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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. Immuno-ultrafiltration as a new strategy in sample clean-up of aflatoxins.

    PubMed

    Reiter, Elisabeth Viktoria; Cichna-Markl, Margit; Chung, Duck-Hwa; Zentek, Jürgen; Razzazi-Fazeli, Ebrahim

    2009-05-01

    The present paper describes the development of a new clean-up strategy for the analysis of aflatoxins (AFs) in food. The sample preparation method is based on immuno-ultrafiltration (IUF) which, in contrast to immunoaffinity chromatography, makes use of antibodies in free form. After selecting an appropriate ultrafiltration (UF) device and optimizing different operation conditions the IUF method was applied to the clean-up of maize and rice. Quantification of AFs was carried out by HPLC and fluorescence detection, after postcolumn derivatization in a Kobracell. The IUF method was shown to be as selective as sample clean-up using commercial immunoaffinity columns. Recovery rates and RSD for the AFs G(2), G(1), B(2) and B(1) in spiked rice were found to be 76 +/- 3, 76 +/- 2, 83 +/- 5 and 99 +/- 14%, respectively. The analysis of a FAPAS (food analysis performance assessment scheme) maize material resulted in AFs concentrations which were in the range assigned by the producer of the reference material. PMID:19472274

  3. 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). PMID:27108048

  4. Photochemical sample treatment for extracts clean up in PCB analysis from sediments.

    PubMed

    Barreca, Salvatore; Orecchio, Santino; Pace, Andrea

    2013-01-15

    Sample purification can be considered the most polluting step of the whole analytical process for PCBs determination in sediment samples. The use of photochemical sample treatment represents an alternative methodology for extracts clean up allowing for a reduction of the used amount of organic solvents. The first application of a photochemical sample treatment for the selective removal or reduction of organic substances interfering with PCBs analyses in sediments is reported. The method's efficiency and robustness were compared with currently used chromatographic purification. Quality parameters such as recovery, linearity and reproducibility were studied. The entire procedure was validated by four replicate analysis of certified reference sediment. The quantification limits (LOQ) obtained by us ranged from 1 to 3.1 ng g(-1). The RSD for each congener was below 15% and recoveries were in the range 40-130%. Results based on the analysis of real and certified samples showed similar or improved detection thresholds and pointed out the advantages of the photochemical methodology in terms of costs and environmental friendly conditions. PMID:23200398

  5. 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

  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. PMID:27207580

  7. Molecularly imprinted polymers for the clean-up of a basic drug from environmental and biological samples.

    PubMed

    Chapuis, Florence; Mullot, Jean-Ulrich; Pichon, Valérie; Tuffal, Gilles; Hennion, Marie-Claire

    2006-12-01

    A molecularly imprinted polymer (MIP) was synthesized and evaluated to selectively extract an alpha-blocker, i.e. alfuzosin, from human plasma. The synthesis of the MIP was performed in dichloromethane with methacrylic acid as monomer and the target drug as template. A first series of experiments was carried out in dichloromethane to estimate the potential of the MIP in its specific recognition medium, i.e. dichloromethane, by developing a selective procedure and by measuring the capacity of the sorbent. An optimized procedure was developed for the selective extraction of alfuzosin with a recovery close to 100% in this medium and a specific capacity of 1.3 micromol g(-1) of MIP was measured. A study in aqueous media was also carried out by a comprehensive approach of the retention mechanism in order to build a selective procedure of extraction. The effects of the amount and of the charge of cations were studied and an optimal pH value was defined to limit matrix effects. Then, the alfuzosin MIP was then directly used to selectively extract the target drug from human plasma with an extraction recovery of 60%. Lastly, a soil was extracted by a pressurized solvent and the resulting extract was cleaned up on the MIP, showing the possibility to use this selective sorbent for the sample treatment of various complex matrices. PMID:17055520

  8. Dispersive solid-phase extraction as a simplified clean-up technique for biological sample extracts. Determination of polybrominated diphenyl ethers by gas chromatography-tandem mass spectrometry.

    PubMed

    Fontana, Ariel R; Camargo, Alejandra; Martinez, Luis D; Altamirano, Jorgelina C

    2011-05-01

    Dispersive solid-phase extraction (DSPE) is proposed for the first time as a simplified, fast and low cost clean-up technique of biological sample extracts for polybrominated diphenyl ethers (PBDEs) determination. The combination of a traditional extraction technique, such as ultrasound-assisted leaching (USAL) with DSPE was successfully applied for sample preparation prior to gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis. The analytes were first extracted from 1g homogenized sample in n-hexane:dichloromethane (8:2) by applying USAL technique and further cleaned-up using DSPE with 0.20 g C(18)-silica as sorbent material. Different solvent mixtures, sorbent type and amount, and lipid digestion procedures were evaluated in terms of clean-up and extraction efficiency. Under optimum conditions, the method detection limits (MDLs) for PBDEs, calculated as three times the signal-to-noise ratio (S/N) were within the range 9-44 pg g(-1) wet weight. The calibration graphs were linear within the concentration range of 53-500,000 pg g(-1), 66-500,000 pg g(-1), 89-500,000 pg g(-1) and 151-500,000 pg g(-1) for BDE-47, BDE-100, BDE-99 and BDE-153, respectively; and the coefficient of determination (r(2)) exceeded 0.9992 for all analytes. The proposed methodology was compared with a reference solid-phase extraction technique. The applicability of the methodology for the screening of PBDEs has been demonstrated by analyzing spiked and real samples of biological nature (fish, egg and chicken) with different lipid content as well as reference material (WELL-WMF-01). Recovery values ranged between 75% and 114% and the measured concentrations in certified material showed a reasonable agreement with the certified ones. BDE-47, BDE-100 and BDE-99 were quantified in three of the seven analyzed samples and the concentrations ranged between 91 and 140 pg g(-1). In addition, this work is the first description of PBDEs detected in fish of Argentinean environment. PMID

  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. PMID:25082754

  10. EVALUATION OF GEL PERMEATION CHROMATOGRAPHY FOR CLEAN UP OF HUMAN ADIPOSE TISSUE SAMPLES FOR GC/MS ANALYSIS OF PESTICIDES AND OTHER CHEMICALS

    EPA Science Inventory

    Gel permeation chromatography (GPC) has been evaluated for clean up of human adipose tissue sample extracts in preparation for confirmatory analysis by gas chromatography-mass spectrometry (GC/MS). Studies were conducted with standard solutions, fortified chicken fat, and actual ...

  11. 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...

  12. Development of sample clean up methods for the analysis of Mycobacterium tuberculosis methyl mycocerosate biomarkers in sputum extracts by gas chromatography–mass spectrometry

    PubMed Central

    Nicoara, Simona C.; Turner, Nicholas W.; Minnikin, David E.; Lee, Oona Y.-C.; O'Sullivan, Denise M.; McNerney, Ruth; Mutetwa, Reggie; Corbett, Liz E.; Morgan, Geraint H.

    2015-01-01

    A proof of principle gas chromatography–mass spectrometry method is presented, in combination with clean up assays, aiming to improve the analysis of methyl mycocerosate tuberculosis biomarkers from sputum. Methyl mycocerosates are generated from the transesterification of phthiocerol dimycocerosates (PDIMs), extracted in petroleum ether from sputum of tuberculosis suspect patients. When a high matrix background is present in the sputum extracts, the identification of the chromatographic peaks corresponding to the methyl derivatives of PDIMs analytes may be hindered by the closely eluting methyl ether of cholesterol, usually an abundant matrix constituent frequently present in sputum samples. The purification procedures involving solid phase extraction (SPE) based methods with both commercial Isolute-Florisil cartridges, and purpose designed molecularly imprinted polymeric materials (MIPs), resulted in cleaner chromatograms, while the mycocerosates are still present. The clean-up performed on solutions of PDIMs and cholesterol standards in petroleum ether show that, depending on the solvent mix and on the type of SPE used, the recovery of PDIMs is between 64 and 70%, whilst most of the cholesterol is removed from the system. When applied to petroleum ether extracts from representative sputum samples, the clean-up procedures resulted in recoveries of 36–68% for PDIMs, allowing some superior detection of the target analytes. PMID:25728371

  13. Passive extraction and clean-up of phenoxy acid herbicides in samples from a groundwater plume using hollow fiber supported liquid membranes.

    PubMed

    Liu, Jing-Fu; Toräng, Lars; Mayer, Philipp; Jönsson, Jan Ake

    2007-08-10

    Hollow fiber supported liquid membranes were applied for the passive extraction of phenoxy acid herbicides from water samples. Polypropylene hollow fiber membranes (240 microm i.d., 30 microm wall thickness, 0.05 microm pore size, 30 cm length) were impregnated with 2.0% tri-n-octylphosphine oxide (TOPO) in di-n-hexyl ether in the pores of the fiber wall to form a liquid membrane. They were then filled with basic solution in the lumen as acceptor and finally placed into the sample (donor). Complete extraction of phenoxy acid herbicides including 2,4-D, MCPA, dichlorprop, and mecoprop from an acidified sample (4 mL, adjusted to pH 1.5 with HCl) into basic acceptor (10 microL of 0.2M NaOH) was achieved after 4 h of shaking (100 rpm) resulting in an enrichment factor of 400 times. The acceptor was then neutralized by addition of HCl and injected into a HPLC system for the determination of the phenoxy acid herbicides. Environmentally relevant salinity (0-3.5% NaCl) and dissolved organic matter (0-25 mg/L of dissolved organic carbon) had no significant effect on the extraction. The method provided extraction efficiencies of more than 91%, detection limits of 0.3-0.6 microg/L, and combined extraction and clean up in one single step. This procedure was applied to determine aqueous concentrations of phenoxy acid herbicides in groundwater samples collected from an old dumping site (Cheminova, Denmark) with detected concentrations up to 5800 microg/L. Although the samples were very dirty with large amounts of suspended particles, non-aqueous phase liquids (NAPLs) and dissolved organic matters, good spike recoveries (80-126%) were obtained for 10 of the 11 samples. PMID:17449052

  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. Development of sample extraction and clean-up strategies for target and non-target analysis of environmental contaminants in biological matrices.

    PubMed

    Baduel, Christine; Mueller, Jochen F; Tsai, Henghang; Gomez Ramos, Maria Jose

    2015-12-24

    Recently, there has been an increasing trend towards multi-targeted analysis and non-target screening methods as a means to increase the number of monitored analytes. Previous studies have developed biomonitoring methods which specifically focus on only a small number of analytes with similar physico-chemical properties. In this paper, we present a simple and rapid multi-residue method for simultaneous extraction of polar and non-polar organic chemicals from biological matrices, containing up to 5% lipid content. Our method combines targeted multi-residue analysis using gas chromatography triple quadrupole mass spectrometry (GC-QqQ-MS/MS) and a multi-targeted analysis complemented with non-target screening using liquid chromatography coupled to a quadrupole time of flight mass spectrometry (LC-QTOF-MS/MS). The optimization of the chemical extraction procedure and the effectiveness of different clean-up methods were evaluated for two biological matrices: fish muscle (lipid content ∼2%) and breast milk (∼4%). To extract a wide range of chemicals, the partition/extraction procedure used for the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach was tested as the initial step for the extraction of 77 target compounds covering a broad compound domain. All the target analytes have different physico-chemical properties (log Kow ranges from -0.3 to 10) and cover a broad activity spectrum; from polar pesticides, pharmaceuticals, personal care products (PPCPs) to highly lipophilic chemicals such as polybrominated diphenyl ethers (PBDEs), polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs) and organochloride pesticides (OCPs). A number of options were explored for the clean-up of lipids, proteins and other impurities present in the matrix. Zirconium dioxide-based sorbents as dispersive solid-phase extraction (d-SPE) and protein-lipid removal filter cartridges (Captiva ND Lipids) provided the best results for GC-MS and LC-MS analysis

  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. PMID:20953778

  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. PMID:24607126

  18. Determination of eight sulfonamides in bovine kidney by liquid chromatography/tandem mass spectrometry with on-line extraction and sample clean-up.

    PubMed

    Van Eeckhout, N; Perez, J C; Van Peteghem, C

    2000-01-01

    A sensitive, high performance liquid chromatography/tandem mass spectrometric (i.e. mass spectrometry/mass spectrometry; LC/MS/MS) method with on-line extraction and sample clean-up for the screening and confirmation of residues of sulfonamides in kidney is described. The sulfonamides are extracted from homogenized kidney with methanol. After centrifugation of the extract, an aliquot of the extract is directly injected on the LC/MS/MS system with further extraction and clean-up of the sample on-line. Detection of the analytes was achieved by positive electrospray ionization (ESI) followed by multiple reaction monitoring. For each sulfonamide the collisional decomposition of the protonated molecule to a common, abundant fragment ion was monitored. The method has been validated for sulfadimethoxine, sulfaquinoxaline, sulfamethazine, sulfamerazine, sulfathiazole, sulfamethoxazole, sulfadiazine and sulfapyridine. Calibration curves resulting from spiked blank kidney samples at the 10-200 microg/kg level showed good linear correlation. At the level of 50, 100 and 200 microg/kg both within- and between-day precision, as measured by relative standard deviation (RSD), were less than 16%. The limits of detection (LODs) ranged from 5 to 13.5 microg/kg. The recoveries ranged from 78 to 82%. The procedure provides a rapid, reliable and sensitive method for the determination of residues of sulfonamides in bovine kidney. The advantage of this method over existing methods is its decreased sample preparation and analysis time, which makes the method more suitable for routine analysis. PMID:11114046

  19. 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. PMID:21871961

  20. High-performance liquid chromatographic determination of ochratoxin A in artificially contaminated cocoa beans using automated sample clean-up.

    PubMed

    Hurst, W J; Martin, R A

    1998-06-12

    A HPLC method is described for the analysis of ochratoxin A at low-ppb levels in samples of artificially contaminated cocoa beans. The samples are extracted in a mixture of methanol-water containing ascorbic acid, adjusted to pH and evaporated to dryness. Samples in this state are then placed onto a Benchmate sample preparation workstation where C18 solid-phase extraction operations are performed. The resulting materials are evaporated to dryness and analyzed by reversed-phase HPLC with fluorescence detection. The method was evaluated for accuracy and precision with R.S.D.s for multiple injections of sample and standard calculated to 1.1% and 2.5% for sample and standard, respectively. Recoveries of ochratoxin A added to cocoa beans ranged from 87-106% over the range of the assay. PMID:9691293

  1. Molecularly imprinted polymers applied to the clean-up of zearalenone and alpha-zearalenol from cereal and swine feed sample extracts.

    PubMed

    Urraca, Javier L; Marazuela, María Dolores; Moreno-Bondi, María C

    2006-08-01

    A molecularly imprinted polymer prepared using 1-allylpiperazine (1-ALPP) as the functional monomer, trimethyltrimethacrylate (TRIM) as the crosslinker and the zearalenone (ZON)-mimicking template cyclododecanyl-2,4-dihydroxybenzoate (CDHB) has been applied to the clean-up and preconcentration of this mycotoxin (zearalenone) and a related metabolite, alpha-zearalenol (alpha-ZOL), from cereal and swine feed sample extracts. The extraction of ZON and alpha-ZOL from the food samples was accomplished using pressurized liquid extraction (PLE) with MeOH/ACN (50:50, v/v) as the extraction solvent, at 50 degrees C and 1500 psi. The extracted samples were cleaned up and preconcentrated through the MIP cartridge and analyzed using HPLC with fluorescence detection (lambda (exc)=271/ lambda (em)=452 nm). The stationary phase was a polar endcapped C18 column, and ACN/MeOH/water 10/55/35 (v/v/v, 15 mM ammonium acetate) at a flow rate of 1.0 mL min(-1) was used as the mobile phase. The method was applied to the analysis of ZON and alpha-ZOL in wheat, corn, barley, rye, rice and swine feed samples fortified with 50, 100 and 400 ng g(-1) of both mycotoxins, and it gave recoveries of between 85 and 97% (RSD 2.1-6.7%, n=3) and 87-97% (RSD 2.3-5.6%, n=3) for alpha-ZOL and ZON, respectively. The method was validated using a corn reference material for ZON. PMID:16628404

  2. 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. PMID:22608412

  3. Determination of chemotherapeutic drugs in human urine by capillary electrophoresis with UV and fluorimetric detection using solid-supported liquid-liquid extraction for sample clean-up.

    PubMed

    Hurtado-Sánchez, María del Carmen; Acedo-Valenzuela, María Isabel; Durán-Merás, Isabel; Rodríguez-Cáceres, María Isabel

    2015-06-01

    Capillary electrophoresis was used for the rapid determination of three chemotherapeutic drugs employed to treat colorectal cancer: irinotecan, tegafur, and leucovorin, and their main metabolites (7-ethyl-10-hydroxycamptothecin and 5-fluorouracil), in human urine samples. A phosphate buffer (pH 11.34; 20 mM) was selected as the background electrolyte. A hydrodynamic injection (9 s, 30 mbar) was applied and the separation was carried out using a separation temperature and voltage of 25°C and 25 kV, respectively. A capillary with two detection windows for serial online UV and fluorescence detection was satisfactorily employed. A solid-supported liquid-liquid extraction procedure was optimized for the clean-up of the urine samples and the extraction of the analytes. Matrix effects were assessed and signal suppression was observed for three of the analytes, thus, matrix-matched calibration was used for compensating residual matrix effects on these analytes. The proposed method allows the separation and quantification of the chemotherapeutics in less than 6 min. Detection limits range between 0.01 and 0.30 mg/L. The method was satisfactorily applied to the determination of the target compounds in human urine samples, with recoveries of 92.4-107.7%. PMID:25820908

  4. 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

  5. Determination of polycyclic aromatic hydrocarbons (PAH) in edible vegetable oils by liquid chromatography and programmed fluorescence detection. Comparison of caffeine complexation and XAD-2 chromatography sample clean-up.

    PubMed

    Welling, P; Kaandorp, B

    1986-08-01

    Two clean-up procedures were compared for the analysis for polycyclic aromatic hydrocarbons (PAHs) in edible vegetable oils. One method comprises a liquid-liquid extraction followed by XAD-2 chromatography and the other a caffeine-formic acid complexation. The clean-up step is followed by gradient reversed-phase HPLC in combination with wavelength-programmed fluorescence detection. Due to better repeatability and simplicity, the XAD-2 method was selected for the determination of PAHs in 14 different vegetable oils. Between the different oil samples large differences were observed in PAH concentrations. PAH concentrations in vegetable oils sampled from the Dutch market appear to be comparable with those found in other countries. PMID:3765851

  6. 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). PMID:25942557

  7. 48 CFR 36.512 - Cleaning up.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... 48 Federal Acquisition Regulations System 1 2011-10-01 2011-10-01 false Cleaning up. 36.512... CONTRACTING CONSTRUCTION AND ARCHITECT-ENGINEER CONTRACTS Contract Clauses 36.512 Cleaning up. The contracting officer shall insert the clause at 52.236-12, Cleaning Up, in solicitations and contracts when a...

  8. 48 CFR 36.512 - Cleaning up.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... 48 Federal Acquisition Regulations System 1 2010-10-01 2010-10-01 false Cleaning up. 36.512... CONTRACTING CONSTRUCTION AND ARCHITECT-ENGINEER CONTRACTS Contract Clauses 36.512 Cleaning up. The contracting officer shall insert the clause at 52.236-12, Cleaning Up, in solicitations and contracts when a...

  9. 48 CFR 36.512 - Cleaning up.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... 48 Federal Acquisition Regulations System 1 2014-10-01 2014-10-01 false Cleaning up. 36.512... CONTRACTING CONSTRUCTION AND ARCHITECT-ENGINEER CONTRACTS Contract Clauses 36.512 Cleaning up. The contracting officer shall insert the clause at 52.236-12, Cleaning Up, in solicitations and contracts when a...

  10. 48 CFR 36.512 - Cleaning up.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ... 48 Federal Acquisition Regulations System 1 2012-10-01 2012-10-01 false Cleaning up. 36.512... CONTRACTING CONSTRUCTION AND ARCHITECT-ENGINEER CONTRACTS Contract Clauses 36.512 Cleaning up. The contracting officer shall insert the clause at 52.236-12, Cleaning Up, in solicitations and contracts when a...

  11. 48 CFR 36.512 - Cleaning up.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... 48 Federal Acquisition Regulations System 1 2013-10-01 2013-10-01 false Cleaning up. 36.512... CONTRACTING CONSTRUCTION AND ARCHITECT-ENGINEER CONTRACTS Contract Clauses 36.512 Cleaning up. The contracting officer shall insert the clause at 52.236-12, Cleaning Up, in solicitations and contracts when a...

  12. Positive- and negative-ion mass spectrometry of diphenylmethane antihistaminics and their analogues and rapid clean-up of them from biological samples.

    PubMed

    Seno, H; Hattori, H; Kumazawa, T; Suzuki, O

    1993-12-01

    Positive-ion electron impact (PIEI), positive-ion chemical ionization (PICI) and negative-ion chemical ionization (NICI) mass spectra are presented for 15 compounds of diphenylmethane antihistaminics and their analogues, and each fragmentation pathway was analyzed. In the PIEI mode, molecular peaks were very small or missing for most compounds. Peaks at m/z 58, due to a dimethylaminomethyl group liberated, constituted base peaks in five compounds. Peaks at m/z 165 and/or 167, due to diaromatic rings plus a methyl group, appeared in most compounds. In the PICI mode, peaks due to M+H and M+C2H5 appeared in all compounds. Peaks due to diaromatic rings plus a methyl or ethyl group constituted base peaks in five compounds, which had an ether bond in their structures. In the NICI mode, anions at m/z M-H appeared in most compounds. Peaks at m/z 35 were observed for compounds having a chlorine group in their structures. Detection limits for total ion monitoring of these compounds were 20-50 ng on column in the PIEI mode, 100-200 ng in the PICI mode and 500-1000 ng in the NICI mode. A rapid and simple clean-up procedure of these drugs with use of Sep-Pak C18 cartridges is also presented. The drugs could be detected by gas chromatography with DB-1 and DB-17 capillary columns with satisfactory separation from impurities in their underivatized forms. The recovery of the drugs, which had been added to whole blood and urine, was more than 60% except for meclizine. PMID:8307529

  13. 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.

  14. Determination of neonicotinoid insecticides residues in bovine milk samples by solid-phase extraction clean-up and liquid chromatography with diode-array detection.

    PubMed

    Seccia, Serenella; Fidente, Paola; Montesano, Domenico; Morrica, Patrizia

    2008-12-19

    In this paper we have developed an analytical method for the simultaneous determination of four nicotinoid insecticides [acetamiprid (ACT), imidacloprid (ICL), thiacloprid (TCL) and thiamethoxam (TMX)] in bovine whole milk. These analytes were extracted, in a single step with dichloromethane, from fortified milk samples, using Chem Elut cartridges, containing diatomaceous earth material. Insecticide's determination and quantification were performed by HPLC with diode-array detection (DAD). Average recoveries of the four insecticides from bovine milk samples were between 85.1 and 99.7% at spiking levels 0.01, 0.05 and 0.1 mg kg(-1). Relative standard deviations (RSDs) were no larger than 10% for all of the recovery tests. The calculated limits of quantitation (LOQ) ranged from 0.01 to 0.04 mg kg(-1) for the four insecticides, being equal to or lower than the maximum residue limits (MRLs) established by European legislation (0.01-0.05 mg kg(-1)). The developed method is linear at concentrations within the tested interval, with coefficients of determination higher than 0.9990. According to Commission Decision 2002/657/EC, decision limit (CCalpha) and detection capability (CCbeta) have been calculated. The proposed method is rapid, simple and could be utilized for the routine analysis of pesticides residues. PMID:19004450

  15. Cleaning up blood samples using a modified "QuEChERS" procedure for the determination of drugs of abuse and benzodiazepines by UPLC-MSMS(☆).

    PubMed

    Anzillotti, Luca; Odoardi, Sara; Strano-Rossi, Sabina

    2014-10-01

    The "QuEChERS" (quick, easy, cheap, effective, rugged, and safe) dispersive SPE (dSPE) method is an emerging sample preparation technique that is becoming increasingly popular in the area of multi-residue pesticide analysis in food and agricultural products. A simplified QuEChERS extraction method followed by ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) has been developed for the simultaneous determination of forensically relevant drugs of abuse (opiates including buprenorphine, methadone and fentanyl and analogues, cocaine and metabolites, amphetamines, LSD) and benzodiazepines and analogues (Z-drugs) in 1mL of human whole blood performing a sole extraction. The method was validated showing good repeatability, accuracy and linearity; LODs were 0.5ng/mL for all benzodiazepines tested while for drugs of abuse LODs varied from 0.05 to 2ng/mL. The method showed high throughput capabilities and was applied on various forensic cases for determination of pharmaceuticals and drugs of abuse. PMID:24907511

  16. Exhaust gas clean up process

    SciTech Connect

    Walker, R.J.

    1989-04-11

    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 valuable sulfate salt.

  17. 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.

  18. 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.

  19. 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. PMID:26208666

  20. 48 CFR 52.236-12 - Cleaning Up.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... 48 Federal Acquisition Regulations System 2 2014-10-01 2014-10-01 false Cleaning Up. 52.236-12 Section 52.236-12 Federal Acquisition Regulations System FEDERAL ACQUISITION REGULATION (CONTINUED... Cleaning Up. As prescribed in 36.512, insert the following clause: Cleaning Up (APR 1984) The...

  1. 48 CFR 52.236-12 - Cleaning Up.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... 48 Federal Acquisition Regulations System 2 2010-10-01 2010-10-01 false Cleaning Up. 52.236-12 Section 52.236-12 Federal Acquisition Regulations System FEDERAL ACQUISITION REGULATION (CONTINUED... Cleaning Up. As prescribed in 36.512, insert the following clause: Cleaning Up (APR 1984) The...

  2. 48 CFR 52.236-12 - Cleaning Up.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... 48 Federal Acquisition Regulations System 2 2013-10-01 2013-10-01 false Cleaning Up. 52.236-12 Section 52.236-12 Federal Acquisition Regulations System FEDERAL ACQUISITION REGULATION (CONTINUED... Cleaning Up. As prescribed in 36.512, insert the following clause: Cleaning Up (APR 1984) The...

  3. 48 CFR 52.236-12 - Cleaning Up.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ... 48 Federal Acquisition Regulations System 2 2012-10-01 2012-10-01 false Cleaning Up. 52.236-12 Section 52.236-12 Federal Acquisition Regulations System FEDERAL ACQUISITION REGULATION (CONTINUED... Cleaning Up. As prescribed in 36.512, insert the following clause: Cleaning Up (APR 1984) The...

  4. 48 CFR 52.236-12 - Cleaning Up.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... 48 Federal Acquisition Regulations System 2 2011-10-01 2011-10-01 false Cleaning Up. 52.236-12 Section 52.236-12 Federal Acquisition Regulations System FEDERAL ACQUISITION REGULATION (CONTINUED... Cleaning Up. As prescribed in 36.512, insert the following clause: Cleaning Up (APR 1984) The...

  5. 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. PMID:24324610

  6. 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

  7. 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.

  8. 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.

  9. 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 263.31 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES (CONTINUED... up. A transporter must clean up any hazardous waste discharge that occurs during transportation...

  10. 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 263.31 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES (CONTINUED... up. A transporter must clean up any hazardous waste discharge that occurs during transportation...

  11. 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 263.31 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES (CONTINUED... up. A transporter must clean up any hazardous waste discharge that occurs during transportation...

  12. 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 263.31 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SOLID WASTES (CONTINUED... up. A transporter must clean up any hazardous waste discharge that occurs during transportation...

  13. 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...

  14. Clean-up criteria for remediation of contaminated soils

    SciTech Connect

    Nguyen, H.D.; Wilson, J.R.; Sato, Chikashi

    1997-08-01

    {open_quotes}How clean is clean?{close_quotes} is a question commonly raised in the remediation of contaminated soils. To help with the answer, criteria are proposed to serve as guidelines for remedial actions and to define a clean-up level such that the remaining contaminant residuals in the soil will not violate the Drinking Water Standards (DWS). The equations for computing those criteria are developed from the principle of conservation of mass and are functions of the maximum concentration level in the water (MCL) and the sorption coefficient. A multiplier, ranging from 10 to 1000, is also factored into the soil standard equation to reflect the effectiveness of various remediation techniques. Maximum allowable concentration in the soil (MSCL) is presented for several contaminants which are being regulated at the present time. Future modifications are recommended for better estimates of the MSCLs as additional transport mechanisms are incorporated to account for other potentially dominant effects.

  15. Addressing the challenges of tetracycline analysis in soil: extraction, clean-up, and matrix effects in LC-MS.

    PubMed

    O'Connor, Seamus; Locke, Jonas; Aga, Diana S

    2007-11-01

    An optimized extraction and clean-up method for the analysis of chlortetracycline, doxycycline, oxytetracycline, and tetracycline antibiotics in soil is presented in this work. Soil extraction using different solvents was performed, but the use of a 50 : 50 (v/v) methanol : acetate buffer (pH 8) solvent mixture in a pressurized liquid extraction (PLE) system proved to give the best extraction efficiency and reproducibility. The effect of soil composition on the PLE extraction efficiency was also examined, and results indicated that recovery data for one soil is not necessarily consistent with other soil types containing different compositions of clay and organic matter content. The percent recoveries of the optimized PLE method varied between the soils and ranged from 22-99%, depending on soil type, and more specifically clay content. In addition, the extent of ionization suppression caused by co-extracted humic acids was examined in an ion trap mass spectrometer (MS), and a single quadrupole MS. It was found that under positive electrospray ionization, the single quadrupole MS was less susceptible to ionization suppression than the ion trap MS. Therefore, various sample clean-up procedures were evaluated to selectively reduce the amount of co-extracted humic acids in the soil extracts. The most effective clean-up was obtained from the use of StrataX sorbent in combination with a strong anion exchange cartridge. PMID:17968453

  16. 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

  17. High-throughput method of dioxin analysis in aqueous samples using consecutive solid phase extraction steps with the new C18 Ultraflow™ pressurized liquid extraction and automated clean-up.

    PubMed

    Youn, Yeu-Young; Park, Deok Hie; Lee, Yeon Hwa; Lim, Young Hee; Cho, Hye Sung

    2015-01-01

    A high-throughput analytical method has been developed for the determination of seventeen 2,3,7,8-substituted congeners of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in aqueous samples. A recently introduced octadecyl (C18) disk for semi-automated solid-phase extraction of PCDD/Fs in water samples with a high level of particulate material has been tested for the analysis of dioxins. A new type of C18 disk specially designed for the analysis of hexane extractable material (HEM), but never previously reported for use in PCDD/Fs analysis. This kind of disk allows a higher filtration flow, and therefore the time of analysis is reduced. The solid-phase extraction technique is used to change samples from liquid to solid, and therefore pressurized liquid extraction (PLE) can be used in the pre-treatment. In order to achieve efficient purification, extracts from the PLE are purified using an automated Power-prep system with disposable silica, alumina, and carbon columns. Quantitative analyses of PCDD/Fs were performed by GC-HRMS using multi-ion detection (MID) mode. The method was successfully applied to the analysis of water samples from the wastewater treatment system of a vinyl chloride monomer plant. The entire procedure is in agreement with EPA1613 recommendations regarding the blank control, MDLs (method detection limits), accuracy, and precision. The high-throughput method not only meets the requirements of international standards, but also shortens the required analysis time from 2 weeks to 3d. PMID:25112208

  18. Screening and confirmation of thyreostatics in urine by gas chromatography with nitrogen-phosphorus detection and gas chromatography-mass spectrometry after sample clean-up with a mercurated affinity column.

    PubMed

    Schilt, R; Weseman, J M; Hooijerink, H; Korbee, H J; Traag, W A; van Steenbergen, M J; Haasnoot, W

    1989-04-01

    Methods are described for the screening and confirmation of residues of the thyreostatics thiouracil, methylthiouracil and propylthiouracil in urine samples of cattle at levels down to 25 micrograms/l. After a selective preconcentration of the thiol-containing thyreostatics on a mercurated affinity column, the analytes are derivatized by extractive alkylation and analysed by gas chromatography with nitrogen-phosphorus or mass spectrometric detection. PMID:2745644

  19. 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.

  20. Kinetics of combined SO/sub 2//NO in flue gas clean-up

    SciTech Connect

    Chang, S.G.; Littlejohn, D.

    1985-03-01

    The kinetics of reactions involving SO/sub 2/, NO, and ferrous chelate additives in wet flue gas simultaneous desulfurization and denitrification scrubbers are discussed. The relative importance of these reactions are assessed. The relevance of these reactions to spray dryer processes for combined SO/sub 2//NO flue gas clean-up is addressed. 37 refs., 7 figs.

  1. 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.

  2. Sulfide clean-up of solutions from heavy metal ions

    SciTech Connect

    Kislinskaya, G.E.; Kozachek, N.N.; Krasnova, G.M.; Shenk, N.I.

    1982-09-20

    The object of the present research was to determine the conditions for thorough clean-up of solutions from cadmium or mercury contamination by use of iron sulfide. Results indicated that the shape of the dependence of the degree of extraction of copper with iron sulfide on the pH value is analogous to the curve for cadmium; that is, copper, like cadmium, is precipitated by chemical reaction. In distinction from cadmium and copper, mercury is extracted by iron sulfide both in acid and also in neutral solutions, that is, it is possible to attain a direct ion exchange by reaction. At high pH values, only small amounts of iron go into solution, therefore FeS can be used very rationally for the extraction of both small (about 1 mg/liter), and also of large (about 1 mg/liter) amounts of mercury from solutions, which are nearly neutral. By adding sodium sulfide and a flocculant, one can accelerate the process of mercury precipitation, and also reduce the solution of iron sulfide. In the present case, iron sulfide plays the role of a substrate for the crystallization of mercury sulfide, since in dilute solutions the latter forms poorly filterable colloidal solutions. Thus when one uses fused iron sulfide with addition of sodium sulfide, a high degree of mercury extraction is attained, and the spent sorbent is filtered well.

  3. 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.

  4. Bioremediation: environmental clean-up through pathway engineering.

    PubMed

    Singh, Shailendra; Kang, Seung Hyun; Mulchandani, Ashok; Chen, Wilfred

    2008-10-01

    Given the immense risk posed by widespread environmental pollution by inorganic and organic chemicals, novel methods of decontamination and clean-up are required. Owing to the relatively high cost and the non-specificity of conventional techniques, bioremediation is a promising alternative technology for pollutant clean-up. Advances in bioremediation harness molecular, genetic, microbiology, and protein engineering tools and rely on identification of novel metal-sequestering peptides, rational and irrational pathway engineering, and enzyme design. Recent advances have been made for enhanced inorganic chemical remediation and organic chemical degradation using various pathway-engineering approaches and these are discussed in this review. PMID:18760355

  5. 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

  6. 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…

  7. 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.

  8. 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...

  9. 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)

  10. Improved clean-up for the determination of lasalocid in 'difficult' food matrices.

    PubMed

    Tarbin, J A; Rawlings, E; Tyler, D; Sharman, M

    2002-01-01

    Methodology has been developed for the determination of lasalocid in analytically 'difficult' matrices such as processed and spiced foods. The procedure was based on an existing silica-based solid-phase extraction (SPE) clean-up to which was added a novel NH2 SPE step before HPLC with fluorescence detection. Use of the additional step enabled the determination of lasalocid in matrices such as baby food, meat pies ('pasties'), etc. Analysis of these matrices was not possible using the standard clean-up on its own. Chromatography showed a massive reduction in the amount of co-extractives and interferences. Validation data were obtained down to the 10-40 mg kg(-1) level for a range of products. Recoveries ranged from 74% at 10 microg kg(-1) for pork sausages to 96% at 40 microg kg(-1) for meat pies. PMID:11817373

  11. 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

  12. 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

    2013-10-01

    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

  13. 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. PMID:26560633

  14. Determination of organochlorine and pyrethroid pesticides in fruit and vegetables using solid phase extraction clean-up cartridges.

    PubMed

    Sharif, Zawiyah; Man, Yaakob Bin Che; Hamid, Nazimah Sheikh Abdul; Keat, Chin Cheow

    2006-09-15

    A method to determine six organochlorine and three pyrethroid pesticides in grape, orange, tomato, carrot and green mustard based on solvent extraction followed by solid phase extraction (SPE) clean-up is described. The pesticides were spiked into the sample prior to analysis, extracted with ethyl acetate, evaporated and reconstituted with a solvent mixture of acetone:n-hexane (3:7). Three different sorbents (Strong Anion Exchanger/Primary Secondary Amine (SAX/PSA), Florisil and C18) were used for the clean-up step. Pesticides were eluted with 5mL of acetone:n-hexane (3:7, v/v) and determined by gas chromatography and electron-capture detection (GC-ECD). SAX/PSA was the sorbent, which provided chromatograms with less interference and the mean recoveries obtained were within 70-120% except for captafol. The captafol recoveries for grape were within acceptable range with C18 clean-up column. PMID:16857206

  15. Interim Site Assessment and Clean-up Guidebook

    SciTech Connect

    Elliott, K.L.

    1996-12-31

    In April 1995 an Interim Site Investigation and Clean-up Guidebook (for petroleum hydrocarbon and volatile organic compound impacted sites) was developed for public use. The purpose of the Guidebook was to offer a new approach to the site cleanup process: one that reduces time, cuts costs, and establishes a defined endpoint for investigations and cleanup actions. The Guidebook provided a matrix to screen for low-risk contaminated sites. After a year of use, the Guidebook was revised in May 1996. The most notable change was in the Petroleum Hydrocarbon Section and the modification of the screening table for petroleum hydrocarbon contaminated sites. The changes considered the strong influence of lithology on contaminant transport and recognized the large attenuation of the long chain, heavy oil and tar, hydrocarbons in soils.

  16. Cleaning up the nuclear weapons complex: A herculean challenge

    SciTech Connect

    Probst, K.N.; McGovern, M.H.

    1996-12-31

    For nearly five decades, the US Department of Energy (DOE) and its predecessors engaged in a highly secretive, complex, and massive endeavor to fabricate nuclear weapons for national security purposes. Large-scale production of nuclear weapons was an unprecedented undertaking requiring thousands of facilities, dozens of large tracts of land, huge volumes of dangerous materials, and great quantities of water. With the Cold Wars end and the emergence of new types of national security concerns, weapons production operations have, for the most part, ceased, and much of the secrecy under which they were shrouded has lifted. The subsequent revelation reveal at many sites tremendous volumes of soil and groundwater are contaminated with both radioactive and hazardous materials. Wastes stored for years pose substantial dangers, and many aging facilities that harbor highly radioactive and sensitive materials are deteriorating. The topics covered in this overview article include the following: more to `cleanup` than cleaning up; a fragmented regulatory regime; new regulatory regimes.

  17. 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.

  18. Recent trends at the state and federal level in accelerating CERCLA clean-ups

    SciTech Connect

    Clegg, B.

    1996-12-31

    Efforts at accelerating remedial action at the federal level focus on the following: the Superfund accelerated clean-up model (SCAM); Brownfields economic redevelopment initiative; guidance documents and policies; and collaboration with state voluntary cleanup programs. At the state level efforts involved in accelerating clean-ups include voluntary clean-up programs and Brownfields initiatives.

  19. Capacity of the bioremediation technology for clean-up of soil and groundwater contaminated with petroleum hydrocarbons.

    PubMed

    Masak, Jan; Machackova, Jirina; Siglova, Martina; Cejkova, Alena; Jirku, Vladimir

    2003-01-01

    A column reactor was designed and used to simulate conditions affecting the bioremediations of petroleum hydrocarbons. The work illustratively describes the aerobic (model) clean-up of soil samples enabling to predict the efficiency of a technology installed in parallel on contaminated former airport. The data showing the performance of thus precharacterized technology are presented. PMID:14524696

  20. Extraction and clean-up of contaminants and toxicants from food for mass spectrometric analysis--a literature review.

    PubMed

    Reid, W J

    1986-01-01

    This report presents a review of the literature on the extraction and clean-up procedures used prior to the analysis, by mass spectrometry, of organic contaminants and toxicants in foods and food-related materials. It includes a brief description of the uses of a mass spectrometer and shows how the mode of operation of the machine can influence the amount of clean-up necessary before a sample is presented for analysis. The review covers a variety of contaminants of different compound types in a wide range of foods and not only discusses sample preparation techniques that have been used for contaminant analysis by mass spectrometry but also considers some that could be used. The most commonly used techniques involve solvent extraction followed by a clean-up using liquid-liquid partition or column chromatography or both, although a number of newer methods being evolved are moving towards the ideal of a single-step extraction and clean-up process. PMID:3514283

  1. Environmental benefits of Boston Harbor clean-up projects

    SciTech Connect

    Connor, M.S.; Smith, W.M. )

    1990-01-09

    The Massachusetts Water Resources Authority has undertaken one of the largest public works projects in the country to control the pollution of Boston Harbor. The project includes construction of a new primary and secondary treatment plant and sludge treatment facilities, excavation of a long ocean outfall and diffuser, and a solution to the overflow of mixed sewage and stormwater during storms; it will take over twenty years and billions of dollars to construct. A comparison of the relative costs and environmental benefits of relative costs and environmental benefits of the various construction projects, and other pollution control strategies, shows that some projects are more cost-effective than others for solving specific pollution problems. The capture and treatment of combined sewer overflow (CSO) will result in a more dramatic reduction of pathogen contamination than will completion of the primary and secondary treatment plants. Although the flow of raw sewage is intermittent and relatively small, it has high concentrations of bacteria and viruses. On the other hand, the new treatment plants will be more important in reducing toxic contamination of fish and shellfish. In summary, all the planned clean-up projects appear to be necessary to reach the goal of a swimmable, fishable Boston Harbor.

  2. Establishing a universal swabbing and clean-up protocol for the combined recovery of organic and inorganic explosive residues.

    PubMed

    Song-im, Nopporn; Benson, Sarah; Lennard, Chris

    2012-11-30

    A single-step solvent extraction and a solid-phase extraction (SPE) clean-up procedure was developed and optimised in order to establish a universal sampling and clean-up protocol for the combined recovery of organic and inorganic explosive residues. Mixtures of three common swabbing solvents (acetone, acetonitrile and methanol) with water, in various ratios, were assessed for the extraction of four target organic explosives [pentaerythritol tetranitrate (PETN), 2,4,6-trinitrotoluene (TNT), hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) and triacetone triperoxide (TATP)] and two inorganic anions (chlorate and nitrate) from alcohol wipes that were used as a swabbing medium. An efficient, single-step extraction of both organic and inorganic compounds from the wipes was achieved using 60% v/v methanol/water. To develop a clean-up procedure, four commercially available SPE cartridges (Oasis HLB, Isolute(®) C18, Bond-Elut(®) ENV and ABS ELUT Nexus) and an in-house packed XAD-7 cartridge were firstly evaluated for their retention capacity toward three organic explosives (PETN, TNT and RDX) in a mixture of methanol and water. A SPE technique was then developed and optimised from the short-listed sorbents with four representative organic explosives (including TATP). The Nexus cartridge was found to provide a suitable sorbent for extract clean-up following swab extraction with 60% v/v methanol/water. By incorporating the optimised clean-up procedure with the application of a polyester-based alcohol wipe as a sampling medium, a universal swabbing protocol for the combined recovery of both organic and inorganic explosive residues was established. The feasibility of the proposed protocol was assessed by collection and quantitation of the residue from a mixture of TNT, PETN and chlorate deposited on a laminate test surface. PMID:22959657

  3. 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.

  4. Application of electrokinetics for stimulating microbial clean-up of contaminated soils

    NASA Astrophysics Data System (ADS)

    Thompson, I.; Lear, G.

    2006-05-01

    Given sufficient time there are few synthetic compounds that can resist microbial degradation, a fact exploited in environmental clean-up. Despite this the performance of micro-organisms in remedial technologies is often sub-optimal. There are many reasons for the failure of indigenous microbial communities to reduce contaminant concentrations, including issues of bioavailability and the inability of the contaminants to switch on genes (catabolic) responsible for contaminant degradation. Even if the presence of the required catabolic genes is confirmed, there continues to be a significant need to develop procedures to stimulate their activity. We have investigated the potential of soil electrokinetics (3-4 A m-2) to stimulate microbial degradation of organic pollutants and move the soil contaminants relative to the degradative microorganisms, so increasing contact between the two components. Using soils contaminated with pentachlorophenol as our model laboratory system, we have demonstrated that the technique is effective at causing gross and controlled movement of PCP through soils at the laboratory-scale. It can also stimulate rates (up to 25% over that of the control) by which introduced bacteria degrade the contaminant. The additional potential benefits of electrokinetics in regard to stimulating microbial activity and soil clean-up will be discussed.

  5. [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. PMID:25764663

  6. 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

  7. 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 Who cleans up radioactive and hazardous material spills? The carrier is typically responsible for cleanup of a radioactive or hazardous material spill with assistance from the shipper...

  8. 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 Who cleans up radioactive and hazardous material spills? The carrier is typically responsible for cleanup of a radioactive or hazardous material spill with assistance from the shipper...

  9. 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 Who cleans up radioactive and hazardous material spills? The carrier is typically responsible for cleanup of a radioactive or hazardous material spill with assistance from the shipper...

  10. 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 Who cleans up radioactive and hazardous material spills? The carrier is typically responsible for cleanup of a radioactive or hazardous material spill with assistance from the shipper...

  11. 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 Who cleans up radioactive and hazardous material spills? The carrier is typically responsible for cleanup of a radioactive or hazardous material spill with assistance from the shipper...

  12. An investigation of critical parameters for optimum perforation clean-up

    SciTech Connect

    Hovem, K.; Joeranson, H.; Espedal, A.; Wilson, S.

    1995-12-31

    Field data presented in the paper suggest that an open-choke perforating practice improves perforation clean-up. An experimental and numerical investigation of this technique confirmed that an open-choke perforating practice leads to higher core flow efficiency compared to closed-choke perforating with subsequent clean-up flow.

  13. 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... Clean up, which will involve 40 divers cleaning the river bottom in Lake Havasu. The Coast Guard is... responsibilities between the Federal Government and Indian tribes. Energy Effects We have analyzed this rule...

  14. 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...

  15. 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...

  16. 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...

  17. 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...

  18. 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...

  19. 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 ADDITIVE PETITIONS General Provisions § 71.4 Samples; additional information. The Commissioner may request samples of the color additive,...

  20. Robotic soil sampler for hazardous waste clean up

    SciTech Connect

    Jaselskis, E.J.

    1992-01-01

    An innovative field sampling system using LA-ICP-AES (laser ablation-inductively coupled plasma -- atomic emission spectrometry) technology is currently being developed through an integrated team approach at Ames Laboratory to provide in-situ, real time analysis of inorganic hazardous waste. This sampling approach is conducted through a mobile testing facility which consists of an instrumentation vehicle called the Mobile Demonstration Laboratory for Environmental Screening Technologies (MDLEST), and an attached trailer called the Robotic Sampling Accessory (RSA). The RSA provides automated sampling capabilities through an attached three-degree-of-freedom robot that will be equipped with surface and subsurface sampling probes. The probes are currently being designed by a multidisciplinary team consisting of engineers and scientists at Ames Laboratory, Iowa State University, and Lockheed. This system is expected to improve sample quality assurance, reduce sampling time and cost, and improve worker safety. Limitations and future areas of research for the MDLEST-RSA are also discussed.

  1. Robotic soil sampler for hazardous waste clean up

    SciTech Connect

    Jaselskis, E.J.

    1992-06-01

    An innovative field sampling system using LA-ICP-AES (laser ablation-inductively coupled plasma -- atomic emission spectrometry) technology is currently being developed through an integrated team approach at Ames Laboratory to provide in-situ, real time analysis of inorganic hazardous waste. This sampling approach is conducted through a mobile testing facility which consists of an instrumentation vehicle called the Mobile Demonstration Laboratory for Environmental Screening Technologies (MDLEST), and an attached trailer called the Robotic Sampling Accessory (RSA). The RSA provides automated sampling capabilities through an attached three-degree-of-freedom robot that will be equipped with surface and subsurface sampling probes. The probes are currently being designed by a multidisciplinary team consisting of engineers and scientists at Ames Laboratory, Iowa State University, and Lockheed. This system is expected to improve sample quality assurance, reduce sampling time and cost, and improve worker safety. Limitations and future areas of research for the MDLEST-RSA are also discussed.

  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. Attitudes toward managing hazardous waste: What should be cleaned up and who should pay for it

    SciTech Connect

    Baron, J.; Kunreuther, H. ); Gowda, R. )

    1993-04-01

    Hazardous waste policy in the United States uses a liability-based approach, including strict, retroactive, and joint and several liability. To assess attitudes toward these basic principles of liability, and toward priorities for clean-up of wastes, a questionnaire was mailed to legislators, judges, executives of oil and chemical companies, environmentalists, and economists. The questionnaire consisted of abstract, simplified cases, which contrasted basic principles rather than dealing with real-world scenarios. Subjects were asked how they would allocate clean-up costs between companies and government as a function of such factors as adherence to standards, adoption of best available technology (BAT), and influence of penalties on future behavior. Most subjects felt that, if the company followed government standards or used the best available technology (BAT), it should pay for only a portion of the clean-up cost, with the government paying the rest. In general, responses did not support the principles underlying current law - strict, retroactive, and joint-and-several liability. Most subjects were more interested in polluters paying for damages than in deterrence or future benefit - even to the extent that they would have harmless' waste sites cleaned up. A bias was found toward complete clean-up of some sites, or zero risk.' Different groups of subjects gave similar answers, although more committed environmentalists were more willing to make companies pay and to clean up waste regardless of the cost. 21 refs., 3 tabs.

  4. Passive treatment technology cleans up colorado mining waste

    SciTech Connect

    Morea, S.; Olsen, R. ); Wildeman, T. )

    1990-12-01

    This article describes the performance of a module designed to treat acid mine drainage from an mining tunnel. The site is one of the many abandoned mineral mines in Colorado. At optimum conditions passive treatment removed up to 98% of the zinc, 99% of the copper, 94% of the lead, and 86% of the iron in the mine drainage. It also increased pH from 3.0 to a value greater than 6.5. This treatment meets the need for a low cost operating and maintenance system. Because of the success of the pilot plant, the project team has obtained a Superfund Innovative Technology Evaluation (SITE) program grant from the EPA to continue operating the pilot plant for two additional years and to prepare the first design manual on passive treatment technology.

  5. Growing Up and Cleaning Up: The Environmental Kuznets Curve Redux.

    PubMed

    Franklin, Rachel S; Ruth, Matthias

    2012-01-01

    Borrowing from the Kuznets curve literature, researchers have coined the term "environmental Kuznets curve" or EKC to characterize the relationship between pollution levels and income: pollution levels will increase with income but some threshold of income will eventually be reached, beyond which pollution levels will decrease. The link between the original Kuznets curve, which posited a similar relationship between income and inequality, and its pollution-concerned offspring lies primarily with the shape of both curves (an upside-down U) and the central role played by income change. Although the EKC literature has burgeoned over the past several years, few concrete conclusions have been drawn, the main themes of the literature have remained constant, and no consensus has been reached regarding the existence of an environmental Kuznets curve. EKC research has used a variety of types of data and a range of geographical units to examine the effects of income levels on pollution. Changes in pollution levels might also be at least partly explained by countries' position in the demographic transition and their general population structure, however little research has included this important aspect in the analysis. In addition, few analyses confine themselves to an evaluation for one country of the long-term relationship between income and pollution. Using United States CO2 emissions as well as demographic, employment, trade and energy price data, this paper seeks to highlight the potential impact of population and economic structure in explaining the relationship between income and pollution levels. PMID:25214678

  6. Growing Up and Cleaning Up: The Environmental Kuznets Curve Redux

    PubMed Central

    Franklin, Rachel S.; Ruth, Matthias

    2014-01-01

    Borrowing from the Kuznets curve literature, researchers have coined the term “environmental Kuznets curve” or EKC to characterize the relationship between pollution levels and income: pollution levels will increase with income but some threshold of income will eventually be reached, beyond which pollution levels will decrease. The link between the original Kuznets curve, which posited a similar relationship between income and inequality, and its pollution-concerned offspring lies primarily with the shape of both curves (an upside-down U) and the central role played by income change. Although the EKC literature has burgeoned over the past several years, few concrete conclusions have been drawn, the main themes of the literature have remained constant, and no consensus has been reached regarding the existence of an environmental Kuznets curve. EKC research has used a variety of types of data and a range of geographical units to examine the effects of income levels on pollution. Changes in pollution levels might also be at least partly explained by countries’ position in the demographic transition and their general population structure, however little research has included this important aspect in the analysis. In addition, few analyses confine themselves to an evaluation for one country of the long-term relationship between income and pollution. Using United States CO2 emissions as well as demographic, employment, trade and energy price data, this paper seeks to highlight the potential impact of population and economic structure in explaining the relationship between income and pollution levels. PMID:25214678

  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. 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. PMID:23939876

  9. Enhanced phyto-extraction not a feasible option to clean up uranium contaminated soil

    SciTech Connect

    Vandenhove, Hildegarde; Duquene, Lise; Wannijn, Jean; Filip, Tack; Baeten, Joke

    2007-07-01

    Available in abstract form only. Full text of publication follows: A greenhouse experiment was set up to evaluate the potential of enhanced phyto-extraction to clean up U contaminated soils. One soil had a naturally high U concentration and the other soil was impacted by effluents from the former radium extraction industry. Enhancement of U solubility and uptake by plants (ryegrass and Indian mustard) was monitored after addition of 5 chemical amendments (5 mmol kg{sup -1} soil dry weight): citric acid, ammonium citrate-citric acid mixture, oxalic acid, EDDS and NTA. Uranium solubilization and uptake were highly influenced by the amendment applied and soil-plant combinations. Citric acid was most effective in increasing U solubility (up to 18-fold increase). Citric acid and the ammonium citrate-citric acid mixture were most effective in increasing U uptake by ryegrass (up to 6-fold). For Indian mustard, EDDS and citric acid were most effective (up to 9- fold). In the optimal scenario only 0.16 % of the total uranium present in the soil could be extracted with one harvest and it would take more than 200 years to reduce the initial uranium content with 10 %. Based on these results, we must conclude that phyto-extraction is not a feasible technique to decrease the uranium concentration of historically contaminated soils. (authors)

  10. Denitrification: a Clean-Up Mechanism for High Nitrate Ground Water Near an Active Swine Facility?

    NASA Astrophysics Data System (ADS)

    Townsend, M. A.

    2001-05-01

    An active swine facility in south central Kansas appears to be cleaning up nitrate in regional ground water in an area with shallow ground water (<10 m), sandy soils, and irrigated and dry land row crop farming. This study used nitrogen stable isotopes and standard water chemistry to determine the impact of a bentonite lined hog lagoon on shallow ground-water chemistry. Regional ground water surrounding the facility had nitrate-nitrogen values routinely measured above 10 ppm. Chloride concentrations in the area ranged from 3 to 25 ppm and bicarbonate values ranged from 45 to 200 ppm. Two periods of sampling in the area showed nitrogen isotope values in the fertilizer range (<+2 to +8) and nitrate-N values above 10 ppm for all wells within a mile of a swine facility except for the monitoring well downgradient of the facility. This well had nitrate-N values of 4 to 5 ppm and nitrogen isotope values in the animal waste range (+13 to +20) which is similar to the value measured for the waste lagoon (+18). Chloride and bicarbonate values at all of the monitoring wells, except the well downgradient from the lagoon, were similar to the regional ground water. The lagoon water had >500 ppm chloride and >1400 ppm ammonium-N. The downgradient monitoring well had chloride values > 100 ppm and bicarbonate values above 400 ppm for the two sampling periods. Use of chloride ratios showed that approximately 30% of the water contributing to the downgradient well sample was from lagoon leakage. Preliminary calculations of the amount of bicarbonate resulting from denitrification processes, chloride ratios, and nitrogen isotope values suggest that the sampled water is a mixture of denitrified regional ground water plus lagoon water. Although the nitrate values near the swine facility appear to be decreasing, the long-term impact of increased salt load on the regional ground water is unknown at this time.

  11. 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.

  12. Analysis of polycyclic aromatic hydrocarbons in vegetable oils combining gel permeation chromatography with solid-phase extraction clean-up.

    PubMed

    Fromberg, A; Højgård, A; Duedahl-Olesen, L

    2007-07-01

    A semi-automatic method for the determination of polycyclic aromatic hydrocarbons (PAHs) in edible oils using a combined gel permeation chromatography/solid-phase extraction (GPC/SPE) clean-up is presented. The method takes advantage of automatic injections using a Gilson ASPEC XL sample handling system equipped with a GPC column (S-X3) and pre-packed silica SPE columns for the subsequent clean-up and finally gas chromatography-mass spectrometry (GC-MS) determination. The method was validated for the determination of PAHs in vegetable oils and it can meet the criteria for the official control of benzo[a]pyrene levels in foods laid down by the Commission of the European Communities. A survey of 69 vegetable oils sampled from the Danish market included olive oil as well as other vegetable oils such as rapeseed oil, sunflower oil, grape seed oil and sesame oil. Levels of benzo[a]pyrene in all the oils were low (<0.2-0.8 microg kg(-1)), except for one sample of sunflower oil containing 11 microg kg(-1) benzo[a]pyrene. PMID:17613061

  13. 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. PMID:24209351

  14. 21 CFR 71.4 - Samples; additional information.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... samples of the color additive, articles used as components thereof, or of the food, drug, or cosmetic in... additive, or articles used as components thereof, or of the food, drug, or cosmetic in which the color... respect to the safety of the color additive or the physical or technical effect it produces. The date...

  15. 21 CFR 71.4 - Samples; additional information.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... samples of the color additive, articles used as components thereof, or of the food, drug, or cosmetic in... additive, or articles used as components thereof, or of the food, drug, or cosmetic in which the color... respect to the safety of the color additive or the physical or technical effect it produces. The date...

  16. 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. PMID:26515281

  17. Ecologically-based clean-up criteria for nitroaromatic explosives using toxicity test results

    SciTech Connect

    Duh, D.; Roberts, B.; Buzgo, S.

    1995-12-31

    A former trinitrotoluene (TNT) production and storage facility was the focus of a Remedial Investigation (RI). Contaminants identified during the RI included 2,4-dinitrotoluene (DNT), 2,6-DNT, and 2,4,6-TNT, PCBs, arsenic, lead and chromium. The Conceptual Site Model determined there to be several complete exposure pathways. One of these identified a route by which soil invertebrate communities could be affected through dermal contact and ingestion of soil contaminants. Maintenance of the soil invertebrate community was chosen as the assessment endpoints for this pathway in the Ecological Risk Assessment. The corresponding measurement endpoint was survival of earthworms in 14-day toxicity tests in which they were exposed to site soils. Seven surficial soil samples were collected from Areas of Concern. Each sample was evaluated for acute toxicity to earthworms using standard USEPA protocols. Chemical concentrations were also measured. An artificial soil was used as the control and diluent to establish the Lethal Concentration (LC{sub 50}) of the test soils to earthworms. From the toxicity test results and the corresponding chemical analysis, a matrix of toxicity and contaminant levels was developed. This table was used to determine a concentration of each contaminant at which no acute lethality would be expected. Lower bounds to the chemical specific LC{sub 50} values were determined and, based on sample-specific toxicity units, appropriate LC{sub 50} values were derived (333 mg/kg 2,4-DNT, 182 mg/kg 2,6-DNT, and 1960 mg/kg 2,4,6TNT). Extrapolation of this level to a chronic No Observable Adverse Effect Level (NOAEL) provided a means of proposing site-specific ecologically based clean-up criteria for the constituents of concern which would be protective of the chosen assessment endpoint.

  18. Determination of etoxazole residues in fruits and vegetables by SPE clean-up and HPLC-DAD.

    PubMed

    Malhat, Farag; Badawy, Hany; Barakat, Dalia; Saber, Ayman

    2013-01-01

    A method for determination of etoxazole residues in apples, strawberries and green beans was developed and validated. The analyte was extracted with acetonitrile from foodstuff and a charcoal-celite cartridge was used for clean-up of raw extracts. Reversed phase high performance liquid chromatography with photodiode array detector (HPLC-DAD) was used for the determination and quantification of etoxazole residues in the studied samples. The calibration graphs of etoxazole in a solvent or three blank matrixes were linear within the tested intervals 0.01-2 mg L(-1), with correlation coefficient of determination >0.999. The combined solid phase extraction (SPE) clean-up and the chromatographic method steps were sensitive and reliable for simultaneous determination of etoxazole residues in the studied samples. The average recoveries of etoxazole in the tested foodstuffs were between 93.4 to 102% at spiking levels of 0.01, 0.10, and 0.50 mg kg(-1), with relative standard deviations ranging from 2.8 to 4.7%, in agreement with directives for method validation in residue analyses. The limit of detection (LOD) of the HPLC-DAD system was 100 pg. The limit of quantification of the entire method was 0.01 mg kg(-1). PMID:23431971

  19. 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...

  20. 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…

  1. 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...

  2. Fast and selective pressurized liquid extraction with simultaneous in cell clean up for the analysis of alkylphenols and bisphenol A in bivalve molluscs.

    PubMed

    Salgueiro-González, N; Turnes-Carou, I; Muniategui-Lorenzoa, S; López-Mahía, P; Prada-Rodríguez, D

    2012-12-28

    A novel and green analytical methodology for the determination of alkylphenols (4-tert-octylphenol, 4-n-octylphenol, 4-n-nonylphenol, nonylphenol technical mixture) and bisphenol A in bivalve mollusc samples was developed and validated. The method was based on selective pressurized liquid extraction (SPLE) with a simultaneous in cell clean up combined with liquid chromatography–electrospray ionization tandem mass spectrometry in negative mode (LC–ESI-MS/MS). Quantitation was performed by standard addition curves in order to correct matrix effects. The analytical features of the method were satisfactory: relative recoveries varied between 80 and 107% and repeatability and intermediate precision were <20% for all compounds. Uncertainty assessment of measurement was estimated on the basis of an in-house validation according to EURACHEM/CITAC guide. Quantitation limits of the method (MQL) ranged between 0.34 (4-n-octylphenol) and 3.6 ng g(−1) dry weight (nonylphenol). The main advantages of the method are sensitivity, selectivity, automaticity, low volumes of solvents required and low sample analysis time (according with the principles of Green Chemistry). The method was applied to the analysis of mussel samples of Galicia coast (NW of Spain). Nonylphenol and 4-tert-octylphenol were measured in all samples at concentrations between 9.3 and 372 ng g(−1) dw. As an approach, the human daily intake of these compounds was estimated and no risk for human health was found. PMID:23218190

  3. 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.

  4. 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.

  5. 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

  6. Planar solid phase extraction clean-up for pesticide residue analysis in tea by liquid chromatography-mass spectrometry.

    PubMed

    Oellig, Claudia; Schwack, Wolfgang

    2012-10-19

    Efficient clean-up is indispensable for preventing matrix effects in multi-residue analysis of pesticides in food by liquid and gas chromatography (LC and GC) coupled to mass spectrometry (MS). High-throughput planar solid phase extraction (HTpSPE) was recently introduced as a new clean-up concept in residue analysis of pesticides in fruit and vegetables (C. Oellig, W. Schwack, 2011 [45]). Thin-layer chromatography (TLC) was used to completely separate pesticides from matrix compounds and to focus them into a sharp zone, followed by extraction of the target zone by the TLC-MS interface. As rather challenging matrices, tea samples were chosen in this study. Besides chlorophylls and polyphenols, high amount of caffeine is co-extracted resulting in strong matrix effects both in LC-MS and GC-MS. The former HTpSPE procedure was adapted to initial extracts of green and black tea resulting in colorless extracts nearly free of matrix effects and interferences, as shown for seven chemically representative pesticides (acetamiprid, penconazole, azoxystrobin, chlorpyrifos, pirimicarb, fenarimol, and mepanipyrim). LC-MS/MS calibration curves obtained in the range of 0.002-0.5 mg/kg from matrix-matched standards and solvent standards were nearly identical and demonstrated the effectiveness of clean-up by HTpSPE. Mean recoveries determined by LC-MS/MS against solvent standards at spiking levels of 0.01 and 0.1 mg/kg ranged between 72 and 114% with relative standard deviations (RSDs) of 0.7-4.7% (n=4), while LC-MS measurements of tea samples spiked at 1 mg/kg provided recoveries of 81-104% with RSDs of 1.2-4.9% (n=6). Using LC-MS/MS, the method showed high sensitivity with signal-to-noise ratios>10 for concentrations below 0.002 mg/kg. HTpSPE of one sample was done in a few minutes, while numerous samples were cleaned in parallel at minimal costs with very low sample and solvent consumption. PMID:22981507

  7. 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

  8. Survey of aflatoxins in rice from Iran using immunoaffinity column clean-up and HPLC with fluorescence detection.

    PubMed

    Feizy, J; Beheshti, H R; Fahim, N Khoshbakht; Janati, S S Fakoor; Davari, G

    2010-01-01

    A study was undertaken to determine levels of aflatoxins in rice. A total of 261 rice samples were analyzed by HPLC using a method was based on the extraction of 50 g of finely ground rice plus 5 g NaCl with 200 ml of 80% methanol. After filtration and immunoaffinity clean-up, 20 µl was injected onto the HPLC. HPLC analysis was carried out using a Genesis RP C18 column (250 × 4.6, 4 µm I.D.) and a mobile phase with a linear gradient of water/methanol/acetonitrile (6 : 2 : 2 v/v) over 16 min. Aflatoxins were determined after post-column derivatisation with iodine by fluorescence detection at excitation and emission wavelengths of 365 and 445 nm, respectively. It was found that 68.9% of the rice samples contained aflatoxin B1 at levels greater than 0.2 ng g(-1). PMID:24779626

  9. 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). PMID:25529710

  10. 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

  11. The effect of water spray upon incineration flue gas clean-up

    NASA Astrophysics Data System (ADS)

    Wang, Haigang; Li, Bin; Liu, Shi; Pan, Zhonggang; Yan, Guizhang

    2000-06-01

    The existence of liquid water was found very important in incineration flue gas clean-up systems for enhancing the absorption of acid components contained. In a newly developed incineration flue gas clean-up tower, which works in a semi-dry mode, the water is injected in the form of spray to maximum its contact surface with the gas. The criteria for the design of the water nozzles would be high water concentration but no liquid impinging on the solid wall and complete evaporation inside the tower. In order to optimize the atomizer design, the effects of the spray type (hollow or solid cone), their initial droplet size distribution and water flow rate on the performance of the acid gas absorption were investigated. The liquid behaviour was studied with a fluid dynamic simulation code, and the overall performance was checked experimentally. This paper presents the use of a commercial CFD code, FLUENT, and some modifications made during such investigation. The modification includes the viscosity of the flue gas defined as a function of the temperature, and the initial mass fraction of different droplet size group described with an exponential distribution formula of Rosin-Rammler. The investigation results (the optimal spray parameters) were used to guide the water nozzle design. The general performance of the flue gas clean-up system measured during the plant operation complied with the design criteria.

  12. 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.

  13. A new multiple-stage electrocoagulation process on anaerobic digestion effluent to simultaneously reclaim water and clean up biogas.

    PubMed

    Liu, Zhiguo; Stromberg, David; Liu, Xuming; Liao, Wei; Liu, Yan

    2015-03-21

    A new multiple-stage treatment process was developed via integrating electrocoagulation with biogas pumping to simultaneously reclaim anaerobic digestion effluent and clean up biogas. The 1st stage of electrocoagulation treatment under the preferred reaction condition led to removal efficiencies of 30%, 81%, 37% and >99.9% for total solids, chemical oxygen demand, total nitrogen and total phosphorus, respectively. Raw biogas was then used as a reactant and pumped into the effluent to simultaneously neutralize pH of the effluent and remove H2S in the biogas. The 2nd stage of electrocoagulation treatment on the neutralized effluent showed that under the selected reaction condition, additional 60% and 10% of turbidity and chemical oxygen demand were further removed. The study concluded a dual-purpose approach for the first time to synergistically combine biogas purification and water reclamation for anaerobic digestion system, which well addresses the downstream challenges of anaerobic digestion technology. PMID:25540943

  14. 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

  15. 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. PMID:11144515

  16. Early aging in Chernobyl clean-up workers: long-term study.

    PubMed

    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

  17. Spinning filter separation system for oil spill clean-up operation

    SciTech Connect

    Wehrle, J.; Fischer, E.C.; Kenney, W.P.; Korczynski, J.F.; Gracik, T.D.

    1996-09-26

    According to current technology, effective clean up of oil spills from the surface of ocean water is performed by an oil sweeper vessel within which oil contaminated water is collected for transport to remotely located on-shore equipment within which oil separation and disposal is performed. The processing of large quantities of oil polluted ocean water is accordingly time consuming as well as costly. It is therefore an important object of the present invention to provide a less costly oil spill clean up system involving more rapid processing of large quantities of oil polluted ocean water. In accordance with the present invention, oil polluted ocean water is processed at an oil spill location by continuous separation during pressurized flow of the water through at least two separator devices within which successive reduction in oil concentration is effected with respect to a separated portion of the water by filtered flow through porous membrane walls to correspondingly increase the oil concentration within the other remaining portion of water being processed. The first portion of the processed water when sufficiently reduced in oil concentration is discharged for return to the oil spill location, while the remaining portion is collected until a sufficient level of oil concentration therein is achieved to permit disposal thereof by burning at the oil spill site.

  18. 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

  19. 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. PMID:23216411

  20. Does further clean-up reduce the matrix enhancement effect in gas chromatographic analysis of pesticide residues in food?

    PubMed

    Schenck, F J; Lehotay, S J

    2000-01-28

    Sample extracts of apples, peas, green beans, oranges, raspberries, clementines, carrots, and wheat obtained using the Food and Drug Administration (acetone extraction) and Canadian Pest Management Regulatory Agency (acetonitrile extraction) multiresidue methods for pesticides were subjected to clean-up using different solid-phase extraction (SPE) cartridges in an attempt to reduce or eliminate the matrix enhancement effect. The matrix enhancement effect is related to the blocking of active sites on the injector liner by matrix components, thereby increasing signal in the presence of matrix versus standards in solvent in which the pesticides themselves interact with the active sites. Graphitized carbon black (GCB) was often used in combination with various anion-exchange SPE cartridges. The extracts were then spiked with organophosphorus insecticides. These process standards were then compared to standards in acetone of the same concentration using gas chromatography with flame photometric detection or ion trap mass spectrometric detection. Sample matrix enhancement varied from little to no effect for some pesticides (e.g. chlorpyrifos, malathion) to >200% in the case of certain susceptible pesticides. The GCB removed color components but showed little effect in reducing matrix enhancement by itself. The anion-exchange cartridges in combination with GCB or not, substantially reduced the matrix enhancement effect but did not eliminate it. PMID:10677079

  1. Cleaning-up atrazine-polluted soil by using Microbial Electroremediating Cells.

    PubMed

    Domínguez-Garay, Ainara; Boltes, Karina; Esteve-Núñez, Abraham

    2016-10-01

    Biodegradation of pollutants in soil is greatly limited by the availability of terminal electron acceptors required for supporting microbial respiration. Such limitation can be overcome if soil-buried electrodes accept the electrons released in the microbial metabolism. We propose the term bioelectroventing for such a environmental treatment. The process would be performed in a device so-called Microbial Electroremediating Cell. Indeed, our studies demonstrate that the presence of electrodes as electron acceptors effectively stimulated by 5-fold the biodegradation rate of the herbicide atrazine (2-chloro-4-ethylamino-6-isopropyl amino-1,3,5-triazine) in comparison with soil natural attenuation. Furthermore, a different set of toxicological test using Pseudokirchneriella subcapitata green alga e, Salmonella typhimorium bacteria and Sorghum saccharatum plant seeds respectively, confirm that atrazine-polluted soil can be effectively cleaned-up in short time by the use of MERCs. PMID:27448317

  2. Soil clean up by in-situ aeration. 6. Effects of variable permeabilities

    SciTech Connect

    Gomez-Lahoz, C.; Rodriguez-Maroto, J.M. ); Wilson, D.J. )

    1991-02-01

    Soil vapor stripping (vacuum extraction) has become an important tool in the remediation of hazardous waste sites contaminated with volatile organic compounds (VOCs) in the vadose zone. A mathematical model for in-situ soil vapor stripping is developed and used to examine the effects of a spatially variable pneumatic permeability tensor on the rate of clean-up of a site contaminated with volatile organic compounds. Runs are made with low-permeability clay lenses placed at various locations in the domain of interest; also the effect of soil moisture distribution on the soil gas flow field is examined. The model permits one to carry out a sensitivity analysis of the effects of heterogeneity in the permeability, and to develop strategies for minimizing the damaging effects of domains of low permeability.

  3. 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.

  4. 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

  5. The integration of science and politics to clean up 50 years in the nuclear sandbox

    SciTech Connect

    Lyons, C.E.; Holeman, T.

    1999-07-01

    The Cold War was fought between world superpowers for approximately 40 years from the end of the second World War until the end of the 1980s. During that time, the US government devoted billions of dollars to the development and production of nuclear weapons. Now the Cold War is over and the US is left with numerous nuclear weapons factories, stockpiles of nuclear materials, and mountains of waste to decontaminate and decommission. In the heat of the Cold War, little or no thought was given to how the facilities building bombs would be dismantled. Far too little attention was paid to the potential human health and environmental impact of the weapons production. Now, dozens of communities across the country face the problems this negligence created. In many cases, the location, extent, and characteristics of the waste and contamination are unknown, due to negligence or due to intentional hiding of waste and associated problems. Water supplies are contaminated and threatened; air quality is degraded and threatened; workers and residents risk contamination and health impacts; entire communities risk disaster from potential nuclear catastrophe. The US government, in the form of the US Department of Energy (DOE), now accepts responsibility for creating and cleaning up the mess. But it is the local communities, the home towns of the bomb factories and laboratories, that carry a significant share of the burden of inventing the science and politics required to clean up 50 years in the nuclear sandbox. The purpose of this paper is to evaluate the role of the local community in addressing the cleanup of the US nuclear weapons complex. Local governments do not own nor are responsible for the environmental aftermath, but remain the perpetual neighbor to the facility, the hometown of workers, and long-term caretaker of the off-site impacts of the on-site contamination and health risks.

  6. [Non-Parametric Analysis of Radiation Risks of Mortality among Chernobyl Clean-Up Workers].

    PubMed

    Gorsky, A I; Maksioutov, M A; Tumanov, K A; Shchukina, N V; Chekin, S Yu; Ivanov, V K

    2016-01-01

    Analysis of the relationship between dose and mortality from cancer and circulation diseases in the cohort of Chernobyl clean-up workers based on the data from the National Radiation and Epidemiological Registry was performed. Medical and dosimetry information on the clean-up workers, males, who got radiation doses from April 26, 1986 to April 26, 1987, which was accumulated from 1992 to 2012, was used for the analysis. The total size of the cohort was 42929 people, 12731 deaths were registered in the cohort, among them 1893 deaths from solid cancers and 5230 deaths were from circulation diseases. An average age of the workers was 39 years in 1992 and the mean dose was 164 mGy. The dose-effect relationship was estimated with the use of non-parametric analysis of survival with regard to concurrence of risks of mortality. The risks were estimated in 6 dose groups of similar size (1-70, 70-130, 130-190, 190-210, 210-230 and.230-1000 mGy). The group "1-70 mGy" was used as control. Estimated dose-effect relationship related to cancers and circulation diseases is described approximately with a linear model, coefficient of determination (the proportion of variability explained by the linear model) for cancers was 23-25% and for circulation diseases - 2-13%. The slope coefficient of the dose-effect relationship normalized to 1 Gy for the ratio of risks for cancers in the linear model was 0.47 (95% CI: -0.77, 1.71), and for circulation diseases it was 0.22 (95% CI: -0.58, 1.02). Risks coefficient (slope coefficient of excess mortality at a dose of 1 Gy) for solid cancers was 1.94 (95% CI: - 3.10, 7.00) x 10(-2) and for circulation diseases it was 0.67 (95% CI: -9.61, 11.00) x 10(-2). 137 deaths from radiation-induced cancers and 47 deaths from circulation diseases were registered during a follow up period. PMID:27534064

  7. Terminating Safeguards on Excess Special Nuclear Material: Defense TRU Waste Clean-up and Nonproliferation - 12426

    SciTech Connect

    Hayes, Timothy; Nelson, Roger

    2012-07-01

    The Department of Energy (DOE) and the National Nuclear Security Administration (NNSA) manages defense nuclear material that has been determined to be excess to programmatic needs and declared waste. When these wastes contain plutonium, they almost always meet the definition of defense transuranic (TRU) waste and are thus eligible for disposal at the Waste Isolation Pilot Plant (WIPP). The DOE operates the WIPP in a manner that physical protections for attractiveness level D or higher special nuclear material (SNM) are not the normal operating condition. Therefore, there is currently a requirement to terminate safeguards before disposal of these wastes at the WIPP. Presented are the processes used to terminate safeguards, lessons learned during the termination process, and how these approaches might be useful for future defense TRU waste needing safeguards termination prior to shipment and disposal at the WIPP. Also described is a new criticality control container, which will increase the amount of fissile material that can be loaded per container, and how it will save significant taxpayer dollars. Retrieval, compliant packaging and shipment of retrievably stored legacy TRU waste has dominated disposal operations at WIPP since it began operations 12 years ago. But because most of this legacy waste has successfully been emplaced in WIPP, the TRU waste clean-up focus is turning to newly-generated TRU materials. A major component will be transuranic SNM, currently managed in safeguards-protected vaults around the weapons complex. As DOE and NNSA continue to consolidate and shrink the weapons complex footprint, it is expected that significant quantities of transuranic SNM will be declared surplus to the nation's needs. Safeguards termination of SNM varies due to the wide range of attractiveness level of the potential material that may be directly discarded as waste. To enhance the efficiency of shipping waste with high TRU fissile content to WIPP, DOE designed an over

  8. 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. PMID:26355664

  9. Multiresidue determination of pesticides in plants by high-performance liquid chromatography following gel permeation chromatographic clean-up.

    PubMed

    Balinova, A

    1998-10-01

    Gel permeation chromatography was applied as a clean-up step in a HPLC multiresidue method for the determination of several pesticides in plants, not amenable to analysis by GC. The pesticides investigated were diflubenzuron, triflumuron, clofentezine, hexythiazox and flufenoxuron. The clean-up technique resulted in a good separation of analytes from co-extractive matrix compounds. Complete HPLC separation of all pesticides was achieved under the conditions selected. The analytical procedure was characterized with high accuracy and precision and acceptable sensitivity to meet requirements for monitoring these pesticides in crops. PMID:9818389

  10. Determination of Aflatoxin M1 in Milk Powder by Ultrasonic-Assisted Extraction and Dispersive Solid-Phase Clean-up.

    PubMed

    Manoochehri, Mahboobeh; Asgharinezhad, Ali Akbar; Safaei, Mahdi

    2015-07-01

    This work describes the application of ultrasound-assisted dispersive solid-phase extraction (UA-DSPE) as a sample preparation approach for aflatoxin M1 (AFM1) and also its subsequent determination by HPLC-fluorescence detection. A Box-Behnken design in combination with response surface methodology was implemented to determine the variables affecting the extraction procedure. The effects of different variables, including type and quantity of clean-up phase, ultrasonication time, ultrasonication temperature, nature and volume of the leaching solvent, were investigated in the optimization study. Primary secondary amine (PSA) and acetonitrile were selected as the clean-up phase and the leaching solvent, respectively. The obtained optimized values were 30 mg of PSA, 10 min ultrasonication time, 32°C ultrasonication temperature and 10 mL of acetonitrile. Under the optimal conditions, the limit of detection and limit of quantification were 0.0012 and 0.0045 µg kg(-1), respectively. The recoveries of the UA-DSPE procedure ranged from 80 to 92%, with relative standard deviations lower than 10% in all cases. Eventually, this method was successfully applied to the extraction of AFM1 in milk powder samples. PMID:25378372

  11. Diving behaviour of wildlife impacted by an oil spill: A clean-up and rehabilitation success?

    PubMed

    Chilvers, B L; Morgan, K M; Finlayson, G; Sievwright, K A

    2015-11-15

    The value of rehabilitating oiled wildlife is an on-going global debate. On October 5, 2011, the cargo vessel C/V Rena grounded on Astrolabe Reef, New Zealand (NZ), spilling over 300 tonnes of heavy fuel oil. As part of the Rena oil spill response, 383 little blue penguins (LBP, Eudyptula minor) were captured, cleaned, rehabilitated and released back into a cleaned environment. This research investigates foraging behaviour changes due either to the oil spill or by the rehabilitation process by comparing the diving behaviour of rehabilitated (n=8) and non-rehabilitated (n=6) LBPs and with LBP populations throughout NZ. Stabile isotope analysis of feathers was also used to investigate diet. There were no foraging behaviour differences between rehabilitated and non-rehabilitated LBPs and the overall diving behaviour of these LBPs have similar, if not less energetic, foraging behaviour than other LBPs in NZ. This suggests the rehabilitation process and clean-up undertaken after the Rena appears effective and helps justify the rehabilitation of oiled wildlife across the world. PMID:26424224

  12. 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.

  13. Diethylaminoethyl-cellulose clean-up of a large volume naphthenic acid extract.

    PubMed

    Frank, Richard A; Kavanagh, Richard; Burnison, B Kent; Headley, John V; Peru, Kerry M; Der Kraak, Glen Van; Solomon, Keith R

    2006-08-01

    The Athabasca oil sands of Alberta, Canada contain an estimated 174 billion barrels of bitumen. During oil sands refining processes, an extraction tailings mixture is produced that has been reported as toxic to aquatic organisms and is therefore collected in settling ponds on site. Investigation into the toxicity of these tailings pond waters has identified naphthenic acids (NAs) and their sodium salts as the major toxic components, and a multi-year study has been initiated to identify the principal toxic components within NA mixtures. Future toxicity studies require a large volume of a NA mixture, however, a well-defined bulk extraction technique is not available. This study investigated the use of a weak anion exchanger, diethylaminoethyl-cellulose (DEAE-cellulose), to remove humic-like material present after collecting the organic acid fraction of oil sands tailings pond water. The NA extraction and clean-up procedure proved to be a fast and efficient method to process large volumes of tailings pond water, providing an extraction efficiency of 41.2%. The resulting concentrated NA solution had a composition that differed somewhat from oil sands fresh tailings, with a reduction in the abundance of lower molecular weight NAs being the most significant difference. This reduction was mainly due to the initial acidification of tailings pond water. The DEAE-cellulose treatment had only a minor effect on the NA concentration, no noticeable effect on the NA fingerprint, and no significant effect on the mixture toxicity towards Vibrio fischeri. PMID:16469358

  14. Determination of diphenamide, napropamide and metolachlor in tobacco by gel permeation chromatographic clean-up and high performance liquid chromatography.

    PubMed

    Liu, Hongxia; Dang, Yuanlin; Zhang, Shusheng; Liu, Huimin; Qu, Lingbo; Liao, Xincheng; Zhao, Yufen; Wu, Yangjie

    2005-05-01

    Diphenamide, napropamide and metolachlor (FIG. 1) are selective, pre-emergence arylamide herbicides used to control the growth of annual grasses and broadleaf weeds in a variety of fields, e.g. fruit trees, nuts, corns, green crops, etc. They possess high activity and moderate toxicity. For food and environment safety, the detailed investigations on their residues and metabolism are very important. Diphenamide, napropamide and metolachlor in the pesticide products, serum, urine, soil, environmental water, fruits and wine have been widely analyzed by ELISA, fluorescence, phosphorescence, capillary electrophoresis, high performance liquid chromatography (HPLC), gas chromatography(GC) and GC mass spectrometry (GC-MS). However, to our knowledge, simultaneous residue analysis of diphenamide, napropamide and metolachlor in tobacco samples has not been extensively documented. Tobacco is greatly consumed by smokers throughout the world. The pesticide residue in tobaccos might be potentially harmful to smokers' health. With this in mind the residue determination and control of diphenamide, napropamide and metolachlor in the tobacco leaves are very important for tobacco products and consumers. For these three herbicides, the tolerable maximum residue limits (MRLs) have been limited ranging from 0.05 (for tobacco products) to 5 mg/kg (for tobacco leaves) in different European countries. For the complex tobacco samples, the GC and HPLC with UV detection suffer from matrix interference making quantification and identification of these herbicides difficult. In such cases the removal of the matrix effects and identification of the target compounds are of great importance. The present work reports the extraction and clean up procedures, as well as, the chromatographic conditions developed for the simultaneous determination of diphenamide, napropamide and metolachlor residues in the fluecured tobacco leaves, from the different sources using HPLC-UV method. PMID:16477944

  15. Determination of cocaine in postmortem human liver exposed to overdose. Application of an innovative and efficient extraction/clean up procedure and gas chromatography-mass spectrometry analysis.

    PubMed

    Magalhães, Elisângela Jaqueline; Ribeiro de Queiroz, Maria Eliana Lopes; Penido, Marcus Luiz de Oliveira; Paiva, Marco Antônio Ribeiro; Teodoro, Janaína Aparecida Reis; Augusti, Rodinei; Nascentes, Clésia Cristina

    2013-09-27

    A simple and efficient method was developed for the determination of cocaine in post-mortem samples of human liver via solid-liquid extraction with low temperature partitioning (SLE-LTP) and analysis by gas chromatography coupled to mass spectrometry (GC-MS). The extraction procedure was optimized by evaluating the influence of the following variables: pH of the extract, volume and composition of the extractor solvent, addition of a sorbent material (PSA: primary-secondary amine) and NaCl to clean up and increase the ionic strength of the extract. A bovine liver sample that was free of cocaine was used as a blank for the optimization of the SLE-LTP extraction procedure. The highest recovery was obtained when crushed bovine liver (2g) was treated with 2mL of ultrapure water plus 8mL of acetonitrile at physiological pH (7.4). The results also indicated no need for using PSA and NaCl. The complete analytical procedure was validated for the following figures of merit: selectivity, lower limit of quantification (LLOQ), calibration curve, recovery, precision and accuracy (for within-run and between-run experiments), matrix effect, dilution integrity and stability. The within-run and between-run precision (at four levels) varied from 2.1% to 9.4% and from 4.0% to 17.0%, respectively. A maximum deviation of 11.62% for the within-run and between-run accuracies in relation to the nominal concentrations was observed. Moreover, the LLOQ value for cocaine was 50.0ngg(-1) whereas no significant effects were noticed in the assays of dilution integrity and stability. To assess its overall performance, the optimized method was applied to the analysis of eight human liver samples collected from individuals who died due to the abusive consumption of cocaine. Due to the existence of a significant matrix effect, a blank human liver was used to construct a matrix-matched analytical curve. The concentrations of cocaine found in these samples ranged from 333.5 to 5969ngg(-1). PMID

  16. 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)

  17. Determination of pesticides in edible oils by liquid chromatography-tandem mass spectrometry employing new generation materials for dispersive solid phase extraction clean-up.

    PubMed

    Dias, Jonatan V; Cutillas, Victor; Lozano, Ana; Pizzutti, Ionara R; Fernández-Alba, Amadeo R

    2016-09-01

    The goal of this work was to evaluate the efficiency of several sorbents on removal fats from edible oils (olive, soya and sunflower) during the clean-up step for posterior determination of 165 pesticides by UHPLC-QqQ-MS/MS system. The extraction procedure employed in this work was the citrate version of QuEChERS method followed by a step of freezing out with dry ice and clean-up evaluation using i) PSA with magnesium sulfate (d-SPE); ii) magnesium sulfate and Z-sep sorbent (d-SPE); iii) Z-sep (column SPE) and iv) Agilent Bond Elut QuEChERS Enhanced Matrix Removal-Lipid (EMR-Lipid). After evaluation of the recovery results at 10, 20 and 50μgkg(-1), the EMR-Lipid showed important advantages comparing to the other sorbents evaluated, such as better recovery rates and RSD%. The method was validated at the three concentrations described above. Analytical curves linearity was evaluated by spiking blank oil samples at 10, 20, 50, 100 and 500μgkg(-1). The method demonstrated good recoveries values between the acceptable range of 70-120% and RSD%<20 for most of evaluated pesticides. In order to evaluate the performance of the method, this same procedure was employed to other oils such as soya and sunflower with very good results. PMID:27507727

  18. 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.

  19. [Simultaneous determination of zeranols and chloramphenicol in foodstuffs of animal origin by combination immunoaffinity column clean-up and liquid chromatography-tandem mass spectrometry].

    PubMed

    Wang, Qing; Wang, Guomin; Xi, Cunxian; Li, Xianliang; Chen, Dongdong; Tang, Bobin; Zhang, Lei; Zhao, Hua

    2014-06-01

    A combination immunoaffinity column (IAC-CZ) clean-up and liquid chromatography-tandem mass spectrometry (LC-MS/MS) analytical method was successfully developed for zearalenol, beta-zearalenol and zearalenone) and chloramphenicol (CAP) in foodstuffs of animal origin. The samples (fish, liver, milk and honey) were enzymatically digested by beta-glucuronidase/sulfatase for about 16 h and then extracted with ether. The extracts were evaporated to dryness and then the residues were dissolved by 1.0 mL of 50% acetonitrile solution. After filtered and diluted with PBS buffer, the reconstituted solution were cleaned-up with a IAC-CZ and then analyzed by LC-MS/MS in multiple reaction monitoring (MRM) mode. The chromatographic separation was performed on a Shimadzu Shim-pack VP-ODS column with gradient elution by acetonitrile and 2 mmol/L ammonium acetate solution. The detection was carried out by electrospray negative ionization mass spectrometry in MRM mode. The proposed method was validated by the limit of detection (0.04-0.10 microg/kg), linearity (R2 > or = 0.999 0), average recoveries (70.9%-95.6%) and precisions (2.0% - 11.8%). The developed method is reliable, sensitive and has good applicability. The combination immunoaffinity column was proved to be an effective pretreatment technique to decrease the matrix effect, and it met the requirements of residue analysis of co-occurring zeranols and chloramphenicol. PMID:25269264

  20. Clinical aspects of the health disturbances in Chernobyl Nuclear Power Plant accident clean-up workers (liquidators) from Latvia.

    PubMed

    Eglite, M E; Zvagule, T J; Rainsford, K D; Reste, J D; Curbakova, E V; Kurjane, N N

    2009-06-01

    The health status of some 6,000 workers from Latvia who went to clean-up the Chernobyl Nuclear Power Plant (CNPP) site following the explosion on 26 April 1986 has been analyzed. The data on these workers have been recorded in the Latvian State Register of Occupational disease patients and people exposed to ionizing radiation due to Chernobyl NPP accident (Latvian State Register) that was established in 1994. From these data, estimates have been made of external ionizing radiation to which these workers were exposed together with observations on the impact of exposure to heavy metals (especially lead and zinc) and radioactive isotopes released during the reactor 'meltdown'. These factors along with psycho-emotional and social-economic stresses account for a marked excess of mortality and morbidity in the group of CNPP accident clean-up workers compared with that of the non-exposed normal Latvian population adjusted for age and sex. The number of diseases or conditions in the CNPP accident clean-up workers has progressively risen from an average of 1.3 in 1986 to 10.9 in 2007. This exceeds for the Latvian population when adjusted for age and sex. The most serious conditions affect the nervous, digestive, respiratory, cardiovascular, endocrine (especially thyroid) and immunological systems. While the morbidity associated with diseases of the respiratory and digestive systems has decreased in recent years that in the other systems is increasing. In recent years, there has been an increased occurrence of cancers affecting the thyroid, prostate and stomach. Clinical and laboratory investigations suggest that surviving CNPP accident clean-up workers exhibit signs of immuno-inflammatory reactions causing premature aging with evidence of autoimmune diseases and immunological deficiencies or abnormalities. It is suggested that the CNPP accident clean-up workers may have a specific syndrome, the 'Chernobyl post-radiation neurosomatic polypathy', due to sustained oxidant

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

    PubMed

    Oellig, Claudia

    2016-05-01

    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. PMID:27059398

  2. 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

  3. 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)

  4. 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. PMID:26653466

  5. Evaluation of a solid-phase extraction dual-layer carbon/primary secondary amine for clean-up of fatty acid matrix components from food extracts in multiresidue pesticide analysis.

    PubMed

    Shimelis, Olga; Yang, Yuhui; Stenerson, Katherine; Kaneko, Toshiro; Ye, Michael

    2007-09-21

    The use of dual-layer solid-phase extraction (SPE), a primary-secondary amine (PSA) in combination with graphitized carbon black (GCB), was evaluated for sample clean-up during multiresidue pesticide screening of agricultural and food products. The retention of fatty acids by the PSA sorbent was quantified and the effect of the elution solvent on the retention of fatty acid on the SPE cartridge was evaluated. The use of stronger elution solvents to elute certain pesticides from graphitized carbon was shown to interfere with the capacity of PSA to bind fatty acids. A suitable protocol was tested using GCB/PSA dual-layer SPE to clean-up several food matrices and to simultaneously screen multiple fortified pesticides with a wide range of physico-chemical properties. With a few exceptions, pesticide recoveries were between 85% and 110%, and sample-to-sample differences of less than 5% were achieved, demonstrating the versatile suitability of the dual-layer SPE to sample clean-up. PMID:17689545

  6. 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)

  7. Methodology and data used for estimating the complex-wide impacts of alternative environmental restoration clean-up goals

    SciTech Connect

    Shay, M.R.; Short, S.M.; Stiles, D.L.

    1994-03-01

    This paper describes the methodologies and data used for estimating the complex-wide impacts of alternative strategies for conducting remediation of all DOE sites and facilities, but does not address issues relating to Waste Management capabilities. Clean-up strategies and their corresponding goals for contaminated media may be driven by concentration-based regulatory standards, land-use standards (e.g., residential, industrial, wild life reserve, or totally restricted), risk-based standards, or other standards determined through stakeholder input. Strategies implemented to achieve these goals usually require the deployment of (a) clean-up technologies to destroy, remove, or contain the contaminants of concern; (b) institutional controls to prevent potential receptors from coming into contact with the contaminants; or (c) a combination of the above.

  8. 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.

  9. Improvement of chemical analysis of antibiotics. IX. A simple method for residual tetracyclines analysis in honey using a tandem cartridge clean-up system.

    PubMed

    Oka, H; Ikai, Y; Kawamura, N; Uno, K; Yamada, M; Harada, K; Uchiyama, M; Asukabe, H; Mori, Y; Suzuki, M

    1987-03-13

    A simple, rapid and precise analytical method for the residual tetracyclines in honey has been established using a tandem cartridge clean-up system (prepacked reversed-phase and ion-exchange cartridges) followed by high-performance liquid chromatography. The recoveries of oxytetracycline (OTC), tetracycline (TC), chlortetracycline (CTC) and doxycycline (DC) from honey spiked at a level of 1.0 ppm are 87.1, 85.3, 98.0 and 99.0%, respectively, with coefficients of variation of 1.1-3.9%. The detection limits in honey are 0.02 ppm for OTC and TC, and 0.05 ppm for CTC and DC, respectively. The time required for the analysis of four samples is only 1 h. PMID:3106387

  10. Effects of demolition and beach clean-up operations on birds on a coastal mudflat in New Jersey

    NASA Astrophysics Data System (ADS)

    Burger, Joanna

    1988-07-01

    Coastal lands are increasingly exposed to disturbances from demolition, beach clean-up, and construction for development. Although data exist concerning the effects of investigators on breeding populations, little information is available for migrant populations. I investigated the effects of demolition and beach clean-up on resident and migrant birds on a coastal mudflat in New Jersey. A year's censusing before work initiation was used to determine when demolition and clean-up would affect the least number of birds. Work activity on and along the beach was from 15 October to 15 November 1985. The overall population size was lower in 1985 compared to the same period in 1984, although the drop in numbers was not due solely to human disturbance. Human work activity influenced avian distribution along the mudflat: birds moved farther along the beach and out onto the mudflat when activity began, and moved back onto the mudflat when activity ceased. For gulls, foraging efficiency was lowered when work began and did not return to previous levels until 60-90 min after work began. Gulls that moved farther out on the mudflat had significantly lower foraging efficiencies than did those that remained close to the beach. Efforts to mitigate the adverse effects on birds by restricting human activity to a 100 m stretch of beach at any one time succeeded in significantly reducing adverse effects and in allowing birds some space to rest and feed.

  11. 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.

  12. Simultaneous determination of four aflatoxins and ochratoxin A in ginger and related products by HPLC with fluorescence detection after immunoaffinity column clean-up and postcolumn photochemical derivatization.

    PubMed

    Wen, Jing; Kong, Weijun; Wang, Jian; Yang, Meihua

    2013-12-01

    Ginger, a widely used spice and traditional Chinese medicine, is prone to be contaminated by mycotoxins. A simple, sensitive, and reproducible method based on immunoaffinity column clean-up coupled with HPLC and on-line postcolumn photochemical derivatization with fluorescence detection was developed for the simultaneous determination of aflatoxins (AFs) B1 , B2 , G1 , G2 , and ochratoxin A (OTA) in 25 batches of gingers and related products marketed in China for the first time. The samples were first extracted by ultrasonication with methanol/water (80:20, v/v) and then cleaned up with immunoaffinity columns for analysis. Under the optimized conditions, the LODs and LOQs for the five mycotoxins were 0.03-0.3 and 0.1-0.9 μg/kg, respectively. The average recoveries ranged from 81.3-100.8% for AFs and from 88.6-99.5% for OTA at three spiking levels. Good linearity was observed for the analytes with correlation coefficients all >0.9995. All moldy gingers were contaminated with at least one kind of the five investigated mycotoxins, while none of them were found in normal gingers. Ginger powder samples were contaminated slightly with the contamination levels below the LOQs, while ginger tea bags were mainly contaminated by OTA at 1.05-1.19 μg/kg and ginger black tea bags were mainly contaminated by AFs at 3.37-5.76 μg/kg. All the contamination levels were below the legally allowable limits. PMID:24115567

  13. 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.

  14. Determination of endocrine disrupting compounds in fish liver, brain, and muscle using focused ultrasound solid-liquid extraction and dispersive solid phase extraction as clean-up strategy.

    PubMed

    Ros, Oihana; Vallejo, Asier; Olivares, Maitane; Etxebarria, Nestor; Prieto, Ailette

    2016-08-01

    This study describes a new method for the simultaneous extraction of several endocrine disrupting compounds, including alkylphenols (APs), estrogen, bisphenol-A (BPA) and one phthalate metabolite (mono-2-ethylhexyl ester, MEHP) in fish liver, brain, and muscle. Parameters affecting the extraction (extraction solvent and temperature) and the clean-up (dispersive phase nature and amount) steps were evaluated. The extraction was performed by means of focused ultrasound solid-liquid extraction (FUSLE) using 10 mL of n-hexane:acetone (50:50, v/v) for 5 min at ~0 °C, and the clean-up was done by means of dispersive solid phase extraction (dSPE) using 100 mg of ENVI-CARB and 100 mg of MgSO4 for the cleaning of brain and muscle extracts together with 100 mg of PSA in the case of liver extracts. Good apparent recoveries were obtained in the case of liver (62-132 %), brain (66-120 %), and muscle (74-129 %), relative standard deviation (RSD%) was always below 26 %, and the method detection limits (MDLs) were at low ng/g level. The developed method was applied to fish captured in Urdaibai estuary (Bay of Biscay) in December 2015, and the concentrations obtained were in the range MDL-1115 ng/g in brain, MDL-962 ng/g in muscle, and MDL-672 ng/g in liver. In general, the highest concentrations were measured in liver, followed by brain and muscle. In addition, diethylstilbestrol was only detected in fish brain. Graphical Abstract MS method scheme for the/MS method scheme for the determination of EDCs in fish liver, brain and muscle. PMID:27342793

  15. Multiresidue determination of 11 new fungicides in grapes and wines by liquid-liquid extraction/clean-up and programmable temperature vaporization injection with analyte protectants/gas chromatography/ion trap mass spectrometry.

    PubMed

    González-Rodríguez, Rosa M; Cancho-Grande, Beatriz; Simal-Gándara, Jesús

    2009-08-01

    A gas chromatographic ion trap mass spectrometry (GC-ITMS) method was developed for the determination of 11 new generation fungicides (benalaxyl, benalaxyl-M, boscalid, cyazofamid, famoxadone, fenamidone, fluquinconazole, iprovalicarb, pyraclostrobin, trifloxystrobin and zoxamide) in grapes and wines. Samples were extracted with ethyl acetate:hexane (1:1, v/v) and cleaned-up with graphitized carbon black/primary secondary amine (GCB/PSA) solid-phase extraction (SPE) cartridges using acetonitrile:toluene (3:1, v/v) as eluent. The addition of analyte protectants (3-ethoxy-1,2-propanediol, d-sorbitol and l-gulonic acid gamma-lactone) in the final extracts allowed to avoid the matrix-induced response enhancement effect on quantitation process with absolute recoveries ca. 100%. Precision (expressed as relative standard deviation) was lower than 16% for all fungicides. Limits of detection and quantitation were lower than 0.01 mg/kg or mg/L, except for cyazofamid, much smaller in all cases than maximum residue levels (MRLs) established by European Union for grapes and by Switzerland and Italy for wines. The proposed method was applied to determine fungicide residues in three different white grapes for vinification produced in Ribeiro area in Galicia (NW Spain), as well as in their corresponding final wines. PMID:19576591

  16. 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

  17. Application of ion-exchange cartridge clean-up in food analysis. V. Simultaneous determination of sulphonamide antibacterials in animal liver and kidney using high-performance liquid chromatography with ultraviolet and mass spectrometric detection.

    PubMed

    Ito, Y; Oka, H; Ikai, Y; Matsumoto, H; Miyazaki, Y; Nagase, H

    2000-11-10

    A simple, rapid, and reliable method for the determination of residual sulphonamide antibacterials (SAs) (sulfadiazine, sulfamerazine, sulfadimidine, sulfamethoxypiridazine, sulfisozole, sulfamonomethoxine, sulfamethoxazole, sulfisoxazole, sulfadimethoxine, and sulfaquinoxaline) in animal liver and kidney was developed using a combination of clean-up on a Bond Elut PSA cartridge and HPLC with UV detection. The SAs were extracted with ethyl acetate and then dissolved in 5 ml of 50 v/v% ethyl acetate-n-hexane after being evaporated to dryness. For clean-up of the crude sample, the resuspended extract was applied to a Bond Elut PAS (primary/secondary amine cartridge), and then SAs were eluted from the cartridge using 5 ml of 20 v/v% acetonitrile-0.05 M ammonium formate before being analysed by HPLC. Recoveries of the SAs at the levels of 0.5 and 0.1 microg/g were 70.8-98.2%, the rerative standard deviation were less than 7.0%, and the detection limits were 0.03 microg/g. The present analysis method of SAs in animal kidney and liver using HPLC with a clean-up procedure was demonstrated to be highly applicable to the direct LC-MS-MS analysis without any modification. PMID:11185627

  18. 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. PMID:25990350

  19. Historical Waste Retrieval and Clean-up Operations at Nuclear facility no.56, at the Cadarache Nuclear Research Centre

    SciTech Connect

    Santucci, C.

    2008-01-15

    Among the different activities of the CEA research centre in Cadarache, located in the south of France, one of the most important involves cleaning, cleansing dismantling, decommissioning, and recovery of legacy wastes. This presentation will give an overview of the waste retrieval project from the historical interim storage facility called INB 56. The project is divided into three different sub-projects: the historical unpacked waste retrieval, the historical canister retrieval and the draining and clean-up of the spent fuel pools. All the described operations are conducted in accordance with the ALARA principle and the optimization of the waste categorization. The overall project, including the complete clean-up of the facility and its de-licensing, is due to end by 2020. The aim of this document is to outline the general ongoing historical waste retrieval operations and future projects on the INB 56 at the Cadarache research centre. In the final analysis, it can be seen that most of the waste is to be sent to the new CEDRA facility. Nevertheless one major goal of this project is to optimize the waste categorization and therefore to send the canisters to the ANDRA LLW site whenever possible. Two means will allow us to reach this goal: - The sorting out of un-packed waste in order to constitute a LLW canister - A wide range of measurements (gamma spectrometry, neutron measurement, tomography) in order to assess the exact nature of the contents in the historical canisters. Taking waste treatment and conditioning into account well in advance is a factor of prime importance that must be managed early in the elaboration of the decommissioning scenario. Precise knowledge of the physical and radiological inventories is of the utmost importance in defining the best waste pathway. Overall operations on the facility are due to end by 2020 including complete clean-up of the facility and its de-licensing.

  20. A Team of Seven--The Tanks Focus Area program providing technical solutions for cleaning up DOE's radioactive waste tanks

    SciTech Connect

    Cosby, Wayne C.

    2000-09-04

    The U.S. Department of Energy initiated the Tanks Focus Area (TFA) concept in 1994 to integrate the cleanup efforts of the sites containing radioactive tank wastes. A team of seven contractors and national laboratories was assembled to develop and implement technical solutions to the unique problems encountered in cleaning up large quantities of highly radioactive wastes in tanks that can only be accessed through riser pipes. TFA work focuses on safety, characterization, retrieval, pretreatment, immobilization, and closure. Many technologies are under development, two of which are the highly successful cesium removal system and the robotic light duty utility arm for deploying equipment inside tanks.

  1. 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.

  2. 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.

  3. 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.

  4. 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...

  5. 49 CFR 199.111 - Retention of samples and additional testing.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... 49 Transportation 3 2014-10-01 2014-10-01 false Retention of samples and additional testing. 199.111 Section 199.111 Transportation Other Regulations Relating to Transportation (Continued) PIPELINE... SAFETY DRUG AND ALCOHOL TESTING Drug Testing § 199.111 Retention of samples and additional testing....

  6. [The retrospective cytogenetic dosimetry using the results of conventional chromosomal analysis in Chernobyl clean-up workers].

    PubMed

    Maznik, N A; Vinnikov, V A

    2005-01-01

    The paper presents the results of the cohortal biodosimetry carried out in 435 Chernobyl clean-up workers, who were surveyed with the conventional cytogenetic technique in terms from several days to 10 years after the end of their duties in the Chernobyl accident exclusive zone. An empirical model of the aberrant cell dynamics was utilized for the calculation of mean initial yields of dicentrics and centric rings in groups with different terms and duration of staying in the Chernobyl zone. Corresponding protracted irradiation doses estimated from aberration levels ranged from 79 to 670 mGy. The probabilistic distribution of the radiation doses was constructed by the applying the Bayesian analysis to initial individual chromosome exchange yields extrapolated to the exposure termination moment. This distribution was characterized by the mean dose about 460 mGy and maximum of probability density in the interval of 50-300 mGy. For the late somatic risk assessment in clean-up workers the probabilistic distribution of equivalentally-acute radiation doses was proposed; that had the mean value about 270 mGy, modal classes of 250-350 mGy and 99.8% of the probability density concentrated within the dose range from 0 to 1000 mGy. PMID:16454338

  7. I{ Relationship between source clean up and mass flux of chlorinated solvents in low permeability settings with fractures}

    NASA Astrophysics Data System (ADS)

    Bjerg, P. L.; Chambon, J. C.; Christiansen, C. M.; Broholm, M. M.; Binning, P. J.

    2009-04-01

    Groundwater contamination by chlorinated solvents, such as perchloroethylene (PCE), often occurs via leaching from complex sources located in low permeability sediments such as clayey tills overlying aquifers. Clayey tills are mostly fractured, and contamination migrating through the fractures spreads to the low permeability matrix by diffusion. This results in a long term source of contamination due to back-diffusion. Leaching from such sources is further complicated by microbial degradation under anaerobic conditions to sequentially form the daughter products trichloroethylene, cis-dichloroethylene (cis-DCE), vinyl chloride (VC) and ethene. This process can be enhanced by addition of electron donors and/or bioaugmentation and is termed Enhanced Reductive Dechlorination (ERD). This work aims to improve our understanding of the physical, chemical and microbial processes governing source behaviour under natural and enhanced conditions. That understanding is applied to risk assessment, and to determine the relationship and time frames of source clean up and plume response. To meet that aim, field and laboratory observations are coupled to state of the art models incorporating new insights of contaminant behaviour. The long term leaching of chlorinated ethenes from clay aquitards is currently being monitored at a number of Danish sites. The observed data is simulated using a coupled fracture flow and clay matrix diffusion model. Sequential degradation is represented by modified Monod kinetics accounting for competitive inhibition between the chlorinated ethenes. The model is constructed using Comsol Multiphysics, a generic finite- element partial differential equation solver. The model is applied at well characterised field sites with respect to hydrogeology, fracture network, contaminant distribution and microbial processes (lab and field experiments). At one of the study sites (Sortebrovej), the source areas are situated in a clayey till with fractures and

  8. 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. PMID:23929782

  9. 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. PMID:25647492

  10. 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. PMID:26747688

  11. Extraction and clean-up procedure for analysis of organochlorine pesticide residues in ethoxylated lanolin.

    PubMed

    Polese, L; Sannomiya, M; de Olivera Sader, A P; Lúcia Ribeiro, M

    2000-01-01

    In the present study an evaluation was made of a method for the determination of organochlorine pesticide residues in ethoxylated lanolin. Samples were homogenized with Celite, transferred to chromatographic columns, prepacked with silica gel deactivated to 10%. The pesticide elution was processed with n-hexane-dichloromethane and the concentrated eluate was analyzed using gas-liquid chromatography (GC) with electron capture detection (ECD). The composition of the elution solvent was a significant factor for the recovery of the pesticides. Mean recoveries obtained for fortified samples ranged from 87 to 94% for p,p'-DDE, dieldrin, endrin, p,p'-DDD and p,p'-DDT. Optimization of the experimental conditions resulted in a small-scale method that combines extraction and cleanup in a single step. PMID:11152246

  12. 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.

  13. 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. PMID:15162854

  14. [Simultaneous determination of 16 organophosphorous pesticides in vegetables, fruits and tea by gas chromatography coupled with clean-up by mesoporous alumina as solid-phase extraction adsorbent].

    PubMed

    Hu, Yeqin; Xi, Cunxian; Cao, Shurui; Wang, Guomin; Li, Xianliang; Zhang, Lei; Zhang, Yunhuai

    2014-07-01

    A gas chromatographic method based on solid-phase extraction was developed for the simultaneous determination of 16 organophosphorous pesticides in vegetables, fruits and tea, including cabbage, lettuce, pumpkin, onion, tomato, turnip, apple, pear and tea. The samples were extracted with ethyl acetate, and clean-up with mesoporous alumina as solid-phase extraction adsorbent. The separation of target compounds was performed on a DB-1701 capillary column, and the quantitative analysis of the organophosphorous pesticides was carried out by gas chromatography with flame photometric detection. The results showed that the calibration curves of the 16 organophosphorous pesticides were linear in the range of 10-2 000 microg/L with good correlation coefficients (R2 > 0.997). The recoveries of the pesticides in different samples at three spiked levels ranged from 83.2% to 103.8% with the relative standard deviations of 2.0%-9.9%. This method has high sensitivity, high accuracy and good repeatability, and can be applied to the determination of the organophosphorus pesticide residues in vegetables, fruits and tea. PMID:25255574

  15. 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.

  16. Clean-up progress at the SNL/NM Classified Waste Landfill

    SciTech Connect

    Slavin, P.J.; Galloway, R.B.

    1999-11-30

    The Sandia National Laboratories/New Mexico (SNL/NM)Environmental Restoration Project is currently excavating the Classified Waste Landfill in Technical Area II, a disposal area for weapon components for approximately 40 years until it closed in 1987. Many different types of classified parts were disposed in unlined trenches and pits throughout the course of the landfill's history. A percentage of the parts contain explosives and/or radioactive components or contamination. The excavation has progressed backward chronologically from the last trenches filled through to the earlier pits. Excavation commenced in March 1998, and approximately 75 percent of the site (as defined by geophysical anomalies) has been completed as of November 1999. The material excavated consists primarily of classified weapon assemblies and related components, so disposition must include demilitarization and sanitization. This has resulted in substantial waste minimization and cost avoidance for the project as upwards of 90 percent of the classified materials are being demilitarized and recycled. The project is using field screening and lab analysis in conjunction with preliminary and in-process risk assessments to characterize soil and make waste determinations in a timely a fashion as possible. Challenges in waste management have prompted the adoption of innovative solutions. The hand-picked crew (both management and field staff) and the ability to quickly adapt to changing conditions has ensured the success of the project. The current schedule is to complete excavation in July 2000, with follow-on verification sampling, demilitarization, and waste management activities following.

  17. Chemical Pollution and Evolution of Massive Starbursts: Cleaning up the Environment in Star-Forming Galaxies

    NASA Astrophysics Data System (ADS)

    Kobulnicky, C.

    1996-12-01

    I present the results of a research program seeking to characterize the impact of massive star-clusters on the chemical and dynamical evolution of metal-poor, irregular and blue compact galaxies. The evolution of high mass stars is thought to contribute the bulk of heavy element enrichment in the interstellar medium, especially alpha -process elements like O, Si, etc. Yet, in actively star-forming galaxies, localized chemical inhomogeneities are seldom observed. Spatially-resolved optical and ultraviolet spectroscopy from the Hubble Space Telescope and ground-based observatories is used to search for chemical enrichment in the vicinity of young star clusters in nearby galaxies. VLA aperture synthesis maps are used to examine the neutral hydrogen content, dynamics, and local environment of the sample galaxies. Despite the spread in evolutionary state of the starbursts determined by the EW of Balmer emission lines and the radio continuum spectral index, few instances of localized enrichment are found. In light of these data, the ``instantaneous enrichment'' scenario for extragalactic HII regions appears less probable than one which operates on long timescales and global spatial scales. The results are consistent with the idea that starburst driven winds expel freshly synthesized metals in a hot 10(6) K phase into the halos of galaxies where they cool, condense into globules, and mix homogeneously with the rest of the galaxy on long (dynamical) timescales. The C/O and N/O ratios of the galaxies are used as new tools for measuring the recent star formation history. Implications for chemical evolution of galaxies both locally and cosmologically are developed.

  18. 40 CFR 80.8 - Sampling methods for gasoline, diesel fuel, fuel additives, and renewable fuels.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... of the Federal Register under 5 U.S.C. 552(a) and 1 CFR part 51. To enforce any edition other than... 40 Protection of Environment 17 2014-07-01 2014-07-01 false Sampling methods for gasoline, diesel... Provisions § 80.8 Sampling methods for gasoline, diesel fuel, fuel additives, and renewable fuels....

  19. 19 CFR 151.11 - Request for samples or additional examination packages after release of merchandise.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... packages after release of merchandise. 151.11 Section 151.11 Customs Duties U.S. CUSTOMS AND BORDER... after release of merchandise. If the port director requires samples or additional examination packages... Administration may obtain samples of any food, drug, device, or cosmetic, the importation of which is governed...

  20. 19 CFR 151.11 - Request for samples or additional examination packages after release of merchandise.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... packages after release of merchandise. 151.11 Section 151.11 Customs Duties U.S. CUSTOMS AND BORDER... after release of merchandise. If the port director requires samples or additional examination packages... Administration may obtain samples of any food, drug, device, or cosmetic, the importation of which is governed...

  1. 19 CFR 151.11 - Request for samples or additional examination packages after release of merchandise.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... packages after release of merchandise. 151.11 Section 151.11 Customs Duties U.S. CUSTOMS AND BORDER... after release of merchandise. If the port director requires samples or additional examination packages... Administration may obtain samples of any food, drug, device, or cosmetic, the importation of which is governed...

  2. 19 CFR 151.11 - Request for samples or additional examination packages after release of merchandise.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... packages after release of merchandise. 151.11 Section 151.11 Customs Duties U.S. CUSTOMS AND BORDER... after release of merchandise. If the port director requires samples or additional examination packages... Administration may obtain samples of any food, drug, device, or cosmetic, the importation of which is governed...

  3. 19 CFR 151.11 - Request for samples or additional examination packages after release of merchandise.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... packages after release of merchandise. 151.11 Section 151.11 Customs Duties U.S. CUSTOMS AND BORDER... after release of merchandise. If the port director requires samples or additional examination packages... Administration may obtain samples of any food, drug, device, or cosmetic, the importation of which is governed...

  4. 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.

  5. 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

  6. 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

  7. Rapid screening method for quinolone residues in livestock and fishery products using immobilised metal chelate affinity chromatographic clean-up and liquid chromatography-fluorescence detection.

    PubMed

    Takeda, N; Gotoh, M; Matsuoka, T

    2011-09-01

    An efficient LC method was developed for screening the presence of quinolones (QLs)--comprising fluoroquinolones (FQs) and acidic quinolones (AQs)--residues in various livestock and fishery products. Targeted analytes were for nine FQs of marbofloxacin (MAR), ofloxacin (OFL), norfloxacin (NOR), ciprofloxacin (CIP), enrofloxacin (ENR), danofloxacin (DAN), orbifloxacin (ORB), difloxacin (DIF) and sarafloxacin (SAR), and three AQs of oxolinic acid (OXA), nalidixic acid (NAL) and flumequine (FMQ). Samples comprised ten different food products covering five matrices: muscle (cattle, swine and chicken), liver (chicken), raw fish (shrimp and salmon), egg (chicken), and processed food (ham, sausage and fish sausage). This method involved a simple extraction with (1:1) acetonitrile-methanol, a highly selective clean-up with an immobilised metal chelate affinity column charged with Fe(3+), a fast isocratic LC analysis using a short column (20 mm × 4.6 mm, 3 µm) with a mobile phase of (15:85:0.1) methanol/water/formic acid, and fluorescence detection (excitation/emission wavelengths of 295 nm/455 nm for FQs (495 nm for MAR), and 320 nm/365 nm for AQs). Among FQs, pairs of NOR/OFL, ORB/DIF and ENR/DAN were incompletely resolved. A confirmatory LC run with a Mg(2+) containing methanolic mobile phase was also proposed for the samples suspected of being positive. The optimised method gave satisfactory recoveries of 88.5% (56.1-108.6%) and 78.7% (44.1-99.5%) for intra- and inter-day assays with relative standard deviations of 7.2% (0.7-18.4%) and 6.8% (1.4-16.6%), respectively. Limits of quantitation ranged from 0.8 µg kg(-1) (DAN) to 6.5 µg kg(-1) (SAR). This method was successfully employed to analyse 113 real samples and two positive samples were found: fish sausage (CIP 990 µg kg(-1)) and shrimp (ENR 20 µg kg(-1)). PMID:21749230

  8. 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)

  9. 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…

  10. 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,…

  11. Cleaning Up High.

    ERIC Educational Resources Information Center

    Rittner-Heir, Robbin M.

    2001-01-01

    Discusses cleaning techniques and equipment for areas in a school that are hard to reach, such as the high spacious ceilings, the tall windows of a school atrium, and high points in gymnasiums and auditoriums. (GR)

  12. Clean Up after Yourself.

    PubMed

    Lepelley, Alice; Ghosh, Sankar

    2016-03-01

    NLRP3 inflammasome activation is accompanied by induction of mitochondrial damage. In the current issue of Cell, Zhong et al. describe an intracellular mechanism orchestrated by NF-κB to remove inflammasome-activating damaged mitochondria and prevent pathologic inflammation. PMID:26942667

  13. Oil spill clean up

    SciTech Connect

    Claxton, L.D.; Houk, V.S.; Williams, R.; Kremer, F.

    1991-01-01

    Due to the consideration of bioremediation for oil spills, it is important to understand the ecological and human health implications of bioremediation efforts. During biodegradation, the toxicity of the polluting material may actually increase upon the conversion of non-toxic constituents to toxic species. Also, toxic compounds refractory to biological degradation may compromise the effectiveness of the treatment technique. In the study, the Salmonella mutagenicity assay showed that both the Prudhoe Bay crude oil and its weathered counterpart collected from oil-impacted water were weakly mutagenic. Results also showed that the mutagenic components were depleted at a faster rate than the overall content of organic material.

  14. 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:

  15. 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. PMID:27492598

  16. Beyond Traditional Sampling Synthesis: Real-Time Timbre Morphing Using Additive Synthesis

    NASA Astrophysics Data System (ADS)

    Haken, Lippold; Fitz, Kelly; Christensen, Paul

    Because of its theoretical advantage for making timbral manipulations, sine wave additive synthesis is an attractive alternative to sampling synthesis, which is currently the most popular method for real-time synthesizers. Nevertheless, until recently performers have seldom used additive synthesis because of the practical difficulty of accomplishing these timbral manipulations, which inherently require modification of large numbers of time-varying amplitude and frequency control functions.

  17. 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

    2013-05-01

    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. PMID:23486692

  18. 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.

  19. Feasibility of photocatalytic oxidation for wastewater clean-up and reuse. Report for 4 Mar 81-31 Mar 81

    SciTech Connect

    Peyton, G.R.; DeBerry, D.W.

    1981-01-01

    A feasibility study has been conducted on a new treatment technology for the destruction of pollutant compounds in wastewater. The process uses solar energy to drive an oxidation which is photocatalyzed at the surface of a semiconductor powder. The process is being investigated particularly for water clean-up prior to industrial resuse, because of its non-energy-intensive nature. Five compounds (chloroform, dimethylamine, methanol, phenol, and ammonia) were used as model substrates, and removal at several pH values, using three different semiconductors (TiO2, ZnO, and Fe2O3) was investigated in the laboratory, using a xenon lamp to simulate solar radiation. While Fe2O3 was found to be ineffective, both ZnO and TiO2 catalyzed the removal of all compounds. Ammonia was not very effectively destroyed, but all four organic compounds experienced 30-50% removal in six hours at intensities slightly above that of normal solar radiation. Favorable cases were confirmed using sunlight. Quantum efficiencies for both sets of experiments were 13-20% for TiO2 and 4-7% using ZnO. Estimated treatment cost for a 1 mgd stream using laboratory conditions ranged from $0.18-$0.72 per thousand gallons, depending on the values of engineering parameters which were not investigated in this feasibility study.

  20. 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. PMID:15876215

  1. 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. PMID:27155437

  2. 49 CFR 199.111 - Retention of samples and additional testing.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... 49 Transportation 3 2013-10-01 2013-10-01 false Retention of samples and additional testing. 199.111 Section 199.111 Transportation Other Regulations Relating to Transportation (Continued) PIPELINE AND HAZARDOUS MATERIALS SAFETY ADMINISTRATION, DEPARTMENT OF TRANSPORTATION (CONTINUED) PIPELINE SAFETY DRUG AND ALCOHOL TESTING Drug Testing...

  3. 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

  4. 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. PMID:26515667

  5. Effects of atmospheric precipitation additions on phytoplankton photosynthesis in Lake Michigan water samples

    SciTech Connect

    Parker, J.I.; Tisue, G.T.; Kennedy, C.W.; Seils, C.A.

    1981-01-01

    The effects of incremental additions (0.1 to 50% v/v) of atmospheric precipitation on phytoplankton photosynthesis (/sup 14/C uptake) were tested in Lake Michigan water samples. Wet deposition was used in experiments I, III, and IV, and a melted snow core was used in experiment II. Additions of precipitation significantly reduced photosynthesis in the first three experiments, starting at about the 5 to 15% treatment level. No significant difference occurred in experiment IV, but photosynthesis was greater than in the control samples and this precipitation sample appeared to stimulate primary productivity. Soluble reactive phosphate, nitrate, and ammonia levels in the precipitation samples exceeded the lake water averages by factors of 10, 2, and 50, respectively. Silicon levels in precipitation reduced pH very little and no consistent relationship was observed with reduced photosynthesis. Alkalinity was greatly reduced in the treated samples and special precautions were required in ce, Ti, Be, Co, Cu, Mo, Ni, P,f the Pd crystals of about 30 A. Possible mechanisms are discussed for isotope exchange in CO molecules in these catalysts and for the promoting effect of Pd on the activity of CuO.

  6. Additive non-uniform random sampling in superimposed fiber Bragg grating strain gauge

    NASA Astrophysics Data System (ADS)

    Ma, Y. C.; Liu, H. Y.; Yan, S. B.; Yang, Y. H.; Yang, M. W.; Li, J. M.; Tang, J.

    2013-05-01

    This paper demonstrates an additive non-uniform random sampling and interrogation method for dynamic and/or static strain gauge using a reflection spectrum from two superimposed fiber Bragg gratings (FBGs). The superimposed FBGs are designed to generate non-equidistant space of a sensing pulse train in the time domain during dynamic strain gauge. By combining centroid finding with smooth filtering methods, both the interrogation speed and accuracy are improved. A 1.9 kHz dynamic strain is measured by generating an additive non-uniform randomly distributed 2 kHz optical sensing pulse train from a mean 500 Hz triangular periodically changing scanning frequency.

  7. Development And Implementation Of A Strategic Technical Baseline Approach For Nuclear Decommissioning And Clean Up Programmes In The UK

    SciTech Connect

    Brownridge, M.; Ensor, B.

    2008-07-01

    The NDA mission as set out within the Energy Act 2004 and stated in the NDA strategy is clear: - 'to deliver a world class programme of safe, cost-effective, accelerated and environmentally responsible decommissioning of the UK's civil nuclear legacy in an open and transparent manner and with due regard to the socio-economic impacts on our communities. Critical to achieving the NDA main objective and overall mission is to accelerate and deliver clean-up programmes through the application of appropriate and innovative technology. The NDA remit also requires us to secure good practice by contractors and carry out and promote research into matters relating to the decommissioning and clean up of nuclear installations and sites. NDA have defined a strategic approach for the underpinning of operational and decommissioning activities where each nuclear site is required to write within the Life Time Plans (LTP) the proposed technical baseline for those activities. This enables the robustness of the activities to be assessed, the gaps and opportunities and accompanying Research and Developments (R and D) requirements to be highlighted and investment to be targeted at key technical issues. NDA also supports the development of a commercial framework where innovation is encouraged and improvements can be demonstrated against the technical baseline. In this paper we will present NDA's overall strategic approach, the benefits already realised and highlight the areas for continued development. In conclusion: The development and implementation of a strategic approach to robustly underpin the technical components of the lifetime plans for operational and decommissioning activities on NDA sites has been extremely successful. As well as showing how mature technology assumptions are and where the key gaps and risks are it has also provided a method for highlighting opportunities to improve on that baseline. The use of a common template across all NDA LTPs has enabled direct comparison

  8. Overview of extraction, clean-up and detection techniques for the determination of organic pollutants in sewage sludge: a review.

    PubMed

    Zuloaga, O; Navarro, P; Bizkarguenaga, E; Iparraguirre, A; Vallejo, A; Olivares, M; Prieto, A

    2012-07-29

    analytical procedure (extraction, clean-up and analysis) have been reviewed. PMID:22769001

  9. 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. PMID:21684581

  10. 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

  11. 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.

  12. Simultaneous extraction and clean-up of polybrominated diphenyl ethers and polychlorinated biphenyls from sheep liver tissue by selective pressurized liquid extraction and analysis by gas chromatography-mass spectrometry.

    PubMed

    Zhang, Zulin; Ohiozebau, Ehimai; Rhind, Stewart M

    2011-02-25

    We describe a selective pressurized liquid extraction (SPLE) method, followed by gas chromatography-mass spectrometry (GC-MS), for the simultaneous extraction and clean-up of polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in sheep liver tissue samples. The on-line clean-up of liver tissue by SPLE was tested using differing amount of acid-modified silica (sulphuric acid:silica gel, 1:2, w/w), the most effective amount being 20 g. Different extraction solvents (iso-hexane and dichloromethane), either alone or in various combinations, were used to extract these target compounds from spiked liver samples. Variables affecting the SPLE extraction efficiency, including temperature, pressure, number of extraction cycles and static extraction time were studied; the optimum parameters were 80 °C, 10.3 MPa, 2 cycles and 5 min, respectively. The SPLE based method was compared with more traditional Soxhlet, off-line PLE, ultrasonic and heating extraction methods. Overall the mean percentage recoveries for all target chemicals using SPLE were 86-103% (n=3, SD < 9%), and compared favourably with the Soxhlet (63-109%, n=3, SD < 8%), off-line PLE (82-104%, n=3, SD < 18%), ultrasonic (86-99%, n=3, SD < 11%) and heating (72-102%, n=3, SD < 21%) extraction methods. The limits of detection of the proposed method were 5-96 pg g⁻¹ and 2-29 pg g⁻¹ for the different PBDE and PCB chemicals studied, respectively. The outputs of the proposed method were linear over the range from 0.02 to 30 ng g⁻¹, for all PCB and PBDE congeners except for PBDE 100 and 153 (0.05-30 ng g⁻¹) and PBDE 183 (0.1-30 ng g⁻¹). The method was successfully applied to sheep liver samples for the determination of the target PBDE and PCB compounds. PMID:21256501

  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. 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. PMID:26724558

  15. 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. PMID:27016959

  16. A novel method for high preconcentration of ultra trace amounts of B₁, B₂, G₁ and G₂ aflatoxins in edible oils by dispersive liquid-liquid microextraction after immunoaffinity column clean-up.

    PubMed

    Afzali, Daryoush; Ghanbarian, Maryam; Mostafavi, Ali; Shamspur, Tayebeh; Ghaseminezhad, Sima

    2012-07-20

    In the present study, a new approach which uses immunoaffinity column clean-up combined with dispersive liquid-liquid microextraction (DLLME) is proposed for the preconcentration of ultra trace amounts of aflatoxins (B₁, B₂, G₁ and G₂). The aflatoxins are then determined using a high-performance liquid chromatography coupled with fluorescent detector. Samples are extracted by immunoaffinity column (IAC) clean-up, and their eluents are used as dispersants of the subsequent DLLME, for further enrichment of aflatoxins. Various parameters (the type of elution solvent, the type and volume of extraction solvent and disperser solvent, extraction time, and centrifugation time) that affect the efficiency of the two steps are optimized. Under the optimum conditions (extraction solvent: 120 μL of chloroform, disperser solvent: 500 μL of acetonitrile, sample pH: 7.4, centrifugation time: 3 min), the calibration for B₁, B₂, G₁ and G₂ was found to be linear with coefficient of estimation (R²) of 0.9994, 0.9976, 0.9989, 0.9973 respectively and the limit of detection (LOD) was between 1.1 × 10⁻⁴ to 5.3 × 10⁻³ ng mL⁻¹ (3σ(b)/m, n=9). The recoveries at the two spiked levels ranged from 96.0 to 110.0% and the relative standard deviation (RSD) was less than 7.8% (n=9). The results show that dispersive liquid-liquid microextraction combined with HPLC is a selective, simple, sensitive, and effective analytical method for the preconcentration and determination of ultra trace amounts of aflatoxins. The proposed method was applied for preconcentration and determination of B₁, B₂, G₁ and G₂ aflatoxin in edible oils. Analysis of aflatoxins in FAPAS test material showed that the proposed method has good accuracy. PMID:22673813

  17. Feasibility of additional HTV operation requirement for sample returning capability from the ISS

    NASA Astrophysics Data System (ADS)

    Imada, Takane

    2006-07-01

    HTV (H-II transfer vehicle) is under development in JAXA as a service vehicle which delivers several items up to 6 ton to the ISS (International Space Station), however, it was not expected to have a recovery capability from the ISS. But after the NASA announcement about the Space Shuttle retirement after 2010, it is expected that the sample returning capability from the ISS will be drastically reduced after the retirement. It may also degrade the worth of the ISS as an experimental center on orbit. So, JAXA started the feasibility study about the additional function on HTV to equip a re-entry capsule in it to enable the recovery operation from the ISS. This study shows the preliminary feasibility assessment result of returning capsule in HTV carrier and the feasibility to equip small capsule and jettison system in carrier without major modification or safety impact to the ISS.

  18. 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.

  19. Pressurized liquid extraction with in-cell clean-up followed by gas chromatography-tandem mass spectrometry for the selective determination of parabens and triclosan in indoor dust.

    PubMed

    Canosa, P; Pérez-Palacios, D; Garrido-López, A; Tena, M T; Rodríguez, I; Rubí, E; Cela, R

    2007-08-17

    A sample preparation method based on the use of pressurized liquid extraction is proposed for the determination of four alkyl parabens and triclosan in indoor dust. Extraction of analytes and removal of interfering species were achieved in the same step, by placing an appropriate sorbent in the extraction cell and by choosing a right combination of washing and elution solvents. Compounds, as silylated derivatives, were determined by gas chromatography in combination with tandem mass spectrometry (GC-MS/MS). Factors affecting the yield and selectivity of the sample preparation procedure were carefully evaluated. Under final conditions, dried samples (0.5 g of dust and 1g of sodium sulphate) were dispersed with 3g of Florisil and loaded into an 11 mL stainless-steel extraction cell containing 1g of the same material as clean-up sorbent. Non-polar species were removed with n-hexane under mild conditions (40 degrees C, 3.4 MPa) and then analytes were extracted with ethyl acetate. The best compromise extraction conditions were 103 degrees C, 13.8 MPa and 3 static extraction cycles of 1 min. The proposed method provided recoveries from 76 to 98%, relative standard deviations under 11% (operating under reproducibility conditions) and quantification limits from 1 to 4 ng/g. The analysis of dust samples from private houses and office buildings confirmed the ubiquitous presence of target bacteriocides in these environments. PMID:17585923

  20. Feed additives diclazuril and nicarbazin in egg and liver samples from Croatian farms.

    PubMed

    Bilandžić, Nina; Dolenc, Jožica; Gačnik, Ksenija Šinigoj; Varenina, Ivana; Kolanović, Božica Solomun

    2013-01-01

    In total 307 egg and 275 liver samples were examined for nicarbazin and 365 eggs for diclazuril over a 30-month period. Enzyme-linked immunosorbent assay methods used for quantification were validated according to European Commission Decision 2002/657/EC. Non-compliant samples were confirmed by LC-MS/MS. Mean diclazuril concentrations in egg samples were 0.31 µg kg⁻¹, which is below the MRL. In only one egg sample, 2.26 µg kg⁻¹ was determined by enzyme-linked immunosorbent assay, although confirmation by LC-MS/MS gave a value of 1.6 µg kg(-1). Mean nicarbazin levels determined were 1.85 µg kg⁻¹ in egg and 21.1 µg kg⁻¹ in liver samples. Four samples, one egg and three livers, yielded elevated concentrations of nicarbazin, but only in the egg sample the LC-MS/MS method confirmed nicarbazin (106 µg kg⁻¹) above the MRL value. PMID:24779872

  1. 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 ...

  2. 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. PMID:25746759

  3. 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

    2014-10-01

    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. PMID:25083511

  4. WashWise cleans up the Northwest: Lessons learned from the Northwest high-efficiency clothes washer initiative

    SciTech Connect

    Gordon, L.M.; Banks, D.L.; Brenneke, M.E.

    1998-07-01

    WashWise is a regional market transformation program designed to promote the sale and acceptance or resource-efficient clothes washers (RECWs) in the Northwest through financial incentives, education, and marketing. The Program is sponsored by the Northwest Energy Efficiency Alliance (the Alliance), a non-profit regional consortium of utilities, government, public interest groups, and private sector organizations. WashWise started in May 1997 and will continue through the end of 1999. WashWise works to transform the clothes washer market primarily at the retail level through an in-store instant rebate and a retailer bonus. In addition to financial incentives, WashWise has undertaken a collaborative marketing and promotional campaign to educate consumers about the financial savings and other benefits of RECWs. The program promotes only RECWs that meet strict energy and water savings criteria. WashWise has far exceeded initial expectations; annual program sales goals were met in the first three months. As of June 1998, 30,000 RECWs have been sold through the program (representing approximately 13 percent of the Northwest residential clothes washer market). In addition, over 540 retailers, including national and regional chains, are participating in the program. Preliminary survey results also have also provided evidence of broad customer satisfaction. This paper reviews the key elements that have contributed to the success of the WashWise program. In addition, the paper provides program results and indicates future directions for WashWise and the RECW market.

  5. 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.

  6. 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. PMID:26342308

  7. Determination of acrylamide in coffee and coffee products by GC-MS using an improved SPE clean-up.

    PubMed

    Soares, C; Cunha, S; Fernandes, J

    2006-12-01

    An improved gas chromatography-mass spectrometry (GC-MS) method to determine acrylamide (AA) in coffee and coffee products was developed. The method was based on two main purification steps: the first with ethanol and Carrez solutions in order to precipitate polysaccharides and proteins, respectively; and the second with a layered solid-phase extraction (SPE) column which proved to be efficient in the elimination of the main chromatographic interferences. The method is applicable to a wide range of coffee products. Twenty-six samples of different coffee products were analysed. The levels of AA were in the range 11.4-36.2 microg l-1 for 'espresso coffee' and 200.8-229.4 microg l-1 for coffee blends with cereals. The results indicate that the presence of cereals significantly increased the levels of AA. PMID:17118870

  8. 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. PMID:23535744

  9. 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%. PMID:22007890

  10. [Determination of organic phosphorus pesticide residues in scallion by gas chromatography coupled with microwave clean-up].

    PubMed

    Jiang, Jun; Li, An; Li, Haiyan; Tong, Kexing; Zhou, Lili; Zhou, Huimin; Zhao, Tong

    2007-05-01

    A method for the determination of organic phosphorus pesticide residues is described. It covers 25 residues in scallion including dichlorvos, ethoprophos, phorate, diazinon, disulfoton, dimethoate, pirimiphos-methyl, chlorpyrifos, malathion, fenitrothion, parathion, chlorfenvinphos, ethion, EPN, dyfonate, chlorpyrifos-methyl, parathion-methyl, fenthion, quinalphos, gardona, methidathion, carbophenothion, phosmet, phosalone, and coumaphos. After the scallion samples were heated for 30 s in microwave oven, the residues were extracted with acetonitrile, and then the organic phase was salted out from the matrix. As a result, most of the interfering impurities were abolished in the heating process. In this study, these pesticides were categorized into two groups for analysis. The gas chromatographic analysis was performed on a capillary column (DB-1701, 30 m x 0.25 mm x 0.25 microm) and determined with a flame photometric detector. Linear correlation coefficients of the 25 organic phosphorus pesticides were not lower than 0.991 0 and the linear ranges for most of the compounds were between 0.1 to 5.0 mg/L. The detection limits were between 0.025 and 0.200 mg/L. In recovery study, average recoveries ranged from 85.2% to 119.6% at the fortification levels of 0.05, 0.2 and 0.5 mg/kg and the relative standard deviations were in the range of 2.1% and 14.8%. The method is a simple, rapid and highly efficient one to determine organic phosphorus pesticide residues in scallion. PMID:17679438

  11. The CERN antiproton source: Controls aspects of the additional collector ring and fast sampling devices

    NASA Astrophysics Data System (ADS)

    Chohan, V.

    1990-08-01

    The upgrade of the CERN antiproton source, meant to gain an order of magnitude in antiproton flux, required the construction of an additional ring to complement the existing antiproton accumulator (AA) and an entire rebuild of the target zone. The AA also needed major modifications to handle the increased flux and perform purely as an accumulator, preceded by collection in the collector ring (AC). The upgrade, known as the ACOL (antiproton collector) project, was approved under strict time and budgetary constraints and the existing AA control system, based on the Proton Synchrotron (PS) Divisional norms of CAMAC and Norsk-Data computers, had to be extended in the light of this. The limited (9 months) installation period for the whole upgrade meant that substantial preparatory and planning activities had to be carried out during the normal running of the AA. Advantage was taken of the upgrade to improve and consolidate the AA. Some aspects of the control system related to this upgrade are discussed together with the integration of new applications and instrumentation. The overall machine installation and running-in was carried out within the defined milestones and the project has now achieved the physics design goals.

  12. A new solid phase extraction clean-up method for the determination of 12 type A and B trichothecenes in cereals and cereal-based food by LC-MS/MS.

    PubMed

    Klötzel, Marianna; Lauber, Uwe; Humpf, Hans-Ulrich

    2006-03-01

    A new reliable and cost-efficient solid phase extraction-based clean-up method for the determination of 12 type A and B trichothecenes [deoxynivalenol (DON), nivalenol, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, fusarenon-X, T-2 toxin, HT-2 toxin, neosolaniol, monoacetoxy-scirpenol, diacetoxyscirpenol, T-2 triol and T-2 tetraol] in cereals and cereal-based food is presented. Furthermore, the suitability for the simultaneous determination of zearalenone is examined. Toxins were extracted from cereal samples using ACN/water (80/20, v/v), purified by means of a new Bond Elut Mycotoxin column and analyzed via liquid chromatography-electrospray ionization tandem mass spectrometry. Limits of detection were calculated for the matrix wheat and ranged from 0.3 to 5 ng/g, depending on the toxin. Average recovery rates for the tested compounds in seven cereal-based matrices have been determined ranging from 65 to 104%. The relative standard deviations of the complete method ranged from 2.67 (DON, wheat) to 20.0% (T-2 toxin, oats). PMID:16521159

  13. Apparatus for direct addition of reagents into a nuclear magnetic resonance (NMR) sample in the NMR probe

    NASA Astrophysics Data System (ADS)

    Perrin, Charles L.; Rivero, Ignacio A.

    1999-04-01

    Nuclear magnetic resonance (NMR) is a widely used tool in chemistry and biochemistry. It is occasionally necessary to add small aliquots of solvents or reagents repeatedly into the NMR tube. Ordinarily this is accomplished only by ejecting the sample and carrying out the addition outside the probe. It would be preferable to add the aliquot directly into the sample. We have designed and implemented a delivery system to accomplish this. This apparatus is particularly applicable to a recent NMR titration method for measuring relative pK's and to experiments where temperature must also be varied. This apparatus provides a safe, simple, and inexpensive method for repeated aliquot addition directly into the sample in the NMR probe.

  14. Metalworkers clean up their waste

    SciTech Connect

    Valenti, M.

    1994-10-01

    This article describes how using methods such as chemical precipitation, filtration, and ion exchange, metal parts manufacturers are reducing the pollutants in their wastewater so it can be reused or safely discharged. Metalworking manufacturer are recovering useful materials, lowering their disposal costs, and reducing pollution by treating their wastewater with methods such as chemical precipitation and ion exchange so that it can be reused or safely discharged. They are also reducing wastes by recycling metalworking coolants. The major wastewater treatment technologies identified by the Environmental Protection Agency are chemical precipitation, or adding flocculants to bind waste particles together; membrane ultrafiltration and reverse osmosis, in which waste is trapped when the water passes through a membrane; and ion exchange, in which specially formulated resins capture dissolved metal salts. Other treatment techniques cited by Elwood Forsht, chief of the chemicals and metals branch at the EPA, include electrowinning, which uses electrolysis to concentrate metallic ions in wastewater, and coolant recycling, a method that removes metal particles by centrifugal force and kills bacteria by pasteurization. Many metalworking operations create wastewater, including drilling, welding, soldering, surface finishing, electroplating, acid treatment, anodizing, assembly, and machining. Companies use wastewater treatment technologies to recycle their wastewater or clean it so that it meets EPA standards and can be discharged into a municipal waste system, thus avoiding high disposal costs.

  15. 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

  16. 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. PMID:26922461

  17. 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.

  18. High-performance liquid chromatographic method for the determination of the anthelmintic nitroxynil in cattle muscle tissue with on-line anion-exchange clean-up.

    PubMed

    Tarbin, J A; Shearer, G

    1993-04-01

    A high-performance liquid chromatographic method for the determination of the anthelmintic nitroxynil has been developed. The drug was extracted from cattle muscle tissue with 1% triethylamine in acetonitrile. The extract was evaporated to dryness and taken up in 0.1 M ammonium acetate-acetonitrile (50:50, v/v). The extract was then injected onto a polymeric anion-exchange precolumn. After clean-up with 0.1 M ammonium acetate-acetonitrile (50:50, v/v) for 5 min, the precolumn was eluted with 1% aqueous trifluoroacetic acid-acetonitrile (50:50, v/v) onto a PLRP-S polymer column and chromatographed with a mobile phase of 0.01 M phosphate pH 7-acetonitrile (80:20, v/v). Detection was by ultraviolet at 273 nm. Average recoveries at four levels from 0.005 to 1.000 mg kg-1 were > 88%. The limit of determination was 0.005 mg kg-1. PMID:8491824

  19. 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. PMID:27260437

  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. Gasoline additives, emissions, and performance

    SciTech Connect

    1995-12-31

    The papers included in this publication deal with the influence of fuel, additive, and hardware changes on a variety of vehicle performance characteristics. Advanced techniques for measuring these performance parameters are also described. Contents include: Fleet test evaluation of gasoline additives for intake valve and combustion chamber deposit clean up; A technique for evaluating octane requirement additives in modern engines on dynamometer test stands; A fleet test of two additive technologies comparing their effects on tailpipe emissions; Investigation into the vehicle exhaust emissions of high percentage ethanol blends; Variability in hydrocarbon speciation measurements at low emission (ULEV) levels; and more.

  2. Method validation for aflatoxin M1 determination in yoghurt using immunoaffinity column clean-up prior to high-performance liquid chromatography.

    PubMed

    Tabari, Mahsa; Karim, Guity; Ghavami, Mehrdad; Chamani, Mohammad

    2011-08-01

    Yoghurt is a popular dairy product in Iran because of its beneficial influence on human health and nutritional value. Aflatoxin M1 (AFM1) is the metabolite of potential carcinogen aflatoxin B1, which can contaminate milk through the feed and is not eliminated by common processing heat treatment. An analytical method using immunoaffinity column for extraction and a high-performance liquid chromatography (HPLC) for quantification was developed for AFM1 in this study. An HPLC method with fluorimetric detection for the determination of AFM1 in yoghurt milk has been optimized and validated according to Commission Decision BS EN ISO 14501: 2007 by using the conventional validation approach. The procedure for determining selectivity, recovery, precision, decision limit (CCα) and detection capability (CCβ) of the method has been reported. The results of the validation process demonstrate the agreement of the method with the provisions of Commission Regulation 401: 2006:EC. A new HPLC method with fluorescence detection was developed to determine aflatoxin M1. The detection limit was 1 ng/kg for yoghurt. The calibration curve was linear from 0.1 to 3.0 μg l⁻¹ injected. The method includes a preliminary clean-up and the average recoveries determined on three different days at the concentration levels of 0.025, 0.050 and 0.075 μg kg⁻¹ were in the range of 72.57%-86.66% with RSD in the range of 2.56%-8.41%. The interday and interlevel mean recovery value, which has been used to correct routine analysis results, was 80%. The method is rapid, easily automatable and therefore useful for accurate and precise screening of aflatoxin M1 in yoghurt. PMID:21385770

  3. 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

  4. Development of a liquid chromatography-tandem mass spectrometry with ultrasound-assisted extraction and auto solid-phase clean-up method for the determination of Fusarium toxins in animal derived foods.

    PubMed

    Chen, Dongmei; Cao, Xiaoqin; Tao, Yanfei; Wu, Qinghua; Pan, Yuanhu; Peng, Dapeng; Liu, Zhenli; Huang, Lingli; Wang, Yulian; Wang, Xu; Yuan, Zonghui

    2013-10-11

    A liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the simultaneous determination of 19 Fusarium toxins and their metabolites including deoxynivalenol (DON), nivalenol (NIV), T-2 toxin (T-2), HT-2 toxin (HT-2), 3-acetyldeoxynivalenol (3-AcDON), 15-acetyldeoxynivalenol (15-AcDON), neosolaniol (NEO), fusarenon-X (F-X), diacetoxyscirpenol (DAS), monoacetoxyscirpenol (MAS), zearalanone (ZAN), zearalenone (ZON), α-Zearalenol (α-ZOL), β-Zearalenol (β-ZOL), a-Zearalanol (α-ZAL), β-Zearalanol (β-ZAL), T-2 triol, T-2 tetraol, deepoxy-deoxynialenol (DOM-1) in the muscle, liver, kidney, fat of swine, bovine and sheep, muscle and liver of chicken, muscle and skin of fish, as well as milk and eggs. Sample preparation procedure includes ultrasound-assisted extraction with acetonitrile/water (90/10, v/v), defatting with n-hexane and final clean-up with auto solid phase extraction (SPE) on Bond Elut Mycotoxin cartridges. The detection and quantification of the analytes were performed by a reversed-phase liquid chromatography coupled with electrospray ionization triple quadrupole mass spectrometry (LC/ESI-MS/MS). DON, NIV, DOM-1, 3-AcDON, 15-AcDON, F-X, ZON, ZAN, α-ZOL, β-ZOL, α-ZAL, β-ZAL, T-2 triol and T-2 tetraol were detected in a negative ion mode, while T-2 toxin, HT-2 toxin, NEO, DAS and MAS were detected in a positive ion mode. The CCα and CCβ of the analytes in different samples varied from 0.16 to 1.37μg/kg and 0.33 to 2.34μg/kg, respectively. The recoveries of spiked sample from 0.5μg/kg to 8μg/kg ranged from 64.8% to 108.2% with the relative standard deviations of less than 19.4%. Performances of the whole analytical procedure meet the criteria established by the European Commission for mass spectrometric detection. PMID:24011505

  5. Adsorption of peptides at the sample drying step: influence of solvent evaporation technique, vial material and solution additive.

    PubMed

    Pezeshki, Adel; Vergote, Valentijn; Van Dorpe, Sylvia; Baert, Bram; Burvenich, Christian; Popkov, Alexander; De Spiegeleer, Bart

    2009-04-01

    Although the efficient and careful removal of solvent from samples by centrifugal evaporation or freeze-drying methods is an important step in peptidomics, the recovery of peptides has not yet been fully investigated with these sample drying methods. Moreover, the surface adsorption of the peptides by the container and efforts to reduce this adsorption by organic additives is only scarcely elaborated until now. In this experiment, the recovery of five model peptides, i.e. bovine insulin, mouse obestatin, goserelin, buserelin and leucine-enkephalin was investigated applying dimethylsulfoxide (DMSO), dimethylformamide (DMF), polyethylene glycol 400 (PEG 400), mannitol and n-nonyl-beta-d-glucopyranoside (C(9)-Glu) in function of the two applied solvent evaporation processes (freeze-drying vs. centrifugal evaporation) and vial types, i.e. polypropylene (PP) and glass. Under our experimental conditions, drying resulted in a decreased recovery of the model peptides by 10% on average. Insulin showed the lowest recovery value relative to the other model peptides. For both drying methods, recovery of the model peptides was increased when C(9)-Glu was present. Overall, the use of PP vials is proposed for freeze-drying, while glass vials are found to be more suitable for centrifugal evaporation. The presence of PEG 400 in PP vials caused significantly reduced recoveries for all model peptides using centrifugal evaporation, although this was not observed in glass vials. As a general conclusion, applying C(9)-Glu as an additive along with choosing appropriate vial type (i.e. PP for lyophilization and glass for centrifugal evaporation) can avoid or diminish peptide loss during the evaporation procedure. PMID:19150589

  6. 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

  7. 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. PMID:25812798

  8. Ionic liquids as mobile phase additives for the high-performance liquid chromatographic analysis of fluoroquinolone antibiotics in water samples.

    PubMed

    Herrera-Herrera, Antonio V; Hernández-Borges, Javier; Rodríguez-Delgado, Miguel Angel

    2008-12-01

    In this work, four ionic liquids differing in the length of the alkyl chain on the imidazolium cation and one ionic liquid containing tetraethylammonium, all with the same counterion, (i.e. 1-ethyl-3-methylimidazolium tetrafluoroborate (EMIm-BF(4)), 1-butyl-3-methylimidazolium tetrafluoroborate (BMIm-BF(4)), 1-hexyl-3-methylimidazolium tetrafluoroborate (HMIm-BF(4)), 1-methyl-3-octylimidazolium tetrafluoroborate (MOIm-BF(4)), and tetraethylammonium tetrafluroborate (Et(4)N-BF(4))) were tested as mobile phase additives for HPLC separation of a group of seven basic fluoroquinolone (FQ) antibiotics for human and veterinary use (i.e. fleroxacin, ciprofloxacin, lomefloxacin, danofloxacin, enrofloxacin, sarafloxacin, and difloxacin) using a conventional reversed-phase Nova-Pak C(18) column. Fluorescence detection was used. Among the ionic liquids selected, use of BMIm-BF(4) enabled effective separation of these compounds with relatively low analysis time (14 min). The best separation was achieved by isocratic elution at 1 mL min(-1) with 5 mmol L(-1) BMIm-BF(4) and 10 mmol L(-1) ammonium acetate at pH 3.0 with 13% (v/v) acetonitrile. Limits of detection (LODs) for fluorescence detection were in the range 0.5-11 microg L(-1). The method was tested by analyzing several water samples after the optimization of a suitable solid-phase extraction (SPE) procedure using Oasis HLB cartridges. Mean recovery values were above 84% for all analytes with LODs in the range 1-29 ng L(-1). PMID:18854988

  9. 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 ...

  10. 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. PMID:24636559

  11. Solid sampling determination of lithium and sodium additives in microsamples of yttrium oxyorthosilicate by high-resolution continuum source graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Laczai, Nikoletta; Kovács, László; Péter, Ágnes; Bencs, László

    2016-03-01

    Solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (SS-HR-CS-GFAAS) methods were developed and studied for the fast and sensitive quantitation of Li and Na additives in microsamples of cerium-doped yttrium oxyorthosilicate (Y2SiO5:Ce) scintillator materials. The methods were optimized for solid samples by studying a set of GFAAS conditions (i.e., the sample mass, sensitivity of the analytical lines, and graphite furnace heating programs). Powdered samples in the mass range of 0.099-0.422 mg were dispensed onto graphite sample insertion boats, weighed and analyzed. Pyrolysis and atomization temperatures were optimized by the use of single-element standard solutions of Li and Na (acidified with 0.144 mol/L HNO3) at the Li I 610.353 nm and Na I 285.3013 nm analytical lines. For calibration purposes, the method of standard addition with Li and Na solutions was applied. The correlation coefficients (R values) of the calibration graphs were not worse than 0.9678. The limit of detection for oxyorthosilicate samples was 20 μg/g and 80 μg/g for Li and Na, respectively. The alkaline content of the solid samples were found to be in the range of 0.89 and 8.4 mg/g, respectively. The accuracy of the results was verified by means of analyzing certified reference samples, using methods of standard (solution) addition calibration.

  12. 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. PMID:19082516

  13. 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.

    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. 

  14. 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. PMID:27004927

  15. Determination of benazolin-ethyl residues in soil and rape seed by SPE clean-up and GC with electron capture detection.

    PubMed

    Liu, Xiaolu; Yang, Tao; Hu, Jiye

    2013-01-01

    A method has been developed and established for residue determination of benazolin-ethyl in soil and rape seed samples by gas chromatography with electron capture detection (GC-ECD). Limits of quantification of the method are 0.005 mg/kg for both soil and rape seed, which are sufficiently below the maximum residue limit, and the limit of detection is 0.0023 ng. The average recoveries of the analyte range from 85.89 to 105.84% with relative standard deviations (coefficient of variation) less than 5.53% at the three spike levels (0.005, 0.1 and 0.5 mg/kg). The half-life of benazolin-ethyl in soil from the experimental field is 4.62 days. The final residues of benazolin-ethyl in soil and rape seed samples are lower than 0.005 mg/kg at harvest time. Direct confirmation of the analyte in real samples is achieved by GC-mass spectrometry. It is demonstrated that the proposed method is simple, rapid and efficient, and reliable to detect benazolin-ethyl residues in soil and rape seed samples. PMID:22718745

  16. Simultaneous determination of 14 oil-soluble synthetic dyes in chilli products by high performance liquid chromatography with a gel permeation chromatography clean-up procedure.

    PubMed

    Zhu, Yonghong; Zhao, Bo; Xiao, Ruiqi; Yun, Wen; Xiao, Zhaojing; Tu, Dawei; Chen, Shiqi

    2014-02-15

    A method was developed for the simultaneous determination of 14 fat-soluble dyes in chilli products. The samples were extracted with hexane/acetone. The cleanup was performed with gel permeation chromatography (GPC) cleanup system. A HPLC separation was performed using variable wavelength detector and a gradient elution with 0.1% formic acid and methanol-acetonitrile (1:1, v/v) as the mobile phases. Good linearity (R² ≥ 0.995) was observed between 0.1 and 5.0 μg/mL. Detection limits of the investigated dyes, which were evaluated at signal to noise ratio of 3, were in the ranges of 11-71 μg/kg. The recoveries of the 14 synthetic colourants in three matrices ranged from 73.4% to 103.5%. Relative standard deviations ranged from 3.7% to 12.3%. The method has been successfully used for the determination of banned dyes in real samples. PMID:24128569

  17. Preparation of molecularly imprinted solid phase extraction using bensulfuron-methyl imprinted polymer and clean-up for the sulfonylurea-herbicides in soybean.

    PubMed

    Tang, Kaijie; Chen, Shangwei; Gu, Xiaohong; Wang, Haijun; Dai, Jun; Tang, Jian

    2008-04-28

    A pre-treatment methodology based on the molecularly imprinted solid phase extraction (MI-SPE) procedure was developed for the determination of bensulfuron-methyl (BSM), tribenuron-methyl (TBM), metsulfuron-methyl (MSM) and nicosulfuron (NS) in soybean samples. A molecular imprinted polymer (MIP) was prepared by precipitation polymerization using BSM as the template molecule, alpha-methacrylic acid (MAA) as the functional monomer, trimethylolpropane trimethacrylate (TRIM) as the cross-linker and dichloromethane as the porogen. The binding behaviors of the template BSM and its analogues on the MIP were evaluated by high performance liquid chromatography (HPLC). Then, solid phase extraction (SPE) with a BSM molecularly imprinted polymer (BSM-MIP) as adsorbent was investigated and the optimum loading, washing, and eluting conditions for MI-SPE of the selected BSM, MSM, TBM, and NS were established. The optimized MI-SPE procedure was used to extract the sulfonylureas and a high recovery was obtained in the soybean samples. PMID:18405688

  18. 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.

  19. 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

  20. 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. PMID:23442715

  1. 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 Central

    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 (r2 = 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. PMID:25873969

  2. 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.

  3. Selective clean-up applicable to aqueous acetone extracts for the determination of carbendazim and thiabendazole in fruits and vegetables by high-performance liquid chromatography with UV detection.

    PubMed

    Di Muccio, A; Girolimetti, S; Attard Barbini, D; Pelosi, P; Generali, T; Vergori, L; De Merulis, G; Leonelli, A; Stefanelli, P

    1999-02-12

    Fungicide residues in vegetables (benomyl, carbendazim, thiabendazole) are analyzed through a clean-up procedure that uses a portion of the aqueous acetone extract prepared for multiresidue methodology. A portion of the aqueous acetone extract (equivalent to 5 g of vegetables) is loaded onto an Extrelut-20 cartridge (the cartridge is filled with a coarse, large-pore diatomaceous material). Then, acetone is partially removed by an upward stream of nitrogen at 2l/min for 30 min. Benzimidazolic fungicides are recovered by percolating the cartridge with 100 ml of 0.1 M phosphoric acid solution, which also serves to convert benomyl to carbendazim. The percolating acid solution is drained on-line through a strong cation-exchange (SCX) solid-phase extraction cartridge with the aid of a slight vacuum. Benzimidazolic fungicides are retained on the SCX cartridge. The phosphoric acid solution is discarded together with the washings of the SCX cartridge, i.e., water followed by methanol-water (75:25), that remove unwanted coextractives. Finally, benzimidazolic fungicides are recovered by eluting the SCX cartridge with methanol-ammonium formate buffer (75:25). The final extract is then analyzed by reversed-phase HPLC with UV detection. Recoveries from crops such as apples, lettuce, strawberries and citrus fruits are generally greater than 80% and no interferences were observed. The clean-up is simple and straightforward, requires only disposable items, water solutions and a few milliliters of solvent and a minimum number of manipulations, and does not require concentration steps or electrical equipment. PMID:10074700

  4. Application of State and Federal Guidelines for Establishing Alternate Soil Clean-Up Levels for the Protection of Groundwater at the Hanford Site

    SciTech Connect

    Leary, K.; McMahon, W.; Hoover, J.

    2008-07-01

    Risk-based soil cleanup levels that are protective of groundwater have been calculated for use in environmental remediation activities at the Hanford Site using vadose zone fate and transport modeling. The determination of soil cleanup levels is important because it involves the technical basis for the levels of contamination that can be left in place, which are protective of human health and the environment. The determination of risk-based soil cleanup levels is an especially important issue at the Hanford Site where site conditions such as a semi-arid climate, and a thick vadose zone of over 100 meters necessitate the use of appropriate risk-based methods. In the absence of an alternative risk-based approach, the cleanup levels default to background, detection limits, or simplistic formulas not intended for applications involving these distinctive site conditions. However, the use of vadose zone fate and transport modeling for risk-based applications such as the determination of soil cleanup levels in the vadose zone are not as well established as modeling for groundwater applications. Thus, the use of models in this manner involves additional challenges for the demonstration of the efficacy of its use for risk-based applications, in accordance with federal and state regulatory requirements and guidelines. An approach has been developed to integrate with federal and state regulatory guidelines in conjunction with the development of the risk-based methodology. Demonstration of integration with these guidelines primarily involves documentation of the objectives of the problem to be solved, the technical basis and rationale associated with the selection of an appropriate risk-based method (e.g., model type and code selection), and documentation associated with the use of the model, e.g., conceptual site model, parameter estimation, uncertainty and assumptions analyses, and model results. (authors)

  5. 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). PMID:25748540

  6. 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.

  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. 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)

  10. 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.

  11. 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…

  12. Cleaning up the customer satisfaction waste dump

    SciTech Connect

    Plunkett, C.; Katz, G.M.

    1994-11-01

    Most electric utilities have been measuring Customer Satisfaction for several years now with the explicit goal of inducing their employees to improve their handling of customers. While many companies experienced early improvements, the scores have now leveled off. Increasingly, utilities are finding that their Customer Satisfaction Measurement system has reverted to little more than a {open_quotes}report card,{close_quotes} with no clear connection to business practice or processes. Even more alarming is the fact that many companies are now questioning the value of this complicated and expensive effort. This phenomenon is not unique to the electric utility industry -- it is happening in almost every industry in America. What companies really need is a way to tie customer satisfaction to business practices. To accomplish this, the Southern Company, along with several other utilities, are using the Voice of the Customer Process, which came out of the Japanese auto industry. It combines Customer Satisfaction Measurement with Quality Function Deployment (QFD) in order to guide the company into linking specific customer wants and needs to explicit performance measures and business process improvement efforts.

  13. Research on Cleaning Up in San Diego.

    ERIC Educational Resources Information Center

    Middleman, Stanley

    1983-01-01

    Discusses the evolution of a set of research programs (dealing with the removal of liquid contaminants from surfaces) used to introduce graduate students to methods of design, evaluation, and modification within the context of a larger research program. Stresses the simultaneity and interaction of theoretical and experimental studies. (JM)

  14. 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. PMID:25797504

  15. PBDEs in environmental samples: sampling and analysis.

    PubMed

    Król, Sylwia; Zabiegała, Bożena; Namieśnik, Jacek

    2012-05-15

    The paper reviews the subject literature concerning analytical procedures routinely sed for monitoring polybrominated diphenyl ethers (PBDE) in environmental samples. It describes and summarizes subsequent stages of analytical procedure including sample collection and preparation, extraction, clean-up and final determination. Different approaches with their advantages and limitations are presented. Special attention is drawn to the newly developed, promising extraction techniques, especially: liquid-liquid-microextraction (LLME) with its modifications, cloud point extraction (CPE) and hollow fiber microextraction. The review compares available detection techniques taking into account their usefulness for determining different PBDEs in complex matrix as well as discussing possible limitations that may occur during the analysis. The quality assurance and quality control aspect of analytical procedure is described. Finally special attention is paid to the determination of highly brominated PBDE compounds (e.g. BDE209), which requires implementation of different analytical approach. PMID:22483870

  16. Restricted access chiral stationary phase synthesized via reversible addition-fragmentation chain-transfer polymerization for direct analysis of biological samples by high performance liquid chromatography.

    PubMed

    Song, Wen-Jun; Wei, Ji-Ping; Wang, Su-Ying; Wang, Huai-Song

    2014-06-17

    Novel hydrophilic microparticles containing β-cyclodextrin (β-CD) were prepared via one-pot synthesis using reversible addition-fragmentation chain-transfer (RAFT) precipitation polymerization, a "controlled/living" radical polymerization technique. The polymerization was initiated by hydrophilic macromolecular chain-transfer agent [poly(2-hydroxyethyl methacrylate), PHEMA]. The hydrophilic PHEMA on the surface of microparticles can well improve their surface hydrophilicity and lead to their biological compatibility. As chiral restricted access material (RAM), the hydrophilic microparticles can be used for determination of enantiomers in biological samples with direct injection via HPLC analysis. PMID:24890695

  17. 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

  18. 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. PMID:23843996

  19. Effect of additional sample bias in Meshed Plasma Immersion Ion Deposition (MPIID) on microstructural, surface and mechanical properties of Si-DLC films

    NASA Astrophysics Data System (ADS)

    Wu, Mingzhong; Tian, Xiubo; Li, Muqin; Gong, Chunzhi; Wei, Ronghua

    2016-07-01

    Meshed Plasma Immersion Ion Deposition (MPIID) using cage-like hollow cathode discharge is a modified process of conventional PIID, but it allows the deposition of thick diamond-like carbon (DLC) films (up to 50 μm) at a high deposition rate (up to 6.5 μm/h). To further improve the DLC film properties, a new approach to the MPIID process is proposed, in which the energy of ions incident to the sample surface can be independently controlled by an additional voltage applied between the samples and the metal meshed cage. In this study, the meshed cage was biased with a pulsed DC power supply at -1350 V peak voltage for the plasma generation, while the samples inside the cage were biased with a DC voltage from 0 V to -500 V with respect to the cage to study its effect. Si-DLC films were synthesized with a mixture of Ar, C2H2 and tetramethylsilane (TMS). After the depositions, scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectrons spectroscopy (XPS), Raman spectroscopy and nanoindentation were used to study the morphology, surface roughness, chemical bonding and structure, and the surface hardness as well as the modulus of elasticity of the Si-DLC films. It was observed that the intense ion bombardment significantly densified the films, reduced the surface roughness, reduced the H and Si contents, and increased the nanohardness (H) and modulus of elasticity (E), whereas the deposition rate decreased slightly. Using the H and E data, high values of H3/E2 and H/E were obtained on the biased films, indicating the potential excellent mechanical and tribological properties of the films. In this paper, the effects of the sample bias voltage on the film properties are discussed in detail and the optimal bias voltage is presented.

  20. Analytical techniques for the detection and identification of chemical warfare materials from environmental samples

    SciTech Connect

    Beaudry, W.T.; Weimaster, J.F.

    1995-06-01

    The detection and identification of chemical warfare (CW) material in diverse and complex matrices has become increasingly important to support the environmental clean-up of military and industrial sites that were historically used in the research, production, use, storage and/or demilitarization of chemical weapons. Reliable and defensible identification of hazardous materials (HM) is necessary to comply with the increasingly stringent regulations imposed by local, state, and federal agencies which govern handling, treatment, storage, and disposal of HM. In addition, before sites can be reutilized, existing HM must be properly identified so that the proper methods of removal, treatment and disposal can be determined. An overview of sample preparation and analytical techniques for the detection and identification of CW materials is presented in this paper.

  1. Improved method for the simultaneous determination of aflatoxins, ochratoxin A and Fusarium toxins in cereals and derived products by liquid chromatography-tandem mass spectrometry after multi-toxin immunoaffinity clean up.

    PubMed

    Lattanzio, Veronica Maria Teresa; Ciasca, Biancamaria; Powers, Stephen; Visconti, Angelo

    2014-08-01

    An improved method for the quantitative determination of aflatoxins (B1, B2, G1, G2), ochratoxin A, fumonisins (B1, B2), zearalenone, deoxynivalenol, nivalenol, T-2 and HT-2 toxins in cereals and derived products, at levels comparable with EU maximum permitted levels, was developed. The effective co-extraction of the mycotoxins under investigation was achieved in 4min by a double extraction approach, using water followed by methanol. Clean up of the extract was performed by a new multi-toxin immunoaffinity column. Analytical performance characteristics were evaluated through single laboratory validation. Raw wheat and maize, corn flakes and maize snacks were chosen as representative matrices for method validation. The validation assay was carried out at 50, 100 and 150% of EU maximum permitted levels for each mycotoxin. Statistical analysis of the results (ANOVA) provided the within laboratory reproducibility and the error contributions from repeatability, between day effects, and influences from different matrix composition. Recoveries generally higher than 70% were obtained for all tested mycotoxins with relative standard deviation (within laboratory reproducibility) lesser than 37%. Limits of quantification (calculated as the lowest amount of each analyte which could be determined with a precision of 10%) ranged from 1μg/kg to 30μg/kg. The trueness of generated data was assessed by analysis of reference materials. The proposed method was proven to be suitable to assess, with a single analysis, compliance of the selected cereal based foods with the EU maximum permitted or recommended levels for all regulated mycotoxins. PMID:24969088

  2. 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

  3. Impact of 2′-hydroxyl sampling on the conformational properties of RNA: Update of the CHARMM all-atom additive force field for RNA

    PubMed Central

    Denning, Elizabeth J.; Priyakumar, U. Deva; Nilsson, Lennart; MacKerell, Alexander D.

    2011-01-01

    Here, we present an update of the CHARMM27 all-atom additive force field for nucleic acids that improves the treatment of RNA molecules. The original CHARMM27 force field parameters exhibit enhanced Watson-Crick (WC) base pair opening which is not consistent with experiment while analysis of MD simulations show the 2′-hydroxyl moiety to almost exclusively sample the O3′ orientation. Quantum mechanical studies of RNA related model compounds indicate the energy minimum associated with the O3′ orientation to be too favorable, consistent with the MD results. Optimization of the dihedral parameters dictating the energy of the 2′-hydroxyl proton targeting the QM data yielded several parameter sets, which sample both the base and O3′ orientations of the 2′-hydroxyl to varying degrees. Selection of the final dihedral parameters was based on reproduction of hydration behavior as related to a survey of crystallographic data and better agreement with experimental NMR J-coupling values. Application of the model, designated CHARMM36, to a collection of canonical and non-canonical RNA molecules reveals overall improved agreement with a range of experimental observables as compared to CHARMM27. The results also indicate the sensitivity of the conformational heterogeneity of RNA to the orientation of the 2′-hydroxyl moiety and support a model whereby the 2′-hydroxyl can enhance the probability of conformational transitions in RNA. PMID:21469161

  4. A multigene phylogeny of the fly superfamily Asiloidea (Insecta): Taxon sampling and additional genes reveal the sister-group to all higher flies (Cyclorrhapha).

    PubMed

    Trautwein, Michelle D; Wiegmann, Brian M; Yeates, David K

    2010-09-01

    Asiloidea are a group of 9 lower brachyceran fly families, considered to be the closest relative to the large Metazoan radiation Eremoneura (Cyclorrhapha+Empidoidea). The evidence for asiloid monophyly is limited, and few characters define the relationships between the families of Asiloidea and Eremoneura. Additionally, enigmatic genera, Hilarimorpha and Apystomyia, retain morphological characters of both asiloids and higher flies. We use the nuclear protein-coding gene CAD and 28S rDNA to test the monophyly of Asiloidea and to resolve its relationship to Eremoneura. We explore the effects of taxon sampling on support values and topological stability, the resolving power of additional genes, and hypothesis testing using four-cluster likelihood mapping. We find that: (1) the 'asiloid' genus Apystomyia is sister to Cyclorrhapha, (2) the remaining asiloids are monophyletic at the exclusion of the family Bombyliidae, and (3) our best estimate of relationships places the asiloid flies excluding Bombyliidae as the sister-group to Eremoneura, though high support is lacking. PMID:20399874

  5. 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. PMID:26593531

  6. 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.

  7. 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.

  8. Non starch polysaccharide hydrolyzing enzymes as feed additives: detection of enzyme activities and problems encountered with quantitative determination in complex samples.

    PubMed

    Vahjen, W; Gläser, K; Froeck, M; Simon, O

    1997-01-01

    Chromogenic substrates, an agar diffusion assay and viscosity reduction were used to estimate beta-glucanase and xylanase activities in water soluble extracts of different feedstuffs and digesta supernatants. The dinitrosalicylic acid reducing sugar method was employed to calibrate results from different methods based on international units (IU, glucose equivalents). The detection of dye release from chromogenic substrates was a suitable method, allowing the detection of 0.05 IU of enzyme activity per ml of extract, although measurements in digesta supernatants were limited in linearity (0.1-0.5 IU/ml supernatant). With the agar diffusion assay the detection of enzyme activity was possible over a wider concentration range (extracts: 0.05-1 IU/ml, digesta supernatants: 0.1-1 IU/ml), but visual evaluation led to inaccurate measurement. Accuracy can be improved by computer based evaluation of digital images. The use of viscosity reduction produced linear standard curves from 0.01 to 0.5 IU/ml in feed extracts, but reliability of measurements depended on modification of substrates. Quantification of enzyme activities was influenced by matrix effects of complex samples. Cereal dependant differences were found in various extracts of feed mixtures and cereal extracts. Digesta supernatants partly inhibited enzyme activity, depending on the origin of the sample. Interaction of substrates with digesta components varied between methods. The sensitivity of the methods is comparable, however, all methods require specific calibrations to account for matrix- and enzyme specific effects. PMID:9345597

  9. State of the art of environmentally friendly sample preparation approaches for determination of PBDEs and metabolites in environmental and biological samples: A critical review.

    PubMed

    Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C

    2016-01-28

    Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed. PMID:26755134

  10. Nano Sized Powder Additives of SiC and Diamond to MgB2 as Artificially Inductor of Pinning Force for the Dense Samples Obtained by High Pressure Technologies

    NASA Astrophysics Data System (ADS)

    Morawski, A.; Pachla, W.; Kuzmenko, D.; Łada, T.; Zaleski, A.; Eibl, O.; Haessler, W.; Kovac, P.

    2006-09-01

    The nano-powder additives of SiC (11nm) and diamond (6 nm) were mixed with Mg and amorphous B powders in the production route of MgB2 bulk and wires samples. Special attention was paid to the precursor powders with the respect to chemical purity, grain morphology and secondary phases. Commercially available MgB2 powders (ex-situ technology) and also mixtures of MgH2 and amorphous B powders (in-situ technology) were applied as the starting precursors. Electron microscopy was used extensively for the characterization of these powders applying both SEM and TEM analysis. Superconducting bulks and wires samples have been produced, by hot pressing, hot isostatic pressing and hydrostatic extrusion processes. High grain refinement and density in the final wire samples have been achieved by the severe plastic deformation (reduction over 99.98%) with the use of the cumulative (multi-step) hydrostatic extrusion. Superconducting properties of these samples were measured, with particular attention paid to the Jc(B) characteristics. Critical currents at lower and higher magnetic fields depended sensitively on the amount of the additives and grain refinement. TEM imaging and electron spectroscopic imaging were used to evaluate the size and distribution of the both of additives within the microstructure. The strain field of the additives resulted from the misfit in thermal expansion coefficient between the additives and the MgB2 matrix was imaged in bright and dark field TEM and is particularly important for the flux-pinning properties of these materials. Influence of such synthesis parameters as pressure, temperature and time on the superconducting properties and the morphology of the products were examined and obtained results were compared. This allowed to choose the optimal conditions for the improvement of the bulk MgB2 characteristics of the wire samples.

  11. Food additives

    MedlinePlus

    Food additives are substances that become part of a food product when they are added during the processing or making of that food. "Direct" food additives are often added during processing to: Add nutrients ...

  12. 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

  13. 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. PMID:24731341

  14. 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. PMID:26212943

  15. Application of the standard addition method for the determination of acrylamide in heat-processed starchy foods by gas chromatography with electron capture detector.

    PubMed

    Zhu, Yonghong; Li, Genrong; Duan, Yunpeng; Chen, Shiqi; Zhang, Chun; Li, Yanfei

    2008-08-15

    A gas chromatography electron capture detector (GC-ECD) using the standard addition method was developed for the determination of acrylamide in heat-processed foods. The method entails extraction of acrylamide with water, filtration, defatting with n-hexane, derivatization with hydrobromic acid and saturated bromine-water, and liquid-liquid extraction with ethyl acetate. The sample pretreatment required no SPE clean-up and concentration steps prior to injection. The final extract was analyzed by GC-ECD. The chromatographic analysis was performed on polar columns, e.g. Supelcowax-10 capillary column, and good retention and peak response of the analyte were achieved under the optimal conditions. The qualification of the analyte was by identifying the peak with same retention time as standard compound 2,3-DBPA and confirmed by GC-MS. GC-MS analysis confirmed that 2,3-DBPA was converted to 2-BPA nearly completely on the polar capillary column, whether or not treated with triethylamine. A four-point standard addition protocol was used to quantify acrylamide in food samples. The limit of detection (LOD) was estimated to be 0.6μg/kg on the basis of ECD technique. Validation and quantification results demonstrated that the method should be regarded as a low-cost, convenient, and reliable alternative for conventional investigation of acrylamide. PMID:26050006

  16. Food additives.

    PubMed

    Berglund, F

    1978-01-01

    The use of additives to food fulfils many purposes, as shown by the index issued by the Codex Committee on Food Additives: Acids, bases and salts; Preservatives, Antioxidants and antioxidant synergists; Anticaking agents; Colours; Emulfifiers; Thickening agents; Flour-treatment agents; Extraction solvents; Carrier solvents; Flavours (synthetic); Flavour enhancers; Non-nutritive sweeteners; Processing aids; Enzyme preparations. Many additives occur naturally in foods, but this does not exclude toxicity at higher levels. Some food additives are nutrients, or even essential nutritents, e.g. NaCl. Examples are known of food additives causing toxicity in man even when used according to regulations, e.g. cobalt in beer. In other instances, poisoning has been due to carry-over, e.g. by nitrate in cheese whey - when used for artificial feed for infants. Poisonings also occur as the result of the permitted substance being added at too high levels, by accident or carelessness, e.g. nitrite in fish. Finally, there are examples of hypersensitivity to food additives, e.g. to tartrazine and other food colours. The toxicological evaluation, based on animal feeding studies, may be complicated by impurities, e.g. orthotoluene-sulfonamide in saccharin; by transformation or disappearance of the additive in food processing in storage, e.g. bisulfite in raisins; by reaction products with food constituents, e.g. formation of ethylurethane from diethyl pyrocarbonate; by metabolic transformation products, e.g. formation in the gut of cyclohexylamine from cyclamate. Metabolic end products may differ in experimental animals and in man: guanylic acid and inosinic acid are metabolized to allantoin in the rat but to uric acid in man. The magnitude of the safety margin in man of the Acceptable Daily Intake (ADI) is not identical to the "safety factor" used when calculating the ADI. The symptoms of Chinese Restaurant Syndrome, although not hazardous, furthermore illustrate that the whole ADI

  17. 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.

  18. Phosphazene additives

    SciTech Connect

    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.

  19. Review of sample preparation strategies for MS-based metabolomic studies in industrial biotechnology.

    PubMed

    Causon, Tim J; Hann, Stephan

    2016-09-28

    Fermentation and cell culture biotechnology in the form of so-called "cell factories" now play an increasingly significant role in production of both large (e.g. proteins, biopharmaceuticals) and small organic molecules for a wide variety of applications. However, associated metabolic engineering optimisation processes relying on genetic modification of organisms used in cell factories, or alteration of production conditions remain a challenging undertaking for improving the final yield and quality of cell factory products. In addition to genomic, transcriptomic and proteomic workflows, analytical metabolomics continues to play a critical role in studying detailed aspects of critical pathways (e.g. via targeted quantification of metabolites), identification of biosynthetic intermediates, and also for phenotype differentiation and the elucidation of previously unknown pathways (e.g. via non-targeted strategies). However, the diversity of primary and secondary metabolites and the broad concentration ranges encompassed during typical biotechnological processes means that simultaneous extraction and robust analytical determination of all parts of interest of the metabolome is effectively impossible. As the integration of metabolome data with transcriptome and proteome data is an essential goal of both targeted and non-targeted methods addressing production optimisation goals, additional sample preparation steps beyond necessary sampling, quenching and extraction protocols including clean-up, analyte enrichment, and derivatisation are important considerations for some classes of metabolites, especially those present in low concentrations or exhibiting poor stability. This contribution critically assesses the potential of current sample preparation strategies applied in metabolomic studies of industrially-relevant cell factory organisms using mass spectrometry-based platforms primarily coupled to liquid-phase sample introduction (i.e. flow injection, liquid

  20. Combining electrochemical sensors with miniaturized sample preparation for rapid detection in clinical samples.

    PubMed

    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

  1. 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

  2. Novel solid phase extraction method for the analysis of 5-nitroimidazoles and metabolites in milk samples by capillary electrophoresis.

    PubMed

    Hernández-Mesa, Maykel; García-Campaña, Ana M; Cruces-Blanco, Carmen

    2014-02-15

    A new sample treatment has been developed for the extraction of 5-nitroimidazole (5-NDZ) drugs in milk samples previous to their determination by micellar electrokinetic chromatography (MEKC). Fat removing and protein precipitation were simultaneously carried out by the addition of trichloroacetic acid (TCA) and subsequent centrifugation. Clean-up and off-line concentration were achieved by a novel solid-phase extraction (SPE) method employing mixed cation exchange (MCX) cartridges, obtaining an off-line concentration factor of 18. Analyses were performed in less than 18 min employing 20mM phosphate buffer (pH 6.5) and 150 mM SDS as background electrolyte (BGE). During the separation procedure a temperature of 20 °C and a voltage of 25 kV (normal mode) were applied. Due to sweeping effects, an on-line concentration was achieved for all the studied compounds and detection limits lower than 1.8 μg L(-1) were obtained. This method has been successfully applied to milk samples of different origins, including raw ewe milk. PMID:24128462

  3. Measurement of n-alkanals and hydroxyalkenals in biological samples.

    PubMed

    Holley, A E; Walker, M K; Cheeseman, K H; Slater, T F

    1993-09-01

    A modified method was developed to measure nM levels of a range of n-alkanals and hydroxyalkenals in biological samples such as blood plasma and tissue homogenates and also in Folch lipid extracts of these samples. Butylated hydroxytoluene (BHT) and desferrioxamine (Desferal) were added to samples to prevent artifactual peroxidation. Aldehydes were reacted with 1,3-cyclohexanedione (CHD), cleaned up by solid-phase extraction on a Sep-Pak C18 cartridge and the fluorescent decahydroacridine derivatives resolved by reverse-phase high-performance liquid chromatography (HPLC) with gradient elution. A wider range of aldehydes was detected in lipid extracts of plasma and liver homogenate compared to whole (unextracted) samples. Human plasma contained nM levels of acetaldehyde, propanal, butanal, pentanal, hexanal, and heptanal. 4-Hydroxynonenal (0.93 nmol/g) and alkanals with two to six carbons (up to 7.36 nmol/g) were detected in rat liver. Recovery of aldehydes added to whole plasma or to lipid extracts of plasma was dependent on carbon chain length, varying from 95% for acetaldehyde to 8% for decanal. Recovery from biological samples was significantly less than that of standards taken through the Sep-Pak clean-up procedure, suggesting that aldehydes can bind to plasma protein and lipid components. PMID:8406128

  4. San Diego perspective on UST clean-ups

    SciTech Connect

    Anderson, J.P.

    1996-12-31

    In June 1994, CalEPA State Water Resources Control Board (State Board) contracted with the Lawrence Livermore National Laboratory/University of California (LLNL/UC) to review the current UST regulatory framework and cleanup process. As a result of their review, LLNL/UC recommended changes to expedite the cleanup process at leaking UST sites. The LLNL/UC report concludes that natural attenuation of petroleum is an important factor in stabilizing plumes and may be the only remedial activity necessary in the absence of the source. After a review of existing literature and a study of selected leaking UST cases primarily from Coastal Range sedimentary or valley alluvium hydrogeochemical provinces, the LLNL/UC report found that petroleum plumes tend to stabilize close to the source, generally occur in shallow groundwater, and rarely impact drinking water wells in the state. The study and report recommendations focused solely on fuel petroleum hydrocarbon constituents.

  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. 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)

  7. 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.

  8. DOE and Public Involvement A Key to Successful Clean Up

    SciTech Connect

    Sarten, S.

    2008-07-01

    The combination of two vital elements in the Oak Ridge, TN area are the Department of Energy and the education of the public, at any age, of the necessary work that is and has been going on this region of the country since the setting aside of land during the World War II era. A wide variety of interested citizens from surrounding counties make up a group of individuals that bring different elements of education and involvement to form a committee of whose interest is the Department of Energy's handling of contaminated material. The effort of one of the committees on this board has given the public a resource of material to develop a better understanding of the history and stewardship efforts taking place at the Oak Ridge Reservation. (authors)

  9. 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].

  10. 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

  11. 75 FR 62923 - WRC-07 Table Clean-up Order

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-10-13

    ...This document makes non-substantive, editorial revisions to the Table of Frequency Allocations (Allocation Table), and to various other Commission rules. The purpose of this action is to update and clarify the Allocation Table, to remove obsolete and outdated provisions from the Commission's rules, and to ensure that the Allocation Table and related rules are consistent with the Commission's......

  12. 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…

  13. 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…

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

    MedlinePlus

    ... successfully trapping rodents in and around the home. Seal Up! Seal up holes inside and outside the home to ... infested areas. Before cleaning, trap the rodents and seal up any entryways to ensure that no rodents ...

  15. 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.

  16. Mercury-binding membranes for flue gas clean-up

    SciTech Connect

    Dr. Franklin O. Kroh; Thane Morgan

    2001-07-31

    All Phase I objectives were met. In the Phase I program, TPL developed a material, T- 450, capable of removing elemental mercury from air. It was found to have high porosity, good mechanical strength, good affinity for aqueous ionic mercury, and good stability to hot acidic gas. The material, used as a granular solid, was tested for adsorption of mercury in two protocols, one involving static room-temperature air and one using flowing hot air. In each case, it was superior to activated carbon. The following results were obtained: 1. Sol-gel methods were found to be applicable for synthesis of silicates containing oxidized thiol (disulfide) groups. 2. Synthetic parameters were determined for silicates with a variety of physical properties and performances. 3. Measurement of physical properties indicate high porosity strength, and stability to conditions found in flue gases. 4. The Hg° adsorption of T-450 was superior to that of activated carbon; static testing indicated a 2.4-fold increase in mercury adsorption, while a flow system mimicking hot flue gas indicated a 3.6-fold increase in Hg adsorption. 5. Economic analysis indicated that T-450 is a strong candidate for scale-up and commercial development. For the cost of removing Hg from flue gas, a savings of 23.5% is estimated, relative to use of activated carbon.

  17. GaAs clean up studied with synchrotron radiation photoemission

    NASA Astrophysics Data System (ADS)

    Tallarida, Massimo; Adelmann, Christoph; Delabie, Annelies; van Elshocht, Sven; Caymax, Matty; Schmeisser, Dieter

    2012-12-01

    In this contribution we describe the chemical changes at the surface of GaAs upon adsorption of tri-methyl-aluminum (TMA). TMA is used to grow Al2O3 with atomic layer deposition (ALD) usually using H2O as oxygen source. Recently, it was pointed out that the adsorption of TMA on various III-V surfaces reduces the native oxide, allowing the growth of an abrupt III-V/High-K interface with reduced density of defects. Synchrotron radiation photoemission spectroscopy (SR-PES) is a powerful method to characterize surfaces and interfaces of many materials, as it is capable to determine their chemical composition as well as the electronic properties. We performed in-situ SR-PES measurements after exposing a GaAs surface to TMA pulses at about 250°C. Upon using the possibility of tuning the incident photon energy we compared the Ga3d spectra at 41 eV, 71 eV, 91 eV and 121 eV, as well as the As3d at 71 eV and 91 eV. Finally, we show that using SR-PES allows a further understanding of the surface composition, which is usually not accessible with other techniques.

  18. 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.

  19. 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…

  20. 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. PMID:25706952

  1. 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.

  2. 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...

  3. 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. PMID:25872437

  4. 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. PMID:26780041

  5. 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.

  6. 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

  7. 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%.

  8. 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. PMID:18567311

  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. 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.

  11. Molecularly imprinted polymer coated solid-phase microextraction fiber prepared by surface reversible addition-fragmentation chain transfer polymerization for monitoring of Sudan dyes in chilli tomato sauce and chilli pepper samples.

    PubMed

    Hu, Xiaogang; Fan, Yanan; Zhang, Yi; Dai, Guimei; Cai, Quanling; Cao, Yujuan; Guo, Changjuan

    2012-06-20

    Surface reversible addition-fragmentation chain transfer (RAFT) polymerization method was firstly applied to the preparation of molecularly imprinted polymer (MIP) coated silicon solid-phase microextraction (SPME) fibers. With Sudan I as template, an ultra-thin MIP coating with about 0.55-μm thickness was obtained with homogeneous structure and controlled composition, due to the controllable radical growing and chain propagation in surface RAFT polymerization. The MIP-coated fibers were found with enhanced selectivity coefficients (3.0-6.5) to Sudan I-IV dyes in contrast with those reported in our previous work. Furthermore, the ultra-thin thickness of MIP coating was helpful to the effective elution of template and fast adsorption/desorption kinetics, so only about 18 min was needed for MIP-coated SPME operation. The detection limits of 21-55 ng L(-1) were achieved for four Sudan dyes, when MIP-coated SPME was coupled with liquid chromatography (LC) and mass spectrometry (MS) detection. The MIP-coated SPME-LC-MS/MS method was tested for the monitoring of ultra trace Sudan dyes in spiked chilli tomato sauce and chilli pepper samples, and high enrichment effect, remarkable matrix peaks-removing capability, and consequent high sensitivities were achieved to four Sudan dyes. PMID:22652263

  12. 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

  13. 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.

  14. Rapid determination of actinides in asphalt samples

    DOE PAGESBeta

    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

  15. Sampling and Sample Preparation

    NASA Astrophysics Data System (ADS)

    Morawicki, Rubén O.

    Quality attributes in food products, raw materials, or ingredients are measurable characteristics that need monitoring to ensure that specifications are met. Some quality attributes can be measured online by using specially designed sensors and results obtained in real time (e.g., color of vegetable oil in an oil extraction plant). However, in most cases quality attributes are measured on small portions of material that are taken periodically from continuous processes or on a certain number of small portions taken from a lot. The small portions taken for analysis are referred to as samples, and the entire lot or the entire production for a certain period of time, in the case of continuous processes, is called a population. The process of taking samples from a population is called sampling. If the procedure is done correctly, the measurable characteristics obtained for the samples become a very accurate estimation of the population.

  16. 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.

  17. Determination of aflatoxins in rice samples by ultrasound-assisted matrix solid-phase dispersion.

    PubMed

    Manoochehri, Mahboobeh; Asgharinezhad, Ali Akbar; Safaei, Mahdi

    2015-01-01

    This work describes the application of ultrasound-assisted matrix solid-phase dispersion as an extraction and sample preparation approach for aflatoxins (B1, B2, G1 and G2) and subsequent determination of them by high-performance liquid chromatography-fluorescence detection. A Box-Behnken design in combination with response surface methodology was used to determine the affecting parameters on the extraction procedure. The influence of different variables including type of dispersing phase, sample-to-dispersing phase ratio, type and quantity of clean-up phase, ultrasonication time, ultrasonication temperature, nature and volume of the elution solvent was investigated in the optimization study. C18, primary-secondary amine (PSA) and acetonitrile were selected as dispersing phase, clean-up phase and elution solvent, respectively. The obtained optimized values were sample-to-dispersing phase ratio of 1 : 1, 60 mg of PSA, 11 min ultrasonication time, 30°C ultrasonication temperature and 4 mL acetonitrile. Under the optimal conditions, the limits of detection were ranged from 0.09 to 0.14 ng g(-1) and the precisions [relative standard deviation (RSD%)] were <8.6%. The recoveries of the matrix solid-phase dispersion process ranged from 78 to 83% with RSD <10% in all cases. Finally, this method was successfully applied to the extraction of trace amounts of aflatoxins in rice samples. PMID:24771057

  18. Selective pressurized liquid extraction of polychlorinated dibenzo-p-dioxins, dibenzofurans and dioxin-like polychlorinated biphenyls from food and feed samples.

    PubMed

    Wiberg, Karin; Sporring, Sune; Haglund, Peter; Björklund, Erland

    2007-01-01

    Selective pressurized liquid extraction (PLE) of polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDD/Fs) and dioxin-like polychlorinated biphenyls (dl-PCBs) from various food and feed samples was performed with a selective PLE method previously developed for bulk PCBs. The method utilizes sulfuric acid impregnated silica inside the extraction cell to oxidize coextracted fat. Extractions were performed at 100 degrees C with n-heptane for 5 min in two cycles. Data obtained by selective PLE combined with gas chromatography/high-resolution mass spectrometry (GC-HRMS) were compared to concentrations derived from reference laboratories applying conventional sample preparation and GC-HRMS. Experiments performed on spiked vegetable oil, naturally contaminated crude fish oil and oil containing compound feed samples showed good results for these relatively simple matrices. The accuracy was generally +/-20% as compared to spiked levels or to values obtained by the reference laboratories. The precision, measured as the relative standard deviation (RSD) for 2,3,7,8-tetrachlorodibenzo-p-dioxin toxic equivalency values (TEQs), was below 10% in all cases. The method was also tested on naturally contaminated herring tissue, chicken tissue, pork tissue and sepiolitic clay, which all caused some trouble. It was observed that sufficient amounts of sodium sulfate should be used for dehydration of tissue samples and additionally, the cells should not be packed too dense in order to avoid suppressed extraction efficiency. Once this was attended to, satisfactory data could be obtained, except for sepiolithic clay. This study demonstrates that selective PLE can be applied with success to a number of food and feed matrices in analysis of PCDD/Fs and dl-PCBs. Since the fat removal step is on-line, the selective PLE method will reduce time and solvent consumption for sample preparation as compared to traditional clean-up. PMID:17109872

  19. 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). PMID:24014893

  20. 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 Central

    Yilmaz, Vedat; Arslan, Zikri; Rose, LaKeysha; Little, Maria D.

    2013-01-01

    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). PMID:24014893

  1. Multivariate optimisation of an ultrasound assisted-matrix solid-phase dispersion method combined with LC-fluorescence detection for simultaneous extraction and determination of aflatoxins in pistachio nut samples.

    PubMed

    Manoochehri, Mahboobeh; Asgharinezhad, Ali Akbar; Safaei, Mahdi

    2013-01-01

    This paper describes the application of ultrasound-assisted matrix solid-phase dispersion as an extraction and clean-up procedure for aflatoxins (B1, B2, G1 and G2) and subsequent determination by LC-fluorescence detection. A Box-Behnken design was used to determine the parameters influencing the extraction procedure through response surface methodology and experimental design. The influence of different variables including type of dispersing phase, sample-to-dispersing phase ratio, type and quantity of clean-up phase, ultrasonication time, ultrasonication temperature, nature and volume of the elution solvent were investigated in the optimisation study. C18, graphitic carbon black and acetonitrile were selected as dispersing phase, clean-up phase and elution solvent, respectively. The optimised values were sample-to-dispersing phase ratio of 1:1, 50 mg of graphitic carbon black, 11 min ultrasonication time, 30°C ultrasonication temperature and 3 ml acetonitrile. Under the optimal conditions the limits of detection (LODs) were ranged from 0.04-0.11 µg kg(-1) and the relative standard deviations (RSDs) of the extraction method were less than 8.6%. The recoveries of the matrix solid-phase dispersion process ranged from 74% to 78% with relative standard deviation lower than 9% in all cases. Finally, the matrix solid-phase dispersion was successfully applied to extraction of trace amounts of aflatoxins in pistachio samples. PMID:24053673

  2. 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.

  3. 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.

  4. Preparation of magnetic molecularly imprinted polymer for the separation of tetracycline antibiotics from egg and tissue samples.

    PubMed

    Chen, Ligang; Liu, Jun; Zeng, Qinglei; Wang, Hui; Yu, Aimin; Zhang, Hanqi; Ding, Lan

    2009-05-01

    Magnetic molecularly imprinted polymers were prepared using hydrophobic Fe(3)O(4) magnetite as the magnetically susceptible component, oxytetracycline as template molecule, methacrylic acid as functional monomer, and styrene and divinylbenzene as polymeric matrix components. The polymers were applied to the separation of tetracycline antibiotics from egg and tissue samples. The extraction and clean-up procedures were carried out in a single step by blending and stirring the sample, extraction solvent and polymers. The analytes can be transferred from the sample matrix to the polymers directly or through the extraction solvent as medium. When the extraction was complete, the polymers adsorbing the analytes were easily separated from the sample matrix by an adscititious magnet. The analytes eluted from the polymers were determined by liquid chromatography-tandem mass spectrometry. The recoveries ranging from 72.8% to 96.5% were obtained with relative standard deviations in the range of 2.9-12.3%. The limit of detection was less than 0.2 ng g(-1). The feasibility of this method was validated by analysis of incurred egg and tissue samples, and the results were compared with those obtained by the classical method in which solvent extraction, centrifugation, and subsequent clean-up and concentration by solid-phase extraction were applied. The proposed method reduced the complicacy of classical method and improved the reliability of method. PMID:19268956

  5. Generalized and rapid supramolecular solvent-based sample treatment for the determination of annatto in food.

    PubMed

    Cardeñosa, Vanessa; Lunar, María Loreto; Rubio, Soledad

    2011-12-16

    A supramolecular solvent (SUPRA) made up of octanoic acid aggregates is proposed for the microextraction of bixin and norbixin, the two major components of the natural food colouring annatto, in food. The procedure involved the extraction of sub-gram quantities (200mg) of homogenized food with 0.8mL of the supramolecular solvent. The overall sample treatment took about 20 min, and several samples could be simultaneously treated using conventional lab equipment. No clean-up or solvent evaporation were required. Extraction efficiencies mainly depended on the major components making up the SUPRAS (i.e. octanoic acid and tetrahydrofuran) and were not affected by the pH or the temperature in the ranges studied (1-4 and 10-80°C, respectively). Bixin and norbixin in the extracts were quantified by liquid chromatography (LC) and diode array detection (DAD). They were separated in a Hypersil C18 column using a mobile phase consisting of 5% acetic acid and methanol (15:85, v/v). The retention times for norbixin and bixin standards were 5.1 and 8.6 min, respectively. Recoveries in samples ranged between about 78% and 113%. The precision of the method, expressed as relative standard deviation, was about 1.5% and the quantitation limits for bixin and norbixin were 0.19 and 0.23 mg kg(-1), respectively, which were far below the maximum limits permitted by the European Union for the level of addition to food. Concentration of norbixin in samples belonging to the five major groups of food commodities defined in the literature, ranged between 3.75 and 43.8 mg kg(-1) whereas bixin was only found in one snack sample (6.6 mg kg(-1)). The method is simple and rapid, while delivering accurate and precise results, and can be used for the routine determination of annatto in food for the control of the compliance of current legislation. PMID:22071422

  6. The reaction of an iridium PNP complex with parahydrogen facilitates polarisation transfer without chemical change† †Electronic supplementary information (ESI) available: Sample preparation, signal enhancements and raw data. CCDC 1026865. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c4dt03088e Click here for additional data file. Click here for additional data file.

    PubMed Central

    Holmes, Arthur J.; Rayner, Peter J.; Cowley, Michael J.; Green, Gary G. R.; Whitwood, Adrian C.

    2015-01-01

    The short lived pincer complex [(C5H3N(CH2P(tBu)2)2)Ir(H)2(py)]BF4 is shown to be active for signal amplification by reversible exchange. This catalyst formulation enables the efficient transfer of polarization from parahydrogen to be placed into just a single molecule of the hyperpolarisation target, pyridine. When the catalysts 1H nuclei are replaced by 2H, increased levels of substrate hyperpolarization result and when the reverse situation is examined the catalyst itself is clearly visible through hyperpolarised signals. The ligand exchange pathways of [(C5H3N(CH2P(tBu)2)2)Ir(H)2(py)]BF4 that are associated with this process are shown to involve the formation of 16-electron [(C5H3N(CH2P(tBu)2)2)Ir(H)2]BF4 and the 18-electron H2 addition product [(C5H3N(CH2P(tBu)2)2)Ir(H)2(H2)]BF4. PMID:25410259

  7. Urine sample preparation of tricyclic antidepressants by means of a supported liquid membrane technique for high-performance liquid chromatographic analysis.

    PubMed

    Trocewicz, J

    2004-03-01

    Supported liquid membrane (SLM) technique for sample work-up and enrichment was used for determination of tricyclic antidepressant drugs in urine by high-performance liquid chromatography (HPLC) with UV detection. The studied antidepressant drugs were amitriptyline, opipramol, noxiptyline and additionally diethazine was used as possible internal standard. Alkaline phosphoric buffer with urine sample, as the donor solution, was passed over the liquid membrane into which investigated substances were extracted. On the other side of the membrane, analyzed compounds were trapped due to creating non-extractable form in acidic acceptor solution. Enriched and cleaned up drugs were then injected into a HPLC system with ultraviolet detection to analyze of their concentration in acceptor solution. Optimum extraction efficiency was determined by changing acceptor and donor solutions pH, application of different flow rates of donor solution and by using different solvents in the membrane. Also, donor solution volume, extraction time and concentration of analytes were varied to check the linearity of extraction process. The highest extraction efficiency: 43% for opipramol, 56% for noxiptyline, 43% for amitriptyline and 42% for diethazine (R.S.D. values were <6% and n=3) was achieved when 0.05 M phosphate buffer pH 4.0 and 9.5 were used as donor and acceptor solutions, respectively, n-undecane with 5% tri-n-octylphosphine oxide (TOPO) was used as liquid membrane. Limit of quantification (LOQ) for tricyclic antidepressants after enrichment of 100ml of urine sample was about 1 ng/ml. PMID:14751789

  8. Development and validation of an on-line multidimensional SPE-LC-MS/MS method for the quantitation of Tetrandrine in blood samples.

    PubMed

    Caglar, Sena; Morello, Rosa; Boos, Karl-Siegfried

    2015-04-15

    On-line solid-phase extraction (SPE) is becoming an increasingly widespread technique in the clean-up of complex matrices such as body fluids, prior to chromatographic analysis. The use of small SPE columns instead of disposable SPE cartridges allows multiple injections and complete automation. In addition, it decreases the cost of consumables and improves the quality of the overall analysis. Coupling of SPE with HPLC combines sample preparation and separation in one system. In this paper a validated on-line multidimensional (MD) SPE-LC-MS/MS method is described for the determination of Tetrandrine (model drug) in human blood samples. The developed method showed the applicability of direct injection of plasma samples to an on-line MD-SPE-LC-MS/MS system to determine small molecules i.e. drugs. The experimental design is unique. Quantification was through tandem mass spectrometry with positive electrospray ionization (ESI) and multiple reactions monitoring (MRM). The limit of detection was calculated as 31.98 ng/mL. The linear range of the method was between 40.0 and 800.0 ng/mL. Pharmacokinetic parameters are usually determined by analysis of drug concentrations in plasma rather than whole blood. Parameters determined using plasma data may be misleading if concentrations of drug differ between plasma and red blood cells. We successfully applied the developed method for the determination of the distribution coefficient of the model drug Tetrandrine between human red blood cells and blood plasma proteins. The determination of distribution coefficient study results demonstrated that the developed method can provide direct and accurate measurement of RBC partitioning in a model drug and could be applied for screening of other compounds for potential high RBC partition, predicting potential drug toxicity and investigating mechanisms associated with RBC partitions. PMID:25746132

  9. 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. PMID:27500642

  10. Mars sample return - Science

    NASA Technical Reports Server (NTRS)

    Blanchard, Douglas P.

    1988-01-01

    The possible scientific goals of a Mars sample return mission are reviewed, including the value of samples and the selection of sampling sites. The fundamental questions about Mars which could be studied using samples are examined, including planetary formation, differentiation, volcanism and petrogenesis, weathering, and erosion. Scenarios are presented for sample acquisition and analysis. Possible sampling methods and tools are discussed, including drilling techniques, types of rovers, and processing instruments. In addition, the possibility of aerocapture out of elliptical or circular orbit is considered.

  11. Quality control of Chinese medicinal preparations LC/ESI(+)/MS/MS analyses of saikosaponins-a and -c as markers of Bupleuri radix samples.

    PubMed

    Liau, Bing-Chung; Hsiao, Shun-Sheng; Lee, Maw-Rong; Jong, Ting-Ting; Chiang, Shu-Tuan

    2007-02-19

    We have used LC/ion trap tandem MS analysis to determine saikosaponin-a and -c as target markers in crude 70% methanol extracts from three different species of Bupleuri radix and the 10 most-popular Chinese medicinal preparations containing "Chaihu" (B. radix) without any clean-up. The optimal ionization characteristics were obtained when using positive-ion electrospray ionization (ESI) with 50 microM sodium acetate as an additive in the mobile phase. We observed good linearity over the range from 0.02 to 2 microg/ml for saikosaponin-a and from 0.02 to 1 microg/ml for saikosaponin-c. The intra-day precisions varied between 3.3 and 8.8% for saikosaponin-a and 0.3 and 11.1% for saikosaponin-c. The limits of detection were 0.01 microg/ml for both markers. The recoveries of saikosaponin-a and -c from the extract of a medicinal preparation sample (Chai-Hu-Ching-Gan-Tang, No. 13 in the table of section Analysis on actual samples) were 97 and 100%, respectively, at a 1 microg/ml spiking concentration of each marker. The highest concentrations of saikosaponin-a and -c among the three B. radixes were found in B. kaoi Liu Chao & Chuang (10.1 mg/g) and in B. falcatum (3.4 mg/g), respectively. The amounts of these saikosaponins in the 10 Chinese medicinal preparations ranged between 0.11 and 1.22 mg/g for saikosaponin-a and between 0.01 and 0.33 mg/g for saikosaponin-c. PMID:17118609

  12. [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. PMID:24772784

  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. Capillary sample

    MedlinePlus

    ... using capillary blood sampling. Disadvantages to capillary blood sampling include: Only a limited amount of blood can be drawn using this method. The procedure has some risks (see below). Capillary ...

  15. 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. PMID:26988495

  16. Evaluation of a sampling and analysis method for determination of polyhalogenated dibenzo-p-dioxins and dibenzofurans in ambient air

    SciTech Connect

    Harless, R.L.; Lewis, R.G.; McDaniel, D.D.; Gibson, J.F.; Dupuy, A.E.

    1992-01-01

    General Metals Works PS-1 PUF air samplers and an analytical method based on high resolution gas chromatography - high resolution mass spectrometry (HRGC-HRMS) were evaluated for determination of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDDs/PCDFs), polybrominated dibenz-p-dioxins and dibenzofurans (PBDDs/PBDFs) and bromo/chloro dibenzo-p-dioxins and dibenzofurans (BCDDs/BCDFs) in ambient air. Dilute solutions of these compounds and (13)C-1,2,3,4-TCDD were used to spike the filters of PS-1 air samplers which were then operated 24 hrs to sample 350-400 cubic meter ambient air. After sampling, each quartz-fiber filter and polyurethane foam (PUF) were spiked with (13)C-12-labeled PCDD, PCDF, PBDD, and PBDF internal standards before separate Soxhlet extractions with benzene. The extracts were subjected to an acid/base clean-up procedure followed by clean-up on microcolumns of silica gel, alumina, and carbon and then analyzed by HRGC-HRMS. Results derived from the study indicated the PS-1 ambient air samplers and the analytical procedures were very efficient and that pg/cubic meter and sub-pg/cubic meter levels of total PCDDs/PCDFs, PBDDs/PBDFs, BCDDs/BCDFs, and 2,3,7,8-substituted congeners could be accurately measured.

  17. Additive usage levels.

    PubMed

    Langlais, R

    1996-01-01

    With the adoption of the European Parliament and Council Directives on sweeteners, colours and miscellaneous additives the Commission is now embarking on the project of coordinating the activities of the European Union Member States in the collection of the data that are to make up the report on food additive intake requested by the European Parliament. This presentation looks at the inventory of available sources on additive use levels and concludes that for the time being national legislation is still the best source of information considering that the directives have yet to be transposed into national legislation. Furthermore, this presentation covers the correlation of the food categories as found in the additives directives with those used by national consumption surveys and finds that in a number of instances this correlation still leaves a lot to be desired. The intake of additives via food ingestion and the intake of substances which are chemically identical to additives but which occur naturally in fruits and vegetables is found in a number of cases to be higher than the intake of additives added during the manufacture of foodstuffs. While the difficulties are recognized in contributing to the compilation of food additive intake data, industry as a whole, i.e. the food manufacturing and food additive manufacturing industries, are confident that in a concerted effort, use data on food additives by industry can be made available. Lastly, the paper points out that with the transportation of the additives directives into national legislation and the time by which the food industry will be able to make use of the new food legislative environment several years will still go by; food additives use data by the food industry will thus have to be reviewed at the beginning of the next century. PMID:8792135

  18. Superposition Enhanced Nested Sampling

    NASA Astrophysics Data System (ADS)

    Martiniani, Stefano; Stevenson, Jacob D.; Wales, David J.; Frenkel, Daan

    2014-07-01

    The theoretical analysis of many problems in physics, astronomy, and applied mathematics requires an efficient numerical exploration of multimodal parameter spaces that exhibit broken ergodicity. Monte Carlo methods are widely used to deal with these classes of problems, but such simulations suffer from a ubiquitous sampling problem: The probability of sampling a particular state is proportional to its entropic weight. Devising an algorithm capable of sampling efficiently the full phase space is a long-standing problem. Here, we report a new hybrid method for the exploration of multimodal parameter spaces exhibiting broken ergodicity. Superposition enhanced nested sampling combines the strengths of global optimization with the unbiased or athermal sampling of nested sampling, greatly enhancing its efficiency with no additional parameters. We report extensive tests of this new approach for atomic clusters that are known to have energy landscapes for which conventional sampling schemes suffer from broken ergodicity. We also introduce a novel parallelization algorithm for nested sampling.

  19. Simplified sample preparation method for triclosan and methyltriclosan determination in biota and foodstuff samples.

    PubMed

    Canosa, P; Rodríguez, I; Rubí, E; Ramil, M; Cela, R

    2008-04-25

    An improved method for the determination of triclosan (TCS) and methyltriclosan (MTCS) in fish and foodstuff samples is presented. Analytes were simultaneously extracted and purified using the matrix solid-phase dispersion (MSPD) technique, and then selectively determined by gas chromatography with tandem mass spectrometry (GC-MS/MS). Several combinations of dispersants, clean-up co-sorbents and extraction solvents were tested in order to obtain lipid-free extracts and quantitative recoveries for TCS and MTCS. Under optimised conditions, 0.5 g samples were dispersed using 1.5 g of neutral silica in a mortar with a pestle, and transferred to a polypropylene cartridge containing 3 g of silica impregnated with 10% of sulphuric acid (SiO2-H2SO4, 10%, w/w). Analytes were recovered with 10 mL of dichloromethane whereas lipids were oxidized in the layer of acidic silica. The extract was concentrated to dryness and re-constituted with 1 mL of ethyl acetate. Then, a fraction of 0.5 mL was mixed with 50 microL of N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA) and injected in the GC-MS/MS system. The developed method provided absolute recoveries between 77 and 120% for different samples spiked at the low ng g(-1) level, quantification limits in the range of 1-2 ng g(-1) and a considerable simplicity in comparison with previously developed sample preparation approaches. Experiments carried out placing sliced food samples in direct contact with TCS-treated kitchenware surfaces showed the capability of the biocide to migrate into foodstuffs. PMID:18329035

  20. An additional middle cuneiform?

    PubMed Central

    Brookes-Fazakerley, S.D.; Jackson, G.E.; Platt, S.R.

    2015-01-01

    Additional cuneiform bones of the foot have been described in reference to the medial bipartite cuneiform or as small accessory ossicles. An additional middle cuneiform has not been previously documented. We present the case of a patient with an additional ossicle that has the appearance and location of an additional middle cuneiform. Recognizing such an anatomical anomaly is essential for ruling out second metatarsal base or middle cuneiform fractures and for the preoperative planning of arthrodesis or open reduction and internal fixation procedures in this anatomical location. PMID:26224890

  1. Levels of dioxins and dioxin-like PCBs in food samples on the Greek market.

    PubMed

    Papadopoulos, Athanasios; Vassiliadou, Irene; Costopoulou, Danae; Papanicolaou, Christina; Leondiadis, Leondios

    2004-11-01

    Food intake is the main source of exposure to dioxin-like compounds for humans. The results of a surveillance programme on polychlorinated dibenzo-p-dioxins (PCDDs), dibenzofurans (PCDFs) and co-planar polychlorinated biphenyls (co-PCBs) in 77 food samples from the Greek market and producers are presented. The study included the analyses of milk and dairy products, meat and meat products, fish, vegetable oil, eggs, fruit, vegetable and rice collected between August and December 2002. After extraction, extracts were cleaned up on a series of carbon column chromatography, silica gel, alumina chromatography, and then analysed by high resolution gas chromatography/high resolution mass spectrometry. All samples had a dioxin content far below the EC Regulation (2375/2001/EC) limits. PMID:15331268

  2. Sensitive determination of herbicides in food samples by nonaqueous CE using pressurized liquid extraction.

    PubMed

    Carabias-Martínez, Rita; Rodríguez-Gonzalo, Encarnacion; Miranda-Cruz, Edith; Domínguez-Alvarez, Javier; Hernández-Méndez, Jesus

    2007-10-01

    We have developed a method involving extraction with mixtures of solvents under pressure (pressurized liquid extraction (PLE)) for the determination of triazine herbicides in a series of samples from the food industry. The organic extracts obtained were subjected to a clean-up step with SPE, using Oasis MCX sorbents, after which they were analyzed by NACE. Potato was chosen as a representative matrix of horticultural products since it has a high water content. Spiked potato samples were used to optimize extraction conditions. In order to compare the results obtained with NACE, different studies were also conducted using HPLC. The detection limits in NACE were similar to those found with HPLC and were of the order of 10-15 microg/kg, depending on the analyte. Satisfactory results were obtained on applying the method proposed for the potato matrix (PLE with separation by electrophoresis) to other food matrices such as other tubercles, fruits, vegetables and cereals. PMID:17893944

  3. 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. PMID:26796977

  4. Recovery of Cryptosporidium oocysts from small and large volume water samples using a compressed foam filter system.

    PubMed

    Sartory, D P; Parton, A; Parton, A C; Roberts, J; Bergmann, K

    1998-12-01

    A novel filter system comprising open cell reticulated foam rings compressed between retaining plates and fitted into a filtration housing was evaluated for the recovery of oocysts of Cryptosporidium from water. Mean recoveries of 90.2% from seeded small and large volume (100-2000 l) tap water samples, and 88.8% from 10-20 l river water samples, were achieved. Following a simple potassium citrate flotation concentrate clean-up procedure, mean recoveries were 56.7% for the tap water samples and 60.9% for river water samples. This represents a marked improvement in capture and recovery of Cryptosporidium oocysts from water compared with conventional polypropylene wound cartridge filters and membrane filters. PMID:9871348

  5. Quantitative microanalysis of bile acids in biological samples. Collaborative study.

    PubMed

    Nakayama, F

    1988-10-28

    The analysis of bile acids in biological samples has always presented a problem because of their complex nature and low concentration. Recently, newer analytical procedures for bile acids have become available, including enzymatic analysis, radioimmunoassay, thin-layer chromatography (TLC), gas chromatography, high-performance liquid chromatography (HPLC) and gas chromatography-mass spectrometry (GC-MS) with selected ion monitoring (SIM). However, they differ greatly with respect to specificity, sensitivity, accuracy and simplicity. On the other hand, the choice of analytical procedure differs according to the specific aims and the nature of biological samples to be analysed. These newer procedures have been compared in a double-blind fashion by distributing bile, plasma and urine samples to seven participating laboratories. GC-MS-SIM was found to be the most sensitive and reliable, but it requires other procedures for preliminary clean-up and fractionation steps. Enzymatic analysis is simple and gives small analytical errors but tends to over-estimate plasma bile acids. Radioimmunoassay gives variable results but is useful as a screening procedure for large numbers of plasma samples. TLC gives reliable results for biliary bile acids in experienced hands, except for differentiation between conjugated dihydroxycholanoic acids. HPLC, whether using derivatization or with fixed 3 alpha-hydroxy steroid dehydrogenase detection, is suitable for the analysis of major bile acids in normal human serum but not for the identification of unknown minor peaks. PMID:3243854

  6. Carbamate deposit control additives

    SciTech Connect

    Honnen, L.R.; Lewis, R.A.

    1980-11-25

    Deposit control additives for internal combustion engines are provided which maintain cleanliness of intake systems without contributing to combustion chamber deposits. The additives are poly(oxyalkylene) carbamates comprising a hydrocarbyloxyterminated poly(Oxyalkylene) chain of 2-5 carbon oxyalkylene units bonded through an oxycarbonyl group to a nitrogen atom of ethylenediamine.

  7. 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

  8. 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. PMID:26830597

  9. Simultaneous determination of 19 triazine pesticides and degradation products in processed cereal samples from Chinese total diet study by isotope dilution-high performance liquid chromatography-linear ion trap mass spectrometry.

    PubMed

    Li, Peng; Yang, Xin; Miao, Hong; Zhao, Yunfeng; Liu, Wei; Wu, Yongning

    2013-06-01

    A selective and sensitive isotope dilution-high performance liquid chromatography-linear ion trap mass spectrometry (Isotope Dilution-HPLC-LIT-MS(3)) method was developed for the simultaneous determination of 19 triazine pesticides and their degradation products in processed cereal samples from Chinese total diet study (TDS). The method integrated the addition of isotope internal standards, liquid-liquid extraction (LLE), clean-up with MCX solid-phase extraction (SPE) cartridges and HPLC-LIT-MS(3) analysis with selected reaction monitoring (SRM) mode. Matrix-matched calibration curves showed good linearity (R(2)≥0.9940) verified by applying the Mandel's fitting test (p>0.087) performed at the 95% confidence level. Decision limits (CCαs) and detection capabilities (CCβs) of the 19 triazine pesticides and their degradation products fell in the ranges of 0.0020-0.4200 μg kg(-1) and 0.0024-0.4500 μg kg(-1), respectively. Recoveries ranged from 70.1% to 112.8%, with the relative standard deviations (RSDs) ranging from 1.5% to 13.5%. Furthermore, the proposed method was applied to analyzing the proposed cereal samples from the fourth Chinese TDS. Eleven triazines were detected in six cereal samples with the concentrations ranging from 0.013 to 0.987 μg kg(-1). This method can also be used for the further determination of the triazines in other food group composites, and ultimately served as a methodological foundation for assessing the triazines in the average Chinese diet in the general population. PMID:23684466

  10. 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.

  11. 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.

  12. 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…

  13. 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.

  14. 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.

  15. 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)

  16. Additional Types of Neuropathy

    MedlinePlus

    ... A A Listen En Español Additional Types of Neuropathy Charcot's Joint Charcot's Joint, also called neuropathic arthropathy, ... can stop bone destruction and aid healing. Cranial Neuropathy Cranial neuropathy affects the 12 pairs of nerves ...

  17. A single-step pesticide extraction and clean-up multi-residue analytical method by selective pressurized liquid extraction followed by on-line solid phase extraction and ultra-high-performance liquid chromatography-tandem mass spectrometry for complex matrices.

    PubMed

    Rodrigues, Elsa Teresa; Pardal, Miguel Ângelo; Salgueiro-González, Noelia; Muniategui-Lorenzo, Soledad; Alpendurada, Maria Fátima

    2016-06-24

    Pesticides, a group of compounds linked to human activity, may, when in toxic levels, have a profound effect on water quality, and hence result in adverse consequences to aquatic life and ultimately to human health. Analytical challenges arise when successfully trying to determine these levels in environmental complex matrices. Therefore, fast, simple, sensitive and selective analytical methodologies for multi-residue determination of pesticides (atrazine, azoxystrobin, bentazon, λ-cyhalothrin, penoxsulam and terbuthylazine) in sediment, macrophytes (algae and aquatic plants) and aquatic animals were developed and validated. The established methods were matrix-dependent and were based on Selective Pressurized Liquid Extraction (SPLE) followed by on-line Solid Phase Extraction and Ultra Performance Liquid Chromatography-tandem Mass Spectrometry (on-line SPE-UPLC-ESI-MS/MS). This cutting-edge research methodology uses a small amount of sample, is time saving and reduces the use of organic solvents in compliance with Green Chemistry principles. The analytical features were adequate for all compounds in all studied matrices. The established methodology was applied on real marine samples and no pesticide concentrations above their respective method quantification limits were measured in sediments or aquatic plants. However, terbuthylazine was found in the macroalgae Ulva spp. (108ngg(-1)dw) and all the prospected pesticides were measured above their respective method quantification limits in the bivalve Scrobicularia plana (atrazine: 48ngg(-1)dw, azoxystrobin: 64ngg(-1)dw, bentazon: 33ngg(-1)dw, λ-cyhalothrin: 2531ngg(-1)dw, penoxsulam: 50ngg(-1)dw, and terbuthylazine: 44ngg(-1)dw). PMID:27234845

  18. Benthic flux sampling device. Operations, methods, and procedures. Final report

    SciTech Connect

    Chadwick, D.B.; Stanley, S.D.

    1993-02-01

    As part of the Navy's clean up program, the Installation Restoration (IR) Program, methods are evaluated to better assess suitable remediation and restoration strategies for sites that contain sediments contaminated with toxic compounds. Toward this goal, we have developed a Benthic Flux Sampling Device (BFSD) to quantify mobility of toxicants from contaminated sediments. The BFSD is a remote instrument for in-situ measurement of toxicant flux rates from sediments. A flux out of or into the sediment is measured by isolating a volume of water above the sediment, drawing off samples from this volume over time, and analyzing these samples for increase or decrease in toxicant concentration. Increasing concentrations indicate that the toxicant is fluxing out of the sediment. Decreasing concentrations indicate that the toxicant is fluxing into the sediment. Initial tests carried out in conjunction with Scripps Institution of Oceanography and the Environmental Protection Agency's Environmental Research Laboratory (Newport, OR) show that the system is capable of measuring a variety of contaminant and nutrient fluxes.... Marine chemistry, Benthic flux.

  19. 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

  20. 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.

  1. 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.

  2. 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.

  3. 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

  4. Fluidic sampling

    SciTech Connect

    Houck, E.D.

    1992-04-20

    This paper covers the development of the fluidic sampler and its testing in a fluidic transfer system. The major findings of this paper are as follows. Fluidic jet samples can dependably produce unbiased samples of acceptable volume. The fluidic transfer system with a fluidic sampler in-line will transfer water to a net lift of 37.2--39.9 feet at an average ratio of 0.02--0.05 gpm (77--192 cc/min). The fluidic sample system circulation rate compares very favorably with the normal 0.016--0.026 gpm (60--100 cc/min) circulation rate that is commonly produced for this lift and solution with the jet-assisted airlift sample system that is normally used at ICPP. The volume of the sample taken with a fluidic sampler is dependant on the motive pressure to the fluidic sampler, the sample bottle size and on the fluidic sampler jet characteristics. The fluidic sampler should be supplied with fluid having the motive pressure of the 140--150 percent of the peak vacuum producing motive pressure for the jet in the sampler. Fluidic transfer systems should be operated by emptying a full pumping chamber to nearly empty or empty during the pumping cycle, this maximizes the solution transfer rate.

  5. Fluidic sampling

    NASA Astrophysics Data System (ADS)

    Houck, E. D.

    1992-04-01

    This paper covers the development of the fluidic sampler and its testing in a fluidic transfer system. The major findings of this paper are as follows. Fluidic jet samples can dependably produce unbiased samples of acceptable volume. The fluidic transfer system with a fluidic sampler in-line will transfer water to a net lift of 37.2-39.9 feet at an average ratio of 0.02-0.05 gpm (77-192 cc/min). The fluidic sample system circulation rate compares very favorably with the normal 0.016-0.026 gpm (60-100 cc/min) circulation rate that is commonly produced for this lift and solution with the jet-assisted airlift sample system that is normally used at ICPP. The volume of the sample taken with a fluidic sampler is dependant on the motive pressure to the fluidic sampler, the sample bottle size and on the fluidic sampler jet characteristics. The fluidic sampler should be supplied with fluid having the motive pressure of the 140-150 percent of the peak vacuum producing motive pressure for the jet in the sampler. Fluidic transfer systems should be operated by emptying a full pumping chamber to nearly empty or empty during the pumping cycle, this maximizes the solution transfer rate.

  6. 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

  7. 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...

  8. Multifunctional fuel additives

    SciTech Connect

    Baillargeon, D.J.; Cardis, A.B.; Heck, D.B.

    1991-03-26

    This paper discusses a composition comprising a major amount of a liquid hydrocarbyl fuel and a minor low-temperature flow properties improving amount of an additive product of the reaction of a suitable diol and product of a benzophenone tetracarboxylic dianhydride and a long-chain hydrocarbyl aminoalcohol.

  9. 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

  10. 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.

  11. 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.

  12. 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.

  13. Boron addition to alloys

    SciTech Connect

    Coad, B. C.

    1985-08-20

    A process for addition of boron to an alloy which involves forming a melt of the alloy and a reactive metal, selected from the group consisting of aluminum, titanium, zirconium and mixtures thereof to the melt, maintaining the resulting reactive mixture in the molten state and reacting the boric oxide with the reactive metal to convert at least a portion of the boric oxide to boron which dissolves in the resulting melt, and to convert at least portion of the reactive metal to the reactive metal oxide, which oxide remains with the resulting melt, and pouring the resulting melt into a gas stream to form a first atomized powder which is subsequently remelted with further addition of boric oxide, re-atomized, and thus reprocessed to convert essentially all the reactive metal to metal oxide to produce a powdered alloy containing specified amounts of boron.

  14. Tackifier for addition polyimides

    NASA Technical Reports Server (NTRS)

    Butler, J. M.; St.clair, T. L.

    1980-01-01

    A modification to the addition polyimide, LaRC-160, was prepared to improve tack and drape and increase prepeg out-time. The essentially solventless, high viscosity laminating resin is synthesized from low cost liquid monomers. The modified version takes advantage of a reactive, liquid plasticizer which is used in place of solvent and helps solve a major problem of maintaining good prepeg tack and drape, or the ability of the prepeg to adhere to adjacent plies and conform to a desired shape during the lay up process. This alternate solventless approach allows both longer life of the polymer prepeg and the processing of low void laminates. This approach appears to be applicable to all addition polyimide systems.

  15. 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.

  16. [Biologically active food additives].

    PubMed

    Velichko, M A; Shevchenko, V P

    1998-07-01

    More than half out of 40 projects for the medical science development by the year of 2000 have been connected with the bio-active edible additives that are called "the food of XXI century", non-pharmacological means for many diseases. Most of these additives--nutricevtics and parapharmacevtics--are intended for the enrichment of food rations for the sick or healthy people. The ecologicaly safest and most effective are combined domestic adaptogens with immuno-modulating and antioxidating action that give anabolic and stimulating effect,--"leveton", "phytoton" and "adapton". The MKTs-229 tablets are residue discharge means. For atherosclerosis and general adiposis they recommend "tsar tablets" and "aiconol (ikhtien)"--on the base of cod-liver oil or "splat" made out of seaweed (algae). All these preparations have been clinically tested and received hygiene certificates from the Institute of Dietology of the Russian Academy of Medical Science. PMID:9752776

  17. 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.

  18. Hydrocarbon fuel additive

    SciTech Connect

    Ambrogio, S.

    1989-02-28

    This patent describes the method of fuel storage or combustion, wherein the fuel supply contains small amounts of water, the step of adding to the fuel supply an additive comprising a blend of a hydrophilic agent chosen from the group of ethylene glycol, n-butyl alcohol, and cellosolve in the range of 22-37% by weight; ethoxylated nonylphenol in the range of 26-35% by weight; nonylphenol polyethylene glycol ether in the range of 32-43% by weight.

  19. 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. PMID:24729671

  20. 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.

  1. Oil additive process

    SciTech Connect

    Bishop, H.

    1988-10-18

    This patent describes a method of making an additive comprising: (a) adding 2 parts by volume of 3% sodium hypochlorite to 45 parts by volume of diesel oil fuel to form a sulphur free fuel, (b) removing all water and foreign matter formed by the sodium hypochlorite, (c) blending 30 parts by volume of 24% lead naphthanate with 15 parts by volume of the sulphur free fuel, 15 parts by volume of light-weight material oil to form a blended mixture, and (d) heating the blended mixture slowly and uniformly to 152F.

  2. Matrix removal in state of the art sample preparation methods for serum by charged aerosol detection and metabolomics-based LC-MS.

    PubMed

    Schimek, Denise; Francesconi, Kevin A; Mautner, Anton; Libiseller, Gunnar; Raml, Reingard; Magnes, Christoph

    2016-04-01

    Investigations into sample preparation procedures usually focus on analyte recovery with no information provided about the fate of other components of the sample (matrix). For many analyses, however, and particularly those using liquid chromatography-mass spectrometry (LC-MS), quantitative measurements are greatly influenced by sample matrix. Using the example of the drug amitriptyline and three of its metabolites in serum, we performed a comprehensive investigation of nine commonly used sample clean-up procedures in terms of their suitability for preparing serum samples. We were monitoring the undesired matrix compounds using a combination of charged aerosol detection (CAD), LC-CAD, and a metabolomics-based LC-MS/MS approach. In this way, we compared analyte recovery of protein precipitation-, liquid-liquid-, solid-phase- and hybrid solid-phase extraction methods. Although all methods provided acceptable recoveries, the highest recovery was obtained by protein precipitation with acetonitrile/formic acid (amitriptyline 113%, nortriptyline 92%, 10-hydroxyamitriptyline 89%, and amitriptyline N-oxide 96%). The quantification of matrix removal by LC-CAD showed that the solid phase extraction method (SPE) provided the lowest remaining matrix load (48-123 μg mL(-1)), which is a 10-40 fold better matrix clean-up than the precipitation- or hybrid solid phase extraction methods. The metabolomics profiles of eleven compound classes, comprising 70 matrix compounds showed the trends of compound class removal for each sample preparation strategy. The collective data set of analyte recovery, matrix removal and matrix compound profile was used to assess the effectiveness of each sample preparation method. The best performance in matrix clean-up and practical handling of small sample volumes was showed by the SPE techniques, particularly HLB SPE. CAD proved to be an effective tool for revealing the considerable differences between the sample preparation methods. This detector

  3. 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%. PMID:18768184

  4. 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.

  5. Multiresidue method for simultaneous determination of quinolone antibacterials in pig kidney samples by liquid chromatography with fluorescence detection.

    PubMed

    Hassouan, M K; Ballesteros, O; Zafra, A; Vílchez, J L; Navalón, A

    2007-11-15

    A new analytical method for simultaneous determination of eight quinolones namely, ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, flumequine, marbofloxacin, oxolinic acid and sarafloxacin, in pig kidney samples was developed. The procedure involves the extraction of the quinolones from the samples by traditional extraction, a step for clean-up and preconcentration of the analytes by solid-phase extraction (SPE) and subsequent liquid chromatography separation with fluorescence detection (LC-FD). The mobile phase was composed of acetonitrile and 10 mM citrate buffer solution of pH 4.5, with an initial composition of acetonitrile-water 12:88 (v/v) and using linear gradient elution. Norfloxacin was used as internal standard. The limits of detection (1-8 microg kg(-1)) and the limits of quantification (5-27 microg kg(-1)) found were lower than the maximum residue limits regulated by the European Union for these compounds in pig kidney. PMID:17951118

  6. 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. PMID:27283719

  7. Performance Boosting Additive

    NASA Technical Reports Server (NTRS)

    1999-01-01

    Mainstream Engineering Corporation was awarded Phase I and Phase II contracts from Goddard Space Flight Center's Small Business Innovation Research (SBIR) program in early 1990. With support from the SBIR program, Mainstream Engineering Corporation has developed a unique low cost additive, QwikBoost (TM), that increases the performance of air conditioners, heat pumps, refrigerators, and freezers. Because of the energy and environmental benefits of QwikBoost, Mainstream received the Tibbetts Award at a White House Ceremony on October 16, 1997. QwikBoost was introduced at the 1998 International Air Conditioning, Heating, and Refrigeration Exposition. QwikBoost is packaged in a handy 3-ounce can (pressurized with R-134a) and will be available for automotive air conditioning systems in summer 1998.

  8. Sewage sludge additive

    NASA Technical Reports Server (NTRS)

    Kalvinskas, J. J.; Mueller, W. A.; Ingham, J. D. (Inventor)

    1980-01-01

    The additive is for a raw sewage treatment process of the type where settling tanks are used for the purpose of permitting the suspended matter in the raw sewage to be settled as well as to permit adsorption of the dissolved contaminants in the water of the sewage. The sludge, which settles down to the bottom of the settling tank is extracted, pyrolyzed and activated to form activated carbon and ash which is mixed with the sewage prior to its introduction into the settling tank. The sludge does not provide all of the activated carbon and ash required for adequate treatment of the raw sewage. It is necessary to add carbon to the process and instead of expensive commercial carbon, coal is used to provide the carbon supplement.

  9. 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.

  10. Plant sampling guidelines

    Technology Transfer Automated Retrieval System (TEKTRAN)

    This document provides GRACEnet guidelines for sampling plant shoots and roots with additional guidelines and references for determining plant quality. Plant biomass including rhizodeposition provides the majority of net primary production that fuels above- and below-ground ecosystems. Thus, high ca...

  11. Application of the SmartSampling Methodology to the Evaluation of Contaminated Landscape Soils at Brookhaven National Laboratory

    SciTech Connect

    RAUTMAN,CHRISTOPHER A.

    2000-08-01

    Portions of the SmartSampling{trademark} analysis methodology have been applied to the evaluation of radioactive contaminated landscape soils at Brookhaven National Laboratory. Specifically, the spatial, volumetric distribution of cesium-137 ({sup 137}Cs) contamination within Area of Concern 16E-1 has been modeled probabilistically using a geostatistical methodology, with the purpose of identifying the likelihood of successfully reducing, with respect to a pre-existing, baseline remediation plan, the volume of soil that must be disposed of offsite during clean-up. The principal objective of the analysis was to evaluate the likelihood of successful deployment of the Segmented Gate System (SGS), a novel remediation approach that emphasizes real-time separation of clean from contaminated materials during remediation operations. One primary requirement for successful application of the segmented gate technology investigated is that a variety of contaminant levels exist at the deployment site, which would enable to the SGS to discriminate material above and below a specified remediation threshold value. The results of this analysis indicate that there is potential for significant volume reduction with respect to the baseline remediation plan at a threshold excavation level of 23 pCi/g {sup 137}Cs. A reduction of approximately 50%, from a baseline volume of approximately 1,064.7 yd{sup 3} to less than 550 yd{sup 3}, is possible with acceptance of only a very small level of engineering risk. The vast majority of this volume reduction is obtained by not excavating almost all of levels 3 and 4 (from 12 to 24 inches in depth), which appear to be virtually uncontaminated, based on the available data. Additional volume reductions related to soil materials on levels 1 (depths of 0--6 inches) and 2 (6--12 inches) may be possible, specifically through use of the SGS technology. Level-by-level evaluation of simulation results suggests that as much as 26 percent of level 1 and as

  12. Validated method for the determination of perfluorinated compounds in placental tissue samples based on a simple extraction procedure followed by ultra-high performance liquid chromatography-tandem mass spectrometry analysis.

    PubMed

    Martín, J; Rodríguez-Gómez, R; Zafra-Gómez, A; Alonso, E; Vílchez, J L; Navalón, A

    2016-04-01

    Xenobiotic exposure during pregnancy is inevitable. Determination of perfluorinated compounds (PFCs), chemicals described as environmental contaminants by Public Health Authorities due to their persistence, bioaccumulation and toxicity, is a challenge. In the present work, a method based on a simplified sample treatment involving freeze-drying, solvent extraction and dispersive clean-up of the extracts using C18 sorbents followed by an ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis was developed and validated for the determination of five perfluorinated carboxylic acids (C4-C8) and perfluorooctane sulfonate (PFOS) in placental tissue samples. The most influential parameters affecting the extraction method and clean-up were optimized using Design of Experiments (DOE). The method was validated using matrix-matched calibration. Found limits of detection (LODs) ranged from 0.03 to 2 ng g(-1) and limits of quantification (LOQs) from 0.08 to 6 ng g(-1), while inter- and intra-day variability was under 14% in all cases. Recovery rates for spiked samples ranged from 94% to 113%. The method was satisfactorily applied for the determination of compounds in human placental tissue samples collected at delivery from 25 randomly selected women. PMID:26838396

  13. 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...

  14. Code-regenerative clean-up loop for a ranging transponder

    NASA Technical Reports Server (NTRS)

    Hurd, W. J.

    1973-01-01

    Digital processing system phase locks on received ranging signal and creates clean replica of received ranging code. System is broadly applicable to variety of terrestrial ranging problems, including oceanic navigation.

  15. 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.

  16. 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.

  17. 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.

  18. 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 ...

  19. 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…

  20. CLEANING UP MIXED WASTE STREAMS--THE TANK TRUCK WASHING EXAMPLE

    EPA Science Inventory

    This Executive Report describes the joint venture of EPA's Office of Energy, Minerals and Industry and the Matlack Corporation into the construction and demonstration of a full-scale tank truck wastewater treatment plant. The report covers the technical and economic viability of ...

  1. 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.

  2. 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...

  3. Does remediation save lives? - on the cost of cleaning up arsenic-contaminated sites in Sweden.

    PubMed

    Forslund, Johanna; Samakovlis, Eva; Johansson, Maria Vredin; Barregard, Lars

    2010-07-15

    Sweden has only just begun remediation of its many contaminated sites, a process that will cost an estimated SEK 60,000 million (USD 9100 million). Although the risk assessment method, carried out by the Swedish EPA, is driven by health effects, it does not consider actual exposure. Instead, the sites are assessed based on divergence from guideline values. This paper uses an environmental medicine approach that takes exposure into account to analyse how cancer risks on and near arsenic-contaminated sites are implicitly valued in the remediation process. The results show that the level of ambition is high. At 23 contaminated sites, the cost per life saved varies from SEK 287 million to SEK 1,835,000 million, despite conservative calculations that in fact probably underestimate the costs. It is concluded that if environmental health risks are to be reduced, there are probably other areas where economic resources can be used more cost-effectively. PMID:20439110

  4. 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…

  5. Development and demonstration of biosorbents for clean-up of uranium in water. CRADA final report

    SciTech Connect

    Faison, B.D.; Hu, M.Z.C.; Norman, J.M.; Reeves, M.E.; Williams, L.; Schmidt-Kuster, W.; Darnell, K. |

    1997-08-01

    Pseudomonas aeruginosa strain CSU, a nongenetically engineered bacterial strain known to bind dissolved hexavalent uranium, shows particular promise as the basis of an immobilized-cell process for removal of dissolved uranium from contaminated wastewaters. It was characterized with respect to its sorptive active. Living, heat-killed, permeabilized, and unreconstituted lyophilized cells were all capable of binding uranium. The uranium biosorption equilibrium could be described by the Langmuir isotherm. The rate of uranium adsorption increased following permeabilization of the outer and/or cytoplasmic membrane by organic solvents such as acetone. P. aeruginosa CSU biomass was significantly more sorptive toward uranium than certain novel, patented biosorbents derived from algal or fungal biomass sources. P. aeruginosa CSU biomass was also competitive with commercial cation-exchange resins, particularly in the presence of dissolved transition metals. Uranium binding by P. aeruginosa was clearly pH dependent. Uranium loading capacity increased with increasing pH under acidic conditions, presumably as a function of uranium speciation and due to the H{sup +} competition at some binding sites. Nevertheless, preliminary evidence suggests that this microorganism is also capable of binding anionic hexavalent uranium complexes. Ferric iron was a strong inhibitor of uranium binding to P. aeruginosa CSU biomass, and the presence of uranium also decreased the Fe{sup 3+} loading when the biomass was not saturated with Fe{sup 3+}, suggesting that Fe{sup 3+} and uranium may share the same binding sites on biomass.

  6. 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…

  7. 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.

  8. 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...

  9. 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.

  10. EMERGENCY RESPONSE EQUIPMENT TO CLEAN UP HAZARDOUS CHEMICAL RELEASES AT SPILLS AND UNCONTROLLED WASTE SITES

    EPA Science Inventory

    This paper reviews some of the research activities of the U.S. Environmental Protection Agency (EPA) regarding the development of emergency response equipment to control hazardous chemical releases. Several devices and systems have been developed by EPA for environmental emergenc...

  11. 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.

  12. USING WASTE TO CLEAN UP THE ENVIRONMENT: CELLULOSIC ETHANOL, THE FUTURE OF FUELS

    EPA Science Inventory

    In the process of converting municipal solid waste (MSW) into ethanol we optimized the first two major steps of pretreatment and enzymatic hydrolysis stages to enhance the sugar yield and to reduce the cost. For the pretreatment process, we tested different parameters of react...

  13. Summary of drag clean-up tests in NASA Langley full-scale tunnel

    NASA Technical Reports Server (NTRS)

    Mckinney, M. O.

    1975-01-01

    This summary of drag results presents tabulations on fighter aircraft and light twin general aviation aircraft wind tunnel tests. The figures show that the friction drag for light twins is larger than that for the fighters because of the greater wetted area and the smaller wing area used for reference. Full scale tunnel tests developed the following design features contributing to excessive drag: cooling flow system, engine exhaust stacks, landing gears, control surface gaps, and wing irregularities and leakages.

  14. 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...

  15. 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...

  16. 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...

  17. 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…

  18. Soil clean up by in-situ aeration. VII. High-speed modeling of diffusion kinetics

    SciTech Connect

    Rodriguez-Maroto, J.M. ); Wilson, D.J. )

    1991-01-01

    A mathematical model for soil vacuum extraction is developed which allows the modeling of vapor stripping from media of highly heterogeneous permeability, in which one may not be able to make the assumption of local equilibrium between the stationary phase(s) and the moving vapor phase with respect to volatile organic compound (VOC) transport. A lumped parameter approximation is used to deal with the kinetics of diffusion (and/or desorption) of the VOC from the interiors of lumps of clay or porous bedrock out into the advecting soil gas. This model, which makes the steady-state approximation for the VOC vapor concentrations, typically uses less than one-twentieth the computer time of an earlier nonsteady-state model and gives results which are in excellent agreement with that model. This model also yields results which are in agreement with a local equilibrium model if the rate constant for diffusion/desorption is large. The effects of impermeable caps and passive vent wells decrease as the rate of diffusion/desorption is decreased.

  19. 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.

  20. 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.

  1. A gas stream clean-up filter and method for forming same

    SciTech Connect

    Mei, J.S.; Halow, J.S.; DeVault, J.D.

    1992-12-31

    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.

  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. 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.

  4. Surgical scrubbing: can we clean up our carbon footprints by washing our hands?

    PubMed

    Somner, J E A; Stone, N; Koukkoulli, A; Scott, K M; Field, A R; Zygmunt, J

    2008-11-01

    A growing scientific consensus states that the global climate is changing and that human activity is responsible for these changes. It folLows that each of us has a responsibility to look at how our own lives impact on the environment. This study aimed to investigate water use during surgical scrubbing. Two water delivery systems were assessed to see whether technological innovation can promote more 'environmentally friendly' scrubbing behaviour. At least 10 different individuals, comprising surgeons, assistants and scrub nurses, were observed at two sites. Twenty-five separate surgical scrubs were observed in each location and the length of time for which the tap was on recorded. The tap was on during surgical scrubbing for a mean of 2 min 23 s at Gartnavel General Hospital (maximum: 4 min 37 s; minimum: 49 s; SD: 55 s) and for a mean of 1 min 7 s at Stobhill Hospital (maximum: 2 min 25 s; minimum: 19 s; SD: 33 s). The mean 'tap on' time (in seconds) at Gartnavel was significantly greater than that at Stobhill [t(39.5)=P<0.001]. A different tap design resulted in a net saving of 5.7 L of hot water, approximately 600 kJ of energy and 80 g of carbon dioxide emitted per surgical scrub. Surgical scrubbing is a ubiquitous procedure performed daily in healthcare settings. A simple technological solution can reduce water and energy use by modifying hand-washing behaviour and thereby reduce the carbon footprint of surgical scrubbing. PMID:18701193

  5. 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.

  6. 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.

  7. 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.

  8. "Get Ready for Migration: Clean-Up Your Collection"--What Does that Mean?

    ERIC Educational Resources Information Center

    Lawrence, Peg; Weber, Lynne

    2008-01-01

    This article discusses some of the premigration tasks at Minnesota State Mankato in preparation for migration to a new integrated library system, ALEPH. The authors describe the review of circulation policies to make sure that only relevant, current data and practices were carried over. There is emphasis on the need for ongoing review of policies…

  9. 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...

  10. 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.

  11. USING VEGETATION TO CLEAN UP TNT-CONTAMINATED SITES. (R825513C013)

    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...

  12. TECHNICAL APPROACHES TO CHARACTERIZING AND CLEANING UP BROWNFIELDS SITES; A SERIES OF GUIDANCE DOCUMENTS

    EPA Science Inventory

    The area of Brownfields Redevelopment is important to Communities for many reasons including financial, community development, and environmental justice issues. Several considerations should be made in decisions involving Brownfields Redevelopment. These considerations often r...

  13. 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.

  14. 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. PMID:23767118

  15. 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.

  16. 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...

  17. 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...

  18. 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...

  19. Cleaning Up and Maintenance in the Wake of an Urban School Administration Tempest.

    ERIC Educational Resources Information Center

    Murtadha-Watts, Khuala

    2000-01-01

    Describes the context of a city corporation's attempt to initiate educational reform, focusing on two city school administrators, a newly hired Latina superintendent and an African American female assistant superintendent. Uses the metaphor of a tempest to describe the tension between the urge for rapid reform of the new superintendent and the…

  20. 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.

  1. Deterministic multidimensional nonuniform gap sampling

    NASA Astrophysics Data System (ADS)

    Worley, Bradley; Powers, Robert

    2015-12-01

    Born from empirical observations in nonuniformly sampled multidimensional NMR data relating to gaps between sampled points, the Poisson-gap sampling method has enjoyed widespread use in biomolecular NMR. While the majority of nonuniform sampling schemes are fully randomly drawn from probability densities that vary over a Nyquist grid, the Poisson-gap scheme employs constrained random deviates to minimize the gaps between sampled grid points. We describe a deterministic gap sampling method, based on the average behavior of Poisson-gap sampling, which performs comparably to its random counterpart with the additional benefit of completely deterministic behavior. We also introduce a general algorithm for multidimensional nonuniform sampling based on a gap equation, and apply it to yield a deterministic sampling scheme that combines burst-mode sampling features with those of Poisson-gap schemes. Finally, we derive a relationship between stochastic gap equations and the expectation value of their sampling probability densities.

  2. A novel addition polyimide adhesive

    NASA Technical Reports Server (NTRS)

    St.clair, T. L.; Progar, D. J.

    1981-01-01

    An addition polyimide adhesive, LARC 13, was developed which shows promise for bonding both titanium and composites for applications which require service temperatures in excess of 533 K. The LARC 13 is based on an oligomeric bis nadimide containing a meta linked aromatic diamine. The adhesive melts prior to polymerization due to its oligomeric nature, thereby allowing it to be processed at 344 kPa or less. Therefore, LARC 13 is ideal for the bonding of honeycomb sandwich structures. After melting, the resin thermosets during the cure of the nadic endcaps to a highly crosslinked system. Few volatiles are evolved, thus allowing large enclosed structures to be bonded. Preparation of the adhesive as well as bonding, aging, and testing of lap shear and honeycomb samples are discussed.

  3. Additive attacks on speaker recognition

    NASA Astrophysics Data System (ADS)

    Farrokh Baroughi, Alireza; Craver, Scott

    2014-02-01

    Speaker recognition is used to identify a speaker's voice from among a group of known speakers. A common method of speaker recognition is a classification based on cepstral coefficients of the speaker's voice, using a Gaussian mixture model (GMM) to model each speaker. In this paper we try to fool a speaker recognition system using additive noise such that an intruder is recognized as a target user. Our attack uses a mixture selected from a target user's GMM model, inverting the cepstral transformation to produce noise samples. In our 5 speaker data base, we achieve an attack success rate of 50% with a noise signal at 10dB SNR, and 95% by increasing noise power to 0dB SNR. The importance of this attack is its simplicity and flexibility: it can be employed in real time with no processing of an attacker's voice, and little computation is needed at the moment of detection, allowing the attack to be performed by a small portable device. For any target user, knowing that user's model or voice sample is sufficient to compute the attack signal, and it is enough that the intruder plays it while he/she is uttering to be classiffed as the victim.

  4. Soil sampling kit and a method of sampling therewith

    DOEpatents

    Thompson, C.V.

    1991-02-05

    A soil sampling device and a sample containment device for containing a soil sample is disclosed. In addition, a method for taking a soil sample using the soil sampling device and soil sample containment device to minimize the loss of any volatile organic compounds contained in the soil sample prior to analysis is disclosed. The soil sampling device comprises two close fitting, longitudinal tubular members of suitable length, the inner tube having the outward end closed. With the inner closed tube withdrawn a selected distance, the outer tube can be inserted into the ground or other similar soft material to withdraw a sample of material for examination. The inner closed end tube controls the volume of the sample taken and also serves to eject the sample. The soil sample containment device has a sealing member which is adapted to attach to an analytical apparatus which analyzes the volatile organic compounds contained in the sample. The soil sampling device in combination with the soil sample containment device allows an operator to obtain a soil sample containing volatile organic compounds and minimizing the loss of the volatile organic compounds prior to analysis of the soil sample for the volatile organic compounds. 11 figures.

  5. Soil sampling kit and a method of sampling therewith

    DOEpatents

    Thompson, Cyril V.

    1991-01-01

    A soil sampling device and a sample containment device for containing a soil sample is disclosed. In addition, a method for taking a soil sample using the soil sampling device and soil sample containment device to minimize the loss of any volatile organic compounds contained in the soil sample prior to analysis is disclosed. The soil sampling device comprises two close fitting, longitudinal tubular members of suitable length, the inner tube having the outward end closed. With the inner closed tube withdrawn a selected distance, the outer tube can be inserted into the ground or other similar soft material to withdraw a sample of material for examination. The inner closed end tube controls the volume of the sample taken and also serves to eject the sample. The soil sample containment device has a sealing member which is adapted to attach to an analytical apparatus which analyzes the volatile organic compounds contained in the sample. The soil sampling device in combination with the soil sample containment device allow an operator to obtain a soil sample containing volatile organic compounds and minimizing the loss of the volatile organic compounds prior to analysis of the soil sample for the volatile organic compounds.

  6. A cost effective, sensitive, and environmentally friendly sample preparation method for determination of Polycyclic Aromatic Hydrocarbons in solid samples

    PubMed Central

    Yamaguchi, Chika; Lee, Wen-Yee

    2010-01-01

    A simple, cost effective, and yet sensitive sample preparation technique was investigated for determining polycyclic aromatic hydrocarbons (PAHs) in solid samples. The method comprises ultrasonic extraction, Stir Bar Sorptive Extraction (SBSE), and thermal desorption-gas chromatography-mass spectrometry (TD – GC/MS) to increase analytical capacity in laboratories. This method required no clean-up and satisfied PAHs recovery and significantly advances cost performance over conventional extraction methods, such as Soxhlet and Microwave Assisted Extraction (MAE). This study evaluated three operational parameters for ultrasonic extraction: solvent composition, extraction time, and sample load. A standard material, SRM 1649 a (urban dust), was used as the solid sample matrix, and 12 priority PAHs on the US Environmental Protection Agency (US EPA) list were analyzed. Combination of non-polar and polar solvents ameliorated extraction efficiency. Acetone/hexane mixtures of 2:3 and 1:1 (v/v) gave the most satisfactory results: recoveries ranged from 63.3 % to 122 %. Single composition solvents (methanol, hexane, and dichloromethane) showed fewer recoveries. Comparing 20 minutes with 60 minutes sonication, longer sonication diminished extraction efficiencies in general. Furthermore, sample load became a critical factor in certain solvent systems, such as MeOH. MAE was also compared to the ultrasonic extraction, and results determined that the 20-minutes ultrasonic extraction using acetone / hexane (2:3 v/v) was as potent as MAE. The SBSE method using 20 mL of 30 % alcohol-fortified solution rendered a limit of detection ranging from 1.7 to 32 ng L−1 and a limit of quantitation ranging from 5.8 to 110 ng L−1 for the 16 US EPA PAHs. PMID:20851399

  7. Waste classification sampling plan

    SciTech Connect

    Landsman, S.D.

    1998-05-27

    The purpose of this sampling is to explain the method used to collect and analyze data necessary to verify and/or determine the radionuclide content of the B-Cell decontamination and decommissioning waste stream so that the correct waste classification for the waste stream can be made, and to collect samples for studies of decontamination methods that could be used to remove fixed contamination present on the waste. The scope of this plan is to establish the technical basis for collecting samples and compiling quantitative data on the radioactive constituents present in waste generated during deactivation activities in B-Cell. Sampling and radioisotopic analysis will be performed on the fixed layers of contamination present on structural material and internal surfaces of process piping and tanks. In addition, dose rate measurements on existing waste material will be performed to determine the fraction of dose rate attributable to both removable and fixed contamination. Samples will also be collected to support studies of decontamination methods that are effective in removing the fixed contamination present on the waste. Sampling performed under this plan will meet criteria established in BNF-2596, Data Quality Objectives for the B-Cell Waste Stream Classification Sampling, J. M. Barnett, May 1998.

  8. An application of new microwave absorption tube in non-polar solvent microwave-assisted extraction of organophosphorus pesticides from fresh vegetable samples.

    PubMed

    Zhao, Xin; Xu, Xu; Su, Rui; Zhang, Hanqi; Wang, Ziming

    2012-03-16

    A new self-designed microwave absorption tube was used in microwave-assisted extraction of seven organophosphorus pesticides from four kinds of vegetable samples. The non-polar solvent was used as extraction solvent, and a new portable microwave extraction apparatus was used. By sealing graphite powder in glass tube, microwave absorption tube was made and used to heat samples directly. The extracts were directly analyzed by GC-MS without any clean-up process. The effects of some experimental parameters on extraction efficiency were investigated and optimized. 3.0 g of sample, 25 mL of hexane and three microwave absorption tubes were added in the microwave extraction vessel, the extraction was carried out under 425 W irradiation power at 70 °C for 8 min. The recoveries were in the range of 76.5-109.4% and the relative standard deviations were lower than 13.1%. PMID:22321952

  9. Comparison of an acetonitrile extraction/partitioning and "dispersive solid-phase extraction" method with classical multi-residue methods for the extraction of herbicide residues in barley samples.

    PubMed

    Díez, C; Traag, W A; Zommer, P; Marinero, P; Atienza, J

    2006-10-27

    An acetonitrile/partitioning extraction and "dispersive solid-phase extraction (SPE)" method that provides high quality results with a minimum number of steps and a low solvent and glassware consumption was published in 2003. This method, suitable for the analysis of multiple classes of pesticide residues in foods, has been given an acronymic name, QuEChERS, that reflects its major advantages (quick, easy, cheap, effective, rugged, safe). In this work, QuEChERS method, which was originally created for vegetable samples with a high amount of water, was modified to optimise the extraction of a wide range of herbicides in barley. Then, it was compared with known conventional multi-residue extraction procedures such as the Luke method, which was simplified and shortened by eliminating the Florisil clean-up (mini Luke) and the ethyl acetate extraction, which involves a subsequent clean-up by gel permeation chromatography (GPC) and which is the official extraction method used by some of European authorities. Finally, a simple acetone extraction was carried out to check the differences with the other three methods. Extracts were analysed by gas chromatography-time-of-flight mass spectrometry (GC-TOF/MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Mini Luke was significantly more effective for the extraction of non-polar and medium-polar compounds, but the best recoveries for polar compounds were achieved by QuEChERS and ethyl acetate methods. QuEChERS was the only method that provided an overall recovery value of 60-70% for non-, medium- and polar compounds, with some exceptions due to co-eluted matrix interferences. Clean-up by dispersive SPE was effective and did not differ so much with ethyl acetate extracts considering that QuEChERS clean-up step is much easier and less time-consuming. As a conclusion, it resulted to be the most universal extraction method by providing a well-defined phase separation without dilution and achieving acceptable

  10. Automated solid-phase extraction for the determination of polybrominated diphenyl ethers and polychlorinated biphenyls in serum--application on archived Norwegian samples from 1977 to 2003.

    PubMed

    Thomsen, Cathrine; Liane, Veronica Horpestad; Becher, Georg

    2007-02-01

    An analytical method comprised of automated solid-phase extraction and determination using gas chromatography mass spectrometry (single quadrupole) has been developed for the determination of 12 polybrominated diphenyl ethers (PBDEs), 26 polychlorinated biphenyls (PCBs), two organochlorine compounds (OCs) (hexachlorobenzene and octachlorostyrene) and two brominated phenols (pentabromophenol, and tetrabromobisphenol-A (TBBP-A)). The analytes were extracted using a sorbent of polystyrene-divinylbenzene and an additional clean-up was performed on a sulphuric acid-silica column to remove lipids. The method has been validated by spiking horse serum at five levels. The mean accuracy given as recovery relative to internal standards was 95%, 99%, 93% and 109% for the PBDEs PCBs, OCs and brominated phenols, respectively. The mean repeatability given as RSDs was respectively 6.9%, 8.7%, 7.5% and 15%. Estimated limits of detection (S/N=3) were in the range 0.2-1.8 pg/g serum for the PBDEs and phenols, and from 0.1 pg/g to 56 pg/g serum for the PCBs and OCs. The validated method has been used to investigate the levels of PBDEs and PCBs in 21 pooled serum samples from the general Norwegian population. In serum from men (age 40-50 years) the sum of seven PBDE congeners (IUPAC No. 28, 47, 99, 100, 153, 154 and 183) increased from 1977 (0.5 ng/g lipids) to 1998 (4.8 ng/g lipids). From 1999 to 2003 the concentration of PBDEs seems to have stabilised. On the other hand, the sum of five PCBs (IUPAC No. 101, 118, 138, 153 and 180) in these samples decreased steadily from 1977 (666 ng/g lipids) to 2003 (176 ng/g lipids). Tetrabromobisphenol-A and BDE-209 were detected in almost all samples, but no similar temporal trends to that seen for the PBDEs were observed for these compounds, which might be due to the short half-lives of these brominated flame retardants (FR) in humans. PMID:17023223

  11. Preparation of environmental samples for the determination of polycyclic aromatic hydrocarbons by thin-layer chromatography.

    PubMed

    Poole, S K; Dean, T A; Poole, C F

    1987-07-29

    An evaluation of extraction procedures, liquid-liquid distribution systems, Sep-Pak cartridges, liquid-solid chromatography using silica, alumina and chemically modified silica packings (acid-base treated ethylammonium nitrate and picric acid impregnated), macroreticular resins and gel permeation columns for the analysis of polycyclic aromatic hydrocarbons (CPAHs) in environmental samples by thin-layer chromatography is discussed. For particulate samples solvent extraction using a Soxhlet apparatus or ultrasonication was found to be preferable to sublimation and liquid-liquid distribution between hexane and dimethyl sulfoxide followed by silica gel column chromatography was the preferred method for sample clean-up. Using this procedure enabled six PAHs (anthracene, fluoranthene, benz[a]anthracene, perylene, pyrene, and coronene) to be determined quantitatively in urban air particulate, diesel engine exhaust particulate, laboratory ventilator dust, household dust, river water, and tea samples. The PAHs were identified by coincidence of retention between the sample and standards in the same chromatographic system and by adequate agreement with standards for their normalized emission response ratios. The two-point calibration method was used for quantitation. Good agreement for the concentration of PAHs in the air particulate and diesel particulate extracts with published data using gas chromatography-mass spectrometry and high-performance liquid chromatography was found. PMID:2444609

  12. Analytical methods for the determination of personal care products in human samples: an overview.

    PubMed

    Jiménez-Díaz, I; Zafra-Gómez, A; Ballesteros, O; Navalón, A

    2014-11-01

    Personal care products (PCPs) are organic chemicals widely used in everyday human life. Nowadays, preservatives, UV-filters, antimicrobials and musk fragrances are widely used PCPs. Different studies have shown that some of these compounds can cause adverse health effects, such as genotoxicity, which could even lead to mutagenic or carcinogenic effects, or estrogenicity because of their endocrine disruption activity. Due to the absence of official monitoring protocols, there is an increasing demand of analytical methods that allow the determination of those compounds in human samples in order to obtain more information regarding their behavior and fate in the human body. The complexity of the biological matrices and the low concentration levels of these compounds make necessary the use of advanced sample treatment procedures that afford both, sample clean-up, to remove potentially interfering matrix components, as well as the concentration of analytes. In the present work, a review of the more recent analytical methods published in the scientific literature for the determination of PCPs in human fluids and tissue samples, is presented. The work focused on sample preparation and the analytical techniques employed. PMID:25127618

  13. Optimisation of sample treatment for arsenic speciation in alga samples by focussed sonication and ultrafiltration.

    PubMed

    Salgado, S García; Quijano Nieto, M A; Bonilla Simón, M M

    2006-02-28

    A procedure for arsenic species fractionation in alga samples (Sargassum fulvellum, Chlorella vulgaris, Hizikia fusiformis and Laminaria digitata) by extraction is described. Several parameters were tested in order to evaluate the extraction efficiency of the process: extraction medium, nature and concentration (tris(hydroxymethyl)aminomethane, phosphoric acid, deionised water and water/methanol mixtures), extraction time and physical treatment (magnetic stirring, ultrasonic bath and ultrasonic focussed probe). The extraction yield of arsenic under the different conditions was evaluated by determining the total arsenic content in the extracts by ICP-AES. Arsenic compounds were extracted in 5mL of water by focussed sonication for 30s and subsequent centrifugation at 14,000xg for 10min. The process was repeated three times. Extraction studies show that soluble arsenic compounds account for about 65% of total arsenic. An ultrafiltration process was used as a clean-up method for chromatographic analysis, and also allowed us to determine the extracted arsenic fraction with a molecular weight lower than 10kDa, which accounts for about 100% for all samples analysed. Speciation studies were carried out by HPLC-ICP-AES. Arsenic species were separated on a Hamilton PRP-X100 column with 17mM phosphate buffer at pH 5.5 and 1.0mLmin(-1) flow rate. The chromatographic method allowed us to separate the species As(III), As(V), MMA and DMA in less than 13min, with detection limits of about 20ng of arsenic per species, for a sample injection volume of 100muL. The chromatographic analysis allowed us to identify As(V) in Hizikia (46+/-2mugg(-1)), Sargassum (38+/-2mugg(-1)) and Chlorella (9+/-1mugg(-1)) samples. The species DMA was also found in Chlorella alga (13+/-1mugg(-1)). However, in Laminaria alga only an unknown arsenic species was detected, which eluted in the dead volume. PMID:18970494

  14. Attention samples stimuli rhythmically.

    PubMed

    Landau, Ayelet Nina; Fries, Pascal

    2012-06-01

    Overt exploration or sampling behaviors, such as whisking, sniffing, and saccadic eye movements, are often characterized by a rhythm. In addition, the electrophysiologically recorded theta or alpha phase predicts global detection performance. These two observations raise the intriguing possibility that covert selective attention samples from multiple stimuli rhythmically. To investigate this possibility, we measured change detection performance on two simultaneously presented stimuli, after resetting attention to one of them. After a reset flash at one stimulus location, detection performance fluctuated rhythmically. When the flash was presented in the right visual field, a 4 Hz rhythm was directly visible in the time courses of behavioral performance at both stimulus locations, and the two rhythms were in antiphase. A left visual field flash exerted only partial reset on performance and induced rhythmic fluctuation at higher frequencies (6-10 Hz). These findings show that selective attention samples multiple stimuli rhythmically, and they position spatial attention within the family of exploration behaviors. PMID:22633805

  15. Evaluation of a sampling and analysis method for determination of polyhalogenated dibenzo-p-dioxins and dibenzofurans in ambient air

    SciTech Connect

    Harless, R.L.; Lewis, R.G.; McDaniel, D.D.; Gibson, J.F.; Dupuy, A.E.

    1991-01-01

    General Metals Works PS-1 PUF air samplers and an analytical method based on high resolution gas chromatography - high resolution mass spectrometry (HRGC-HRMS) were evaluated for determination of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDDs/PCDFs), polybrominated dibenzo-p-dioxins and dibenzofurans (PBDDs/PBDFs) and bromo/chloro dibenzo-p-dioxins and dibenzofurans (BCDDs/BCDFs) in ambient air. Dilute solutions of these compounds and (13)C12-1,2,3,4-TCDD were used to spike the filters of PS-1 air samplers which were then operated 24 hrs to sample 350-400 cu m ambient air. After sampling, each quartz-fiber filter and polyurethane foam (PUF) were spiked with (13)C12-labeled PCDD, PCDF, PBDD, and PBDF internal standards before separate Soxhlet extractions with benzene. The extracts were subjected to an acid/base clean-up procedure followed by clean-up on microcolumns of silica gel, alumina, and carbon and then analyzed by HRGC-HRMS. Results derived from the study indicated the PS-1 ambient air samplers and the analytical procedures were very efficient and that pg/cu m and sub-pg/cu m levels of total PCDDs/PCDFs, PBDDs/PBDFs, BCDDs/BCDFs, and 2,3,7,8-substituted congeners could be accurately measured. Background levels of these compounds in the ambient air were also determined. Total PCDDs, PCDFs, TBDFs, and PeBDFs were detected in a low concentration range of 0.3 to 3.0 pg/cu m.

  16. Acid Rain Analysis by Standard Addition Titration.

    ERIC Educational Resources Information Center

    Ophardt, Charles E.

    1985-01-01

    The standard addition titration is a precise and rapid method for the determination of the acidity in rain or snow samples. The method requires use of a standard buret, a pH meter, and Gran's plot to determine the equivalence point. Experimental procedures used and typical results obtained are presented. (JN)

  17. Evaluation and validation of the use of a molecularly imprinted polymer coupled to LC-MS for benzylpenicillin determination in meat samples.

    PubMed

    Van Royen, Geert; Dubruel, Peter; Van Weyenberg, Stephanie; Daeseleire, Els

    2016-07-01

    This article describes a full analytical method for the clean-up and detection of benzylpenicillin in chicken and beef meat samples using a previously developed molecularly imprinted polymer in a solid-phase extraction cleanup step followed by analysis using LC-MS/MS. The method was validated based on the criteria and the requirements of the European Commission Decision 2002/657/EC. This validation revealed method performance characteristics that meet all the criteria in the Decision with limits of detection for chicken and beef meat samples of 6.2 and 14.4μg/kg, respectively, 8 and 3.5 times lower than the MRL. This method holds strong potential when a specific cleanup of benzylpenicillin is required, because with slight modifications it is also applicable in a milk matrix [1]. PMID:27209268

  18. Determination of five nitroimidazole residues in artificial porcine muscle tissue samples by capillary electrophoresis.

    PubMed

    Lin, Yingyun; Su, Yan; Liao, Xiulin; Yang, Na; Yang, Xiupei; Choi, Martin M F

    2012-01-15

    A capillary electrophoresis (CE) method with ultraviolet detection has been developed for simultaneous detection and quantification of five nitroimidazoles including benzoylmetronidazole, dimetridazole, metronidazole, ronidazole, and secnidazole in porcine muscles. Nitroimidazoles in samples were extracted by ethyl acetate with subsequent clean-up by a strong cation exchange solid phase extraction column. The clean extracts were subjected to CE separation with optimal experimental conditions: pH 3.0 running buffer containing 25mM sodium phosphate and 0.10mM tetrabutylammonium bromide, 5s hydrodynamic injection at 0.5psi and 28kV separation voltage. The nitroimidazoles could be monitored and detected at 320nm within 18min. The limits of detection were below 1.0μg/kg and limits of quantification were lower than 3.2μg/kg for all nitroimidazoles in the muscle samples. The recoveries and relative standard deviations were 85.4-96.0, 83.5-92.5, 1.3-3.9, and 1.1-4.2%, respectively for the intra-day and inter-day analyses. The proposed CE method has been successfully applied to determine nitroimidazoles in artificial porcine muscle samples with good accuracy and recovery, demonstrating that it has potential for detection and quantification of multi-nitroimidazole residue in real muscle samples. PMID:22265553

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

    PubMed

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

    2015-01-01

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

  20. Aflatoxin M1 contamination in commercial samples of milk and dairy products in Kuwait.

    PubMed

    Srivastava, V P; Bu-Abbas, A; Alaa-Basuny; Al-Johar, W; Al-Mufti, S; Siddiqui, M K

    2001-11-01

    As part of the programme on monitoring of environmental contaminants in food stuff in Kuwait, 54 samples of fresh full cream and skimmed milk, powdered milk, yoghurt, and infant formula were analysed for aflatoxin M1 (AFM1) by HPLC following sample clean up using immuno-affinity columns. Of samples, 28% were contaminated with AFM1 with 6% being above the maximum permissible limit of 0.2 microgl(-1). Three fresh cow milk samples collected from a private local producer showed the highest level of 0.21 microg l(-1) AFM1. There was no contamination with AFM1 in powdered milk and infant formulas. These results show the necessity of a survey involving a larger number of milk and its products and suggest that presently the contamination of milk and milk products with AFM1 does not appear to be a serious health problem in Kuwait. Nevertheless, a continuous surveillance programme may be warranted to monitor regularly the occurrence of aflatoxins in the animal feeds responsible for current limited contamination and to note rapidly and worsening in the situation that may depend on market changes or on unfavourable climatic developments. PMID:11665741