged with DNase-degraded and hematin-inhibited samples. The nuTH01-nuSRY-nuCSF-IPC quadruplex qPCR assay is envisioned to assist in the choice of the most informative DNA typing system available, which may include standard autosomal STR typing when the results indicate the presence of non-degraded, single gender DNA or non-degraded, male:female mixtures at ratios expected to yield probative alleles; Y STR typing in samples containing a male component that is overwhelmed by the presence of an excess of female DNA; reduced amplicon size STR typing ("MiniSTRs") where the nuCSF:nuTH01 ratio indicates the sample is highly degraded; enhanced STR amplification with additional AmpliTaq Gold/BSA and/or sample clean-up when the presence of PCR inhibitors is suggested by a delayed IPC C(T) value or mitochondrial DNA typing in samples where little to no nuclear DNA is detected. The present study includes evaluations of species specificity, sensitivity, precision, reproducibility, male-female mixtures, population samples and applications to various casework-type samples as indicated by the Scientific Working Group on DNA Analysis Methods (SWGDAM

  8. Biobased lubricant additives

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Fully biobased lubricants are those formulated using all biobased ingredients, i.e. biobased base oils and biobased additives. Such formulations provide the maximum environmental, safety, and economic benefits expected from a biobased product. Currently, there are a number of biobased base oils that...

  9. More Than Additional Space...

    ERIC Educational Resources Information Center

    CEFP Journal, 1973

    1973-01-01

    A much needed addition to the Jamestown Elementary School turned out to be more than an expansion of walls for more space. A new educational program, a limited budget, and a short time line were tackled on a team approach basis and were successfully resolved. (Author)

  10. Sampling Strategy

    NASA Technical Reports Server (NTRS)

    2008-01-01

    Three locations to the right of the test dig area are identified for the first samples to be delivered to the Thermal and Evolved Gas Analyzer (TEGA), the Wet Chemistry Lab (WCL), and the Optical Microscope (OM) on NASA's Phoenix Mars Lander. These sampling areas are informally labeled 'Baby Bear', 'Mama Bear', and 'Papa Bear' respectively. This image was taken on the seventh day of the Mars mission, or Sol 7 (June 1, 2008) by the Surface Stereo Imager aboard NASA's Phoenix Mars Lander.

    The Phoenix Mission is led by the University of Arizona, Tucson, on behalf of NASA. Project management of the mission is by NASA's Jet Propulsion Laboratory, Pasadena, Calif. Spacecraft development is by Lockheed Martin Space Systems, Denver.

  11. Vinyl capped addition polyimides

    NASA Technical Reports Server (NTRS)

    Vannucci, Raymond D. (Inventor); Malarik, Diane C. (Inventor); Delvigs, Peter (Inventor)

    1991-01-01

    Polyimide resins (PMR) are generally useful where high strength and temperature capabilities are required (at temperatures up to about 700 F). Polyimide resins are particularly useful in applications such as jet engine compressor components, for example, blades, vanes, air seals, air splitters, and engine casing parts. Aromatic vinyl capped addition polyimides are obtained by reacting a diamine, an ester of tetracarboxylic acid, and an aromatic vinyl compound. Low void materials with improved oxidative stability when exposed to 700 F air may be fabricated as fiber reinforced high molecular weight capped polyimide composites. The aromatic vinyl capped polyimides are provided with a more aromatic nature and are more thermally stable than highly aliphatic, norbornenyl-type end-capped polyimides employed in PMR resins. The substitution of aromatic vinyl end-caps for norbornenyl end-caps in addition polyimides results in polymers with improved oxidative stability.

  12. Electrophilic addition of astatine

    SciTech Connect

    Norseev, Yu.V.; Vasaros, L.; Nhan, D.D.; Huan, N.K.

    1988-03-01

    It has been shown for the first time that astatine is capable of undergoing addition reactions to unsaturated hydrocarbons. A new compound of astatine, viz., ethylene astatohydrin, has been obtained, and its retention numbers of squalane, Apiezon, and tricresyl phosphate have been found. The influence of various factors on the formation of ethylene astatohydrin has been studied. It has been concluded on the basis of the results obtained that the univalent cations of astatine in an acidic medium is protonated hypoastatous acid.

  13. Functional Generalized Additive Models.

    PubMed

    McLean, Mathew W; Hooker, Giles; Staicu, Ana-Maria; Scheipl, Fabian; Ruppert, David

    2014-01-01

    We introduce the functional generalized additive model (FGAM), a novel regression model for association studies between a scalar response and a functional predictor. We model the link-transformed mean response as the integral with respect to t of F{X(t), t} where F(·,·) is an unknown regression function and X(t) is a functional covariate. Rather than having an additive model in a finite number of principal components as in Müller and Yao (2008), our model incorporates the functional predictor directly and thus our model can be viewed as the natural functional extension of generalized additive models. We estimate F(·,·) using tensor-product B-splines with roughness penalties. A pointwise quantile transformation of the functional predictor is also considered to ensure each tensor-product B-spline has observed data on its support. The methods are evaluated using simulated data and their predictive performance is compared with other competing scalar-on-function regression alternatives. We illustrate the usefulness of our approach through an application to brain tractography, where X(t) is a signal from diffusion tensor imaging at position, t, along a tract in the brain. In one example, the response is disease-status (case or control) and in a second example, it is the score on a cognitive test. R code for performing the simulations and fitting the FGAM can be found in supplemental materials available online.

  14. Siloxane containing addition polyimides

    NASA Technical Reports Server (NTRS)

    Maudgal, S.; St. Clair, T. L.

    1984-01-01

    Addition polyimide oligomers have been synthesized from bis(gamma-aminopropyl) tetramethyldisiloxane and 3, 3', 4, 4'-benzophenonetetracarboxylic dianhydride using a variety of latent crosslinking groups as endcappers. The prepolymers were isolated and characterized for solubility (in amide, chlorinated and ether solvents), melt flow and cure properties. The most promising systems, maleimide and acetylene terminated prepolymers, were selected for detailed study. Graphite cloth reinforced composites were prepared and properties compared with those of graphite/Kerimid 601, a commercially available bismaleimide. Mixtures of the maleimide terminated system with Kerimid 601, in varying proportions, were also studied.

  15. Platelet additive solution - electrolytes.

    PubMed

    Azuma, Hiroshi; Hirayama, Junichi; Akino, Mitsuaki; Ikeda, Hisami

    2011-06-01

    Recent attention to solutions that replace most or all plasma in platelet concentrates, while maintaining satisfactory platelet function, is motivated by the potential of plasma reduction or depletion to mitigate various transfusion-related adverse events. This report considers the electrolytic composition of previously described platelet additive solutions, in order to draw general conclusions about what is required for platelet function and longevity. The optimal concentrations of Na(+) and Cl(-) are 69-115 mM. The presence of both K(+) and Mg(2+) in platelet suspension at nearly physiological concentrations (3-5mM and 1.5-3mM, respectively) is indispensable for good preservation capacity because both electrolytes are required to prevent platelet activation. In contrast to K(+) and Mg(2+), Ca(2+) may not be important because no free Ca(2+) is available in M-sol, which showed excellent platelet preservation capacity at less than 5% plasma concentration. The importance of bicarbonate (approximately 40 mM) can be recognized when the platelets are suspended in additive solution under less than 5% residual plasma concentration.

  16. Comparison of different modifications on QuEChERS sample preparation method for PAHs determination in black, green, red and white tea.

    PubMed

    Sadowska-Rociek, Anna; Surma, Magdalena; Cieślik, Ewa

    2014-01-01

    The aim of this work was the evaluation of QuEChERS extraction method for polycyclic aromatic hydrocarbon (PAH) determination in various types of tea. In the experiment, different kinds of extraction solvents, sorbents and a final method of sample preparation were compared. The final extracts were analysed by gas chromatography-selected ion monitoring-mass spectrometry. The results suggest that acetonitrile extraction, clean up with SAX and final liquid-liquid extraction was the best combination giving the most purified extracts and acceptable compound recoveries for different types of teas. In the study of real samples, compounds belonging to light PAHs were mostly detected, and heavy polycyclic aromatic hydrocarbons, including benzo[a]pyrene, were not identified in any of samples.

  17. High-throughput automated microfluidic sample preparation for accurate microbial genomics

    PubMed Central

    Kim, Soohong; De Jonghe, Joachim; Kulesa, Anthony B.; Feldman, David; Vatanen, Tommi; Bhattacharyya, Roby P.; Berdy, Brittany; Gomez, James; Nolan, Jill; Epstein, Slava; Blainey, Paul C.

    2017-01-01

    Low-cost shotgun DNA sequencing is transforming the microbial sciences. Sequencing instruments are so effective that sample preparation is now the key limiting factor. Here, we introduce a microfluidic sample preparation platform that integrates the key steps in cells to sequence library sample preparation for up to 96 samples and reduces DNA input requirements 100-fold while maintaining or improving data quality. The general-purpose microarchitecture we demonstrate supports workflows with arbitrary numbers of reaction and clean-up or capture steps. By reducing the sample quantity requirements, we enabled low-input (∼10,000 cells) whole-genome shotgun (WGS) sequencing of Mycobacterium tuberculosis and soil micro-colonies with superior results. We also leveraged the enhanced throughput to sequence ∼400 clinical Pseudomonas aeruginosa libraries and demonstrate excellent single-nucleotide polymorphism detection performance that explained phenotypically observed antibiotic resistance. Fully-integrated lab-on-chip sample preparation overcomes technical barriers to enable broader deployment of genomics across many basic research and translational applications. PMID:28128213

  18. Additive composition, for gasoline

    SciTech Connect

    Vataru, M.

    1989-01-10

    An admixture is described that comprises Diesel fuel and an additive composition added thereto which is between about 0.05 to about 2.0 percent by weight of the fuel, the composition comprising: (a) between about 0.05 and 25% relative weight parts of an organic peroxide, and (b) between about 0.1 and 25% relative weight parts of detergent selected from the component group that consists of: (i) fatty amines; (ii) ethoxylated and propoxylated derivatives of fatty amines; (iii) fatty diamines; (iv) fatty imidazlines; (v) polymeric amines and derivatives thereof; (vi) combination of one or more of the (i) through (v) components with carboxylic acid or acids having from three to forth carbon atoms, (c) from about 99.0 to about 50% by weight of a hydrocarbon solvent.

  19. Teardrop bladder: additional considerations

    SciTech Connect

    Wechsler, R.J.; Brennan, R.E.

    1982-07-01

    Nine cases of teardrop bladder (TDB) seen at excretory urography are presented. In some of these patients, the iliopsoas muscles were at the upper limit of normal in size, and additional evaluation of the perivesical structures with computed tomography (CT) was necessary. CT demonstrated only hypertrophied muscles with or without perivesical fat. The psoas muscles and pelvic width were measured in 8 patients and compared with the measurements of a control group of males without TDB. Patients with TDB had large iliopsoas muscles and narrow pelves compared with the control group. The psoas muscle width/pelvic width ratio was significantly greater (p < 0.0005) in patients with TDB than in the control group, with values of 1.04 + 0.05 and 0.82 + 0.09, respectively. It is concluded that TDB is not an uncommon normal variant in black males. Both iliopsoas muscle hypertrophy and a narrow pelvis are factors that predispose a patient to TDB.

  20. Perspectives on Additive Manufacturing

    NASA Astrophysics Data System (ADS)

    Bourell, David L.

    2016-07-01

    Additive manufacturing (AM) has skyrocketed in visibility commercially and in the public sector. This article describes the development of this field from early layered manufacturing approaches of photosculpture, topography, and material deposition. Certain precursors to modern AM processes are also briefly described. The growth of the field over the last 30 years is presented. Included is the standard delineation of AM technologies into seven broad categories. The economics of AM part generation is considered, and the impacts of the economics on application sectors are described. On the basis of current trends, the future outlook will include a convergence of AM fabricators, mass-produced AM fabricators, enabling of topology optimization designs, and specialization in the AM legal arena. Long-term developments with huge impact are organ printing and volume-based printing.