A validated method for rapid determination of dibenzo-p-dioxins/furans (PCDD/Fs), polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in human milk: focus on utility of tandem solid phase extraction (SPE) cleanup.

PubMed

Lin, Yuanjie; Feng, Chao; Xu, Qian; Lu, Dasheng; Qiu, Xinlei; Jin, Yu'e; Wang, Guoquan; Wang, Dongli; She, Jianwen; Zhou, Zhijun

2016-07-01

An improved method based on tandem solid phase extraction (SPE) cleanup and gas chromatography-high resolution mass spectrometry (GC-HRMS) has been validated for a rapid determination of dibenzo-p-dioxins/furans (PCDD/Fs), dioxin-like polychlorinated biphenyls (PCBs), marker polychlorinated biphenyls (M-PCBs), and polybrominated diphenyl ethers (PBDEs) using a large volume (50 mL) of human milk. This method was well validated for the measurement of these analytes in human milk from the general population with low limits of detection (LODs, 0.004-0.12 ng/g lipid), satisfactory accuracy (75-120 % of recoveries), and precision [less than 10 % of relative standard deviations (RSDs)]. To comprehensively evaluate the performance of this method, a good, presently validated and routinely used method based on an automated sample clean-up system (ASCS, based on the commercial acid multilayer silica, basic alumina, and carbon columns) was used in parallel for comparison. Compared with the ASCS method, this method presented comparable specificity. Additionally, this method, in contrast to ASCS method, highly reduced consumption of solvents (40 mL versus 500 mL), which results in much lower background in the procedural blank, reduced time, and enhanced sample pretreatment throughput. This method was also applied in a pilot study to measure a batch of human milk samples with satisfactory results. Graphical Abstract Characteristics of the application of tandem SPE cleanup for determination of PCDD/Fs, DL-PCBs,M-PCBs and PBDEs in human milk.

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

PubMed

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

2013-05-07

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

Determination of chloramphenicol and zeranols in pig muscle by immunoaffinity column clean-up and LC-MS/MS analysis.

PubMed

Wang, Qing; Zhao, Hua; Xi, Cunxian; Wang, Guomin; Chen, Dongdong; Ding, Shijia

2014-01-01

An immunoaffinity column clean-up and LC-MS/MS method was successfully developed for simultaneous determination of chloramphenicol, zearalanone, α-zearalanol, β-zearalanol, zearalenone, α-zearalenol and β-zearalenol in pig muscle. The sample was extracted with diethyl ether after enzymatic digestion by β-glucuronidase/sulfatase. The extracted solution was evaporated to dryness and the residue was then dissolved in 1 ml of 50% acetonitrile solution. After filtration and dilution with phosphate buffer solution (PBS), the reconstituted solution was cleaned-up with an IAC-CZ immunoaffinity column and then analysed by HPLC-MS/MS. The established method were validated by linearity (r ≥ 0.9990), precision (RSD ≥ 2.9%), average recovery (74.5-105.0%) and limit of detection (0.04-0.10 μg kg(-1)). The developed method is rapid, reliable, sensitive, accurate and has good applicability for real samples.

Ultrasonication extraction and gel permeation chromatography clean-up for the determination of polycyclic aromatic hydrocarbons in edible oil by an isotope dilution gas chromatography–mass spectrometry.

PubMed

Wang, Jian-Hua; Guo, Cui

2010-07-09

An analytical method for the determination of US EPA priority pollutant 16 polycyclic aromatic hydrocarbons (PAHs) in edible oil was developed by an isotope dilution gas chromatography-mass spectrometry (GC-MS). Extraction was performed with ultrasonication mode using acetonitrile as solvent, and subsequent clean-up was applied using narrow gel permeation chromatographic column. Three deuterated PAHs surrogate standards were used as internal standards for quantification and analytical quality control. The limits of quantification (LOQs) were globally below 0.5 ng/g, the recoveries were in the range of 81-96%, and the relative standard deviations (RSDs) were lower than 20%. Further trueness assessment of the method was also verified through participation in international cocoa butter proficiency test (T0638) organised by the FAPAS with excellent results in 2008. The results obtained with the described method were satisfying (z ≤ 2). The method has been applied to determine PAH in real edible oil samples.

Determination of the effect of formation water on fracture-fluid cleanup

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

NONE

1998-03-01

Understanding hydraulic-fracture cleanup is essential for improving well stimulation. Residual gel damages fracture conductivity, shortens effective fracture half-length, and limits well productivity. The drive to develop fluids, additives, and procedures that minimize this damage continues to be a dominant theme in fracture-fluid-development programs. Fracture cleanup is a complex problem, and many parameters (e.g., fluid system, job design, flowback procedure, and reservoir conditions) can influence polymer and fluid recovery efficiencies. Often, specific products and methods that work well in one reservoir have little effect in another. Systematic analysis of fluid and polymer returns after a treatment is completed is the onlymore » way to quantify fracture cleanup. This is referred to as flowback analysis. This paper discusses a flowback-analysis field study on large hydraulic-fracturing treatments in the Taylor zone of the Cotton Valley formation in east Texas. This is a low-permeability (approximately 0.01 md) tight gas formation. It is a heterogeneous zone with layers of productive sandstone interspersed with relatively impermeable layers of shale. A typical well in this field initially produces approximately 0.75 to 1.3 MMcf/D gas and 35 to 40 bbl of water/MMcf of gas. The returns from 10 wells in this field were analyzed thoroughly.« less

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

PubMed

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

2013-01-01

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

Intergenerational equity and environmental restoration cleanup levels.

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

Hocking, E. K.; Environmental Assessment

2001-01-01

The United States Department of Energy environmental restoration program faces difficult decisions about the levels of cleanup to be achieved at its many contaminated sites and has acknowledged the need for considering intergenerational equity in its decision making. Intergenerational equity refers to the fairness of access to resources across generations. Environmental restoration cleanup levels can have unintended and unfair consequences for future generations access to resources. The potentially higher costs associated with using low, non-risk-based cleanup levels for remediation may divert funding from other activities that could have a greater beneficial impact on future generations. Low, non-risk-based cleanup levels couldmore » also result in more damage to the nation's resources than would occur if a higher cleanup level were used. The loss or impairment of these resources could have an inequitable effect on future generations. However, intergenerational inequity could arise if sites are not completely restored and if access to and use of natural and cultural resources are unfairly limited as a result of residual contamination. In addition to concerns about creating possible intergenerational inequities related to selected cleanup levels, the tremendous uncertainties associated with sites and their restoration can lead site planners to rely on stewardship by default. An ill-conceived stewardship program can contribute to intergenerational inequity by limiting access to resources while passing on risks to future generations and not preparing them for those risks. This paper presents a basic model and process for designing stewardship programs that can achieve equity among generations.« less

Report: Some States Cannot Address Assessment Needs and Face Limitations in Meeting Future Superfund Cleanup Requirements

EPA Pesticide Factsheets

Report #2004-P-00027, September 1, 2004. The five States have established hazardous waste site cleanup programs that address contaminated sites posing human health and environmental risks ranging from low to high.

Plutonium mining for cleanup.

PubMed

Bramlitt, E T

1988-08-01

Cleanup is the act of making a contaminated site relatively free of Pu so it may be used without radiological safety restrictions. Contaminated ground is the focus of major cleanups. Cleanup traditionally involves determining Pu content of soil, digging up soil in which radioactivity exceeds guidelines, and relocating excised soil to a waste-disposal site. Alternative technologies have been tested at Johnston Atoll (JA), where there is as much as 100,000 m3 of Pu-contaminated soil. A mining pilot plant operated for the first 6 mo of 1986 and made 98% of soil tested "clean", from more than 40 kBq kg-1 (1000 pCi g-1) to less than about 500 Bq kg-1 (15 pCi g-1) by concentrating Pu in 2% of the soil. The pilot plant is now installed at the U.S. Department of Energy Nevada Test Site for evaluating cleanup of other contaminated soils and refining cleanup effectiveness. A full-scale cleanup plant has been programmed for JA in 1988. In this paper, previous cleanups are reviewed, and the mining endeavor at JA is detailed. "True soil cleanup" is contrasted with the classical "soil relocation cleanup." The mining technology used for Pu cleanup has been in use for more than a century. Mining for cleanup, however, is unique. It is envisioned as being prominent for radiological and other cleanups in the future.

Enrichment and low-level determination of glyphosate, aminomethylphosphonic acid and glufosinate in drinking water after cleanup by cation exchange resin.

PubMed

Küsters, Markus; Gerhartz, Michael

2010-04-01

For the determination of glyphosate, aminomethylphosphonic acid and glufosinate in drinking water, different procedures of enrichment and cleanup were examined using anion exchange or SPE. In many cases interactions of, e.g. alkaline earth metal ions especially calcium could be observed during enrichment and cleanup resulting in loss of analytes. For that reason, a novel cleanup and enrichment procedure for the determination of these phosphonic acid herbicides has been developed in drinking water using cation-exchange resin. In summary, the cleanup procedure with cation-exchange resin developed in this study avoids interactions as described above and is applicable to calcium-rich drinking water samples. After derivatization with 9-fluorenylmethylchloroformate followed by LC with fluorescence detection, LOD of 12, 14 and 12 ng/L and mean recoveries from real-world drinking water samples of 98+/-9, 100+/-16 and 101+/-11% were obtained for glyphosate, aminomethylphosphonic acid and glufosinate, respectively. The low LODs and the high precision permit the analysis of these phosphonic acid herbicides according to the guidelines of the European Commission.

Comparison of pulse glow discharge-ion mobility spectrometry and liquid chromatography with tandem mass spectrometry based on multiplug filtration cleanup for the analysis of tricaine mesylate residues in fish and water.

PubMed

Zou, Nan; Chen, Ronghua; Qin, Yuhong; Song, Shuangyu; Tang, Xinglin; Pan, Canping

2016-09-01

Analytical methods based on multiplug filtration cleanup coupled with pulse glow discharge-ion mobility spectrometry and liquid chromatography tandem mass spectrometry were developed for the analysis of tricaine mesylate residue in fish and fish-raising water samples. A silica fiber holder and an appropriate new interface were designed to make the direct introduction of the fiber into the pulse glow discharge-ion mobility spectrometry introduction mechanism. The multiplug filtration cleanup method with adsorption mixtures was optimized for the determination of tricaine mesylate in fish samples. Good linear relationships were obtained by the two methods. For fish samples, limits of detection were 6 and 0.6 μg/kg by ion mobility spectrometry and liquid chromatography with tandem mass spectrometry, respectively. The matrix effect of the established liquid chromatography tandem mass spectrometry method was negligible for fish samples but that of the ion mobility spectrometry method was not. The two methods were compared. The ion mobility spectrometry system could be used a rapid screening tool on site with the advantage of rapidity, simplicity, and portability, and the liquid chromatography tandem mass spectrometry system could be used for validation in laboratory conditions with the advantage of lower limit of detection, stability, and precision. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-Throughput Analytical Techniques for Determination of Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea--Part V: A Comparative Study of the Influence of Tea Hydration on the Efficiency of Pesticide Multiresidue Determination Using Three Sample Preparation Methods and GC/MS/MS.

PubMed

Chen, Xi; Li, Yan; Chang, Qiao-Ying; Hu, Xue-Yan; Pang, Guo-Fang; Fan, Chun-Lin

2015-01-01

This paper describes a comparative study of the influence of three sample preparation techniques (M1: hydration+oscillating extraction+partial extraction solution hexane partitioning cleanup; M2: hydration+oscillating extraction+overall extraction solution SPE cleanup; and M3: pure acetonitrile homogeneous extraction+overall extraction SPE cleanup) on the determination efficiency of 456 pesticide multiresidues in tea. First, it was discovered from the mathematical correlation equation of 329 pesticide recoveries established and log Kow values that the extraction efficiency of hydration method M1 has obvious correlation with pesticide log Kow, making the extraction efficiency of M1 take the shape of an arc trend line with a certain arc hanging down from both ends of polar pesticides and nonpolar pesticides. Second, regarding the M1 method, the interfering matter after co-extraction increased in large quantities, which markedly lowered the S/N of the target pesticides and method sensitivity, leading to an obvious decrease of the method efficiency. The fortification experiment of the uniform limit 0.010 mg/kg proved that with the M1 hydration method there are 23 pesticides with recoveries between 70 and 120% and RSD<20%, accounting for only 5.0%, while with nonhydration method M3 there are 229 pesticides, making up 50%.

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. Copyright © 2016 Elsevier Ltd. All rights reserved.

Influence of pre-treatment process on matrix effect for the determination of musk fragrances in fish and mussel.

PubMed

Vallecillos, Laura; Pocurull, Eva; Borrull, Francesc

2015-03-01

Musk compounds are widely used as fragrances in personal care products. On account of their widespread use and their low biodegradation, they can be found in environmental samples. In our study two extraction methodologies were compared and different clean-up strategies were also studied in order to develop a reliable analytical method, with minimum matrix effect and good detection limits, to determine synthetic musk fragrances- six polycyclic musks, three nitro musks and the degradation product of one polycyclic musk- in fish and mussel samples. The first extraction technique involves a QuEChERS extraction, a consolidate extraction methodology in the field of food analysis of growing interest over recent years, followed by a dispersive solid-phase extraction (dSPE) as clean-up strategy. The second extraction technique consists of a conventional pressurised liquid extraction (PLE) with dichloromethane and an in-cell clean-up to decrease the matrix effect and remove the undesired components(⁎)present in PLE extracts. Large volume injection (LVI) followed by gas chromatography-ion trap-tandem mass spectrometry (GC-IT-MS/MS) was chosen as the separation and detection technique. Validation parameters, such as method detection limits and method quantification limits were found at ng g(-1) levels for both fish and mussel matrices. Good levels of intra-day and inter-day repeatabilities were obtained analysing fish and mussel samples spiked at 50 ng g(-1) (d.w.) (n=5, RSDs<17%). The developed PLE/GC-IT-MS/MS method was successfully applied to determine the target musk fragrances present in fish and mussel samples from the local market in Tarragona and fish samples from the Ebro River. The results showed the presence of galaxolide (2.97-18.04 ng g(-1) (d.w.)) and tonalide (1.17-8.42 ng g(-1) (d.w.)) in all the samples analysed, while the remaining polycyclic musks such as cashmeran, celestolide and phantolide, were only detected in some of the fish samples analysed. None of the samples analysed contained detectable traces of the nitro musks studied. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of pesticides associated with suspended sediments in the San Joaquin River, California, USA, using gas chromatography-ion trap mass spectrometry

USGS Publications Warehouse

Bergamaschi, B.A.; Baston, D.S.; Crepeau, K.L.; Kuivila, K.M.

1999-01-01

An analytical method useful for the quantification of a range of pesticides and pesticide degradation products associated with suspended sediments was developed by testing a variety of extraction and cleanup schemes. The final extraction and cleanup methods chosen for use are suitable for the quantification of the listed pesticides using gas chromatography-ion trap mass spectrometry and the removal of interfering coextractable organic material found in suspended sediments. Methylene chloride extraction followed by Florisil cleanup proved most effective for separation of coextractives from the pesticide analytes. Removal of elemental sulfur was accomplished with tetrabutylammonium hydrogen sulfite. The suitability of the method for the analysis of a variety of pesticides was evaluated, and the method detection limits (MDLs) were determined (0.1-6.0 ng/g dry weight of sediment) for 21 compounds. Recovery of pesticides dried onto natural sediments averaged 63%. Analysis of duplicate San Joaquin River suspended-sediment samples demonstrated the utility of the method for environmental samples with variability between replicate analyses lower than between environmental samples. Eight of 21 pesticides measured were observed at concentrations ranging from the MDL to more than 80 ng/g dry weight of sediment and exhibited significant temporal variability. Sediment-associated pesticides, therefore, may contribute to the transport of pesticides through aquatic systems and should be studied separately from dissolved pesticides.

A Rapid Method for the Quantitative Determination of 34 Pesticides in Nonalcoholic Carbonated Beverages Using Liquid-Liquid Extraction Coupled to Dispersive Solid-Phase Cleanup Followed by Gas Chromatography with Tandem Mass Spectrometry.

PubMed

Rai, Satyajeet; Gullapalli, Madhuri Devi; Srivastava, Anshuman; Shaik, Hussain; Siddiqui, Mohammed Haris; Mudiam, Mohana Krishna Reddy

2017-05-01

An economical, rapid, and sensitive multiresidue method using liquid-liquid extraction (LLE) coupled with dispersive SPE (dSPE) cleanup was developed for the quantitative determination of 34 multiclass multiresidue (MCMR) pesticides (14 organochlorines, eight organophosphates, 10 synthetic pyrethroids, and two herbicides) in nonalcoholic carbonated beverages (cola, orange, lemon-lime, and citra) using GC with tandem MS. The procedure mainly involved LLE by dichloromethane and dSPE cleanup in the presence of magnesium sulfate, primary secondary amine, and C18. The RSD of the developed method was found to be less than 14%. The LOD and LOQ values for all the analyzed pesticides were found in the ranges of 0.001-0.027 μg/L and 0.004-0.088 μg/L, respectively. The LOQ levels of the pesticides analyzed were found to be well below the recommended limit by the European Union (0.1 μg/L in water). The mean recoveries of pesticides in different nonalcoholic carbonated beverages (cola, orange, lemon-lime, and citra) were found to be in the range of 79-111%, with RSDs less than 11%. The validation data prove that the method can be acceptable to regulatory agencies for the routine analysis of MCMR pesticides in nonalcoholic carbonated beverages.

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

Not Available

This interim notice covers the following: extractable organic halides in solids, total organic halides, analysis by gas chromatography/Fourier transform-infrared spectroscopy, hexadecane extracts for volatile organic compounds, GC/MS analysis of VOCs, GC/MS analysis of methanol extracts of cryogenic vapor samples, screening of semivolatile organic extracts, GPC cleanup for semivolatiles, sample preparation for GC/MS for semi-VOCs, analysis for pesticides/PCBs by GC with electron capture detection, sample preparation for pesticides/PCBs in water and soil sediment, report preparation, Florisil column cleanup for pesticide/PCBs, silica gel and acid-base partition cleanup of samples for semi-VOCs, concentrate acid wash cleanup, carbon determination in solids using Coulometrics` CO{submore » 2} coulometer, determination of total carbon/total organic carbon/total inorganic carbon in radioactive liquids/soils/sludges by hot persulfate method, analysis of solids for carbonates using Coulometrics` Model 5011 coulometer, and soxhlet extraction.« less

Simple and sensitive determination of five quinolones in food by liquid chromatography with fluorescence detection.

PubMed

Ramos, Macarena; Aranda, Angela; Garcia, Elena; Reuvers, Thea; Hooghuis, Henny

2003-06-15

A simple and sensitive high-performance liquid chromatographic (HPLC) method has been developed for the determination of five different quinolones: enrofloxacin, ciprofloxacin, sarafloxacin, oxolinic acid and flumequine in pork and salmon muscle. The method includes one extraction and clean-up step for the five quinolones together which are detected in two separated HPLC runs by means of their fluorescence. The proposed analytical method involves homogenizing of the tissue sample with 0.05 M phosphate buffer, pH 7.4 and clean-up by Discovery DS-18 cartridges. For chromatographic separation a Symmetry C(18) column is used in two different runs: (1) ciprofloxacin, enrofloxacin and sarafloxacin with acetonitrile-0.02 M phosphate buffer pH 3.0 (18:82) as mobile phase and the detector at excitation wavelength: 280 nm and emission wavelength 450 nm; and (2) oxolinic acid and flumequine with acetonitrile-0.02 M phosphate buffer pH 3.0 (34:66) as mobile phase and excitation wavelength: 312 nm and emission wavelength: 366 nm. Detection limit was as low as 5 ng g(-1), except for sarafloxacin which had a limit of 10 ng g(-1). Standard curves using blank muscle tissues spiked at different levels showed a good linear correlation coefficient, r(2) higher than 0.999 for all quinolones.

Sticky foam as a less-than-lethal technology

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

Scott, S.H.

1996-12-31

Sandia National Labs (SNL) in 1994 completed a project funded by the National Institute of Justice (NIJ) to determine the applicability of sticky foam for correctional applications. Sticky foam is an extremely tacky, tenacious material used to block, entangle, and impair individuals. The NIJ project developed a gun capable of firing multiple shots of sticky foam, tested the gun and sticky foam effectiveness on SNL volunteers acting out prison and law enforcement scenarios, and had the gun and sticky foam evaluated by correctional representatives. Based on the NIJ project work, SNL supported the Marine Corps Mission, Operation United Shield, withmore » sticky foam guns and supporting equipment to assist in the withdrawal of UN Peacekeepers from Somalia. Prior to the loan of the equipment, the Marines were given training in sticky foam characterization, toxicology, safety issues, cleanup and waste disposal, use limitations, use protocol and precautions, emergency facial clean-up, skin cleanup, gun filling, targeting and firing, and gun cleaning. The Marine Corps successfully used the sticky foam guns as part of that operation. This paper describes these recent developments of sticky foam for non-lethal uses and some of the lessons learned from scenario and application testing.« less

Determination of 255 pesticides in edible vegetable oils using QuEChERS method and gas chromatography tandem mass spectrometry.

PubMed

He, Zeying; Wang, Yuehua; Wang, Lu; Peng, Yi; Wang, Wenwen; Liu, Xiaowei

2017-02-01

In this study, a simple and high-throughput method for determination of 255 pesticides in vegetable oils was developed based on QuEChERS sample preparation method combined with gas chromatography-triple quadrupole mass spectrometry. Different clean-up approaches were tested: A, 150 mg PSA + 150 mg C18; B, 250 mg PSA + 250 mg C18; C, 250 mg PSA + 250 mg C18 + 15 mg GCB; D, 250 mg PSA + 250 mg C18 + 50 mg GCB; and E, EMR-Lipid TM . Best clean-up capacity was observed for EMR clean-up. The extraction procedures and parameters, including extraction time, solvent/sample ratio, and buffer system, were also thoroughly investigated and optimized. The limits of quantification (LOQ) ranged between 5 and 50 μg kg -1 , and for the majority of the pesticides the LOQs were 5 μg kg -1 , which were below the regulatory MRLs. Most recoveries at seven spiking levels were in the range of 70-120 % with RSDs <20 % indicating satisfactory accuracy. The coefficient of determination (r 2 ) was >0.99 within the calibration linearity range of 2-500 μg L -1 for the majority of the pesticides. This method was proved to be simple, sensitive, and effective, which can be applied for large-scale pesticide screening and quantification in vegetable oils.

Quantitation of acrylamide in foods by high-resolution mass spectrometry.

PubMed

Troise, Antonio Dario; Fiore, Alberto; Fogliano, Vincenzo

2014-01-08

Acrylamide detection still represents one of the hottest topics in food chemistry. Solid phase cleanup coupled to liquid chromatography separation and tandem mass spectrometry detection along with GC-MS detection are nowadays the gold standard procedure for acrylamide quantitation thanks to high reproducibility, good recovery, and low relative standard deviation. High-resolution mass spectrometry (HRMS) is particularly suitable for the detection of low molecular weight amides, and it can provide some analytical advantages over other MS techniques. In this paper a liquid chromatography (LC) method for acrylamide determination using HRMS detection was developed and compared to LC coupled to tandem mass spectrometry. The procedure applied a simplified extraction, no cleanup steps, and a 4 min chromatography. It proved to be solid and robust with an acrylamide mass accuracy of 0.7 ppm, a limit of detection of 2.65 ppb, and a limit of quantitation of 5 ppb. The method was tested on four acrylamide-containing foods: cookies, French fries, ground coffee, and brewed coffee. Results were perfectly in line with those obtained by LC-MS/MS.

Determination of the cyanobacterial toxin cylindrospermopsin in algal food supplements.

PubMed

Liu, H; Scott, P M

2011-06-01

For the analysis of blue-green algal food supplements for cylindrospermopsin (CYN), a C18 solid-phase extraction column and a polygraphitized carbon solid-phase extraction column in series was an effective procedure for the clean-up of extracts. Determination of CYN was by liquid chromatography with ultraviolet light detection. At extract spiking levels of CYN equivalent to 25-500 µg g(-1), blue-green algal supplement recoveries were in the range 70-90%. CYN was not detected in ten samples of food supplements and one chocolate product, all containing blue-green algae. The limit of detection for the method was 16 µg g(-1), and the limit of quantification was 52 µg g(-1).

[Immunoaffinity columns and determination of ochratoxin A in cereals by HPLC. Part I.: Evaluation of extraction using methanol/water].

PubMed

Czerwiecki, Ludwik; Czyzyk, Kamila; Kwiecień, Agnieszka; Wilczyńska, Grazyna

2004-01-01

The method for ochratoxin A determination in cereals (wheat, rye) was described. Application of immunoaffinity columns (IAC) for clean-up of extracts was investigated. The ochratoxin A content was determined by high-performance liquid chromatography using C18 column and fluorimetric detection at 330 nm (excitation) and 460 nm (emission). The mean recovery of ochratoxin A was 65-78%. The limits of detection (LOD) and quantification (LOQ) were 0.015 and 0.025 microg/kg, respectively. The positive results were confirmed by reaction with BF3 complex in methanol.

DEVELOPMENT AND APPLICATION OF IMMUNOAFFINITY COLUMN CHROMATOGRAPHY AS A CLEANUP METHOD FOR THE DETERMINATION OF ATRAZINE IN COMPLEX ENVIRONMENTAL SAMPLE MEDIA

EPA Science Inventory

A rabbit antibody immunoaffinity (IA) column procedure was evaluated as a cleanup method for the determination of atrazine in soil, sediment, and food. Four IA columns were prepared by immobilizing a polyclonal rabbit anti-atrazine antibody solution to HiTrap Sepharose columns. A...

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

Ochratoxin A in cocoa and chocolate sampled in Canada.

PubMed

Turcotte, A-M; Scott, P M

2011-06-01

In order to determine the levels of ochratoxin A (OTA) in cocoa and cocoa products available in Canada, a previously published analytical method, with minor modifications to the extraction and immunoaffinity clean-up and inclusion of an evaporation step, was initially used (Method I). To improve the low method recoveries (46-61%), 40% methanol was then included in the aqueous sodium bicarbonate extraction solvent (pH 7.8) (Method II). Clean-up was on an Ochratest™ immunoaffinity column and OTA was determined by liquid chromatography (LC) with fluorescence detection. Recoveries of OTA from spiked cocoa powder (0.5 and 5 ng g(-1)) were 75-84%; while recoveries from chocolate were 93-94%. The optimized method was sensitive (limit of quantification (LOQ) = 0.07-0.08 ng g(-1)), accurate (recovery = 75-94%) and precise (coefficient of variation (CV) < 5%). It is applicable to cocoa and chocolate. Analysis of 32 samples of cocoa powder (16 alkalized and 16 natural) for OTA showed an incidence of 100%, with concentrations ranging from 0.25 to 7.8 ng g(-1); in six samples the OTA level exceeded 2 ng g(-1), the previously considered European Union limit for cocoa. The frequency of detection of OTA in 28 chocolate samples (21 dark or baking chocolate and seven milk chocolate) was also 100% with concentrations ranging from 0.05 to 1.4 ng g(-1); one sample had a level higher than the previously considered European Union limit for chocolate (1 ng g(-1)).

Development and validation of an LC-UV method for the determination of sulfonamides in animal feeds.

PubMed

Kumar, P; Companyó, R

2012-05-01

A simple LC-UV method was developed for the determination of residues of eight sulfonamides (sulfachloropyridazine, sulfadiazine, sulfadimidine, sulfadoxine, sulfamethoxypyridazine, sulfaquinoxaline, sulfamethoxazole, and sulfadimethoxine) in six types of animal feed. C18, Oasis HLB, Plexa and Plexa PCX stationary phases were assessed for the clean-up step and the latter was chosen as it showed greater efficiency in the clean-up of interferences. Feed samples spiked with sulfonamides at 2 mg/kg were used to assess the trueness (recovery %) and precision of the method. Mean recovery values ranged from 47% to 66%, intra-day precision (RSD %) from 4% to 15% and inter-day precision (RSD %) from 7% to 18% in pig feed. Recoveries and intra-day precisions were also evaluated in rabbit, hen, cow, chicken and piglet feed matrices. Calibration curves with standards prepared in mobile phase and matrix-matched calibration curves were compared and the matrix effects were ascertained. The limits of detection and quantification in the feeds ranged from 74 to 265 µg/kg and from 265 to 868 µg/kg, respectively. Copyright © 2011 John Wiley & Sons, Ltd.

Determination of insoluble soap in agricultural soil and sewage sludge samples by liquid chromatography with ultraviolet detection.

PubMed

Cantarero, Samuel; Zafra-Gómez, Alberto; Ballesteros, Oscar; Navalón, Alberto; Vílchez, José L; Crovetto, Guillermo; Verge, Coral; de Ferrer, Juan A

2010-11-01

We have developed a new analytical procedure for determining insoluble Ca and Mg fatty acid salts (soaps) in agricultural soil and sewage sludge samples. The number of analytical methodologies that focus in the determination of insoluble soap salts in different environmental compartments is very limited. In this work, we propose a methodology that involves a sample clean-up step with petroleum ether to remove soluble salts and a conversion of Ca and Mg insoluble salts into soluble potassium salts using tripotassium ethylenediaminetetraacetate salt and potassium carbonate, followed by the extraction of analytes from the samples using microwave-assisted extraction with methanol. An improved esterification procedure using 2,4-dibromoacetophenone before the liquid chromatography with ultraviolet detection analysis also has been developed. The absence of matrix effect was demonstrated with two fatty acid Ca salts that are not commercial and are never detected in natural samples (C₁₃:₀ and C₁₇:₀). Therefore, it was possible to evaluate the matrix effect because both standards have similar environmental behavior (adsorption and precipitation) to commercial soaps (C₁₀:₀) to C₁₈:₀). We also studied the effect of the different variables on the clean-up, the conversion of Ca soap, and the extraction and derivatization procedures. The quantification limits found ranged from 0.4 to 0.8 mg/kg. The proposed method was satisfactorily applied for the development of a study on soap behavior in agricultural soil and sewage sludge samples. © 2010 SETAC.

Multiresidue method for the determination of 227 pesticides in hot pepper (Capsicum annuum L.) by liquid chromatography with tandem mass spectrometry.

PubMed

Zhu, Yong-Zhe; Zhao, Mei-Ai; Nan Feng, Ya; Han Kim, Jeong

2014-10-01

A high-throughput, rapid, and efficient modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method with a simple cleanup procedure has been developed for simultaneously determining 227 pesticides in pepper samples by liquid chromatography with tandem mass spectrometry (running time: 10 min). Pesticide residues were extracted/partitioned with an acetonitrile/DisQuE QuEChERS pouch, and the resulting samples were cleaned up with different methods: dispersive solid-phase extraction with primary secondary amines or multiwalled carbon nanotubes and graphitized carbon solid mini cartridge column. The results indicated that multiwalled carbon nanotubes dispersive sorbents achieved the best recoveries and had less matrix interference. The numbers of pesticides with a recovery in the range of 70-120% were 199 at a spiked level of 40 μg/kg. The correlation coefficients (r(2)) for 227 pesticides were above 0.99, while the limits of quantitation of pesticides in pepper samples ranged from 0.13 to 13.51 μg/kg (S/N = 10), and the limits of detection ranged from 0.04 to 4.05 μg/kg (S/N = 3). The relative standard deviations of approximately 197 pesticides were below 20% at spiked levels of 40 μg/kg. Based on these results, the proposed method was chosen as the most suitable cleanup procedure for the determination of multiresidue pesticides in pepper samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

CONTAMINANTS AND REMEDIAL OPTIONS AT SELECTED METAL-CONTAMINATED SITES

EPA Science Inventory

This document provides information that facilitates characterization of the site and selection of treatment technologies at metals-contaminated sites that would be capable of meeting site-specific cleanup levels. he document does not facilitate the determination of cleanup levels...

Multiwall carbon nanotube- zirconium oxide nanocomposite hollow fiber solid phase microextraction for determination of polyaromatic hydrocarbons in water, coffee and tea samples.

PubMed

Yazdi, Mahnaz Nozohour; Yamini, Yadollah; Asiabi, Hamid

2018-06-15

The purpose of this study was to evaluate the application of hollow fiber solid-phase microextraction (HF-SPME) followed by HPLC-UV to determine the ultra-trace amounts of polycyclic aromatic hydrocarbons (PAHs) as model analytes in complex coffee and tea samples. HF-SPME can be effectively used as an alternative to the direct immersion SPME (DI-SPME) method in complex matrices. The DI-SPME method suffers from serious limitation in dirty and complicated matrices with low sample clean-up, while the HF-SPME method has high clean-up and selectivity due to the high porosity of hollow fiber that can pick out analyte from complicated matrices. As a hollow fiber sorbent, a novel multiwall carbon nanotube/zirconium oxide nanocomposite (MWCNT/ZrO 2 ) was fabricated. The excellent adsorption of PAHs on the sorbent was attributed to the dominant roles of π-π stacking interaction and hydrophobic interaction. Under the optimized extraction conditions, the wide linear range of 0.1-200 μg L -1 with coefficients of determination better than 0.998 and low detection limits of 0.033-0.16 μg L -1 with satisfactory precision (RSD < 6.6%) were obtained. The relative recoveries obtained by spiking the PAHs in water, coffee and tea samples were in the range of 92.0-106.0%. Compared to other methods, MWCNT/ZrO 2 hollow fiber solid phase microextraction demonstrated a good capability for determination of PAHs in complex coffee and tea samples. Copyright © 2018 Elsevier B.V. All rights reserved.

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

USDA-ARS?s Scientific Manuscript database

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...

An Evaluation of Public Preferences for Superfund Site Cleanup, Volume II: Pilot Study (1995)

EPA Pesticide Factsheets

In volume II, the authors present the detailed technical results of a pilot market research study that was conducted to determine preferences for the specific type and level of cleanup desired by the public at Superfund sites.

Evaluation of a recent product to remove lipids and other matrix co-extractives in the analysis of pesticide residues and environmental contaminants in foods.

PubMed

Han, Lijun; Matarrita, Jessie; Sapozhnikova, Yelena; Lehotay, Steven J

2016-06-03

This study demonstrates the application of a novel lipid removal product to the residue analysis of 65 pesticides and 52 environmental contaminants in kale, pork, salmon, and avocado by fast, low pressure gas chromatography - tandem mass spectrometry (LPGC-MS/MS). Sample preparation involves QuEChERS extraction followed by use of EMR-Lipid ("enhanced matrix removal of lipids") and an additional salting out step for cleanup. The optimal amount of EMR-Lipid was determined to be 500mg for 2.5mL extracts for most of the analytes. The co-extractive removal efficiency by the EMR-Lipid cleanup step was 83-98% for fatty samples and 79% for kale, including 76% removal of chlorophyll. Matrix effects were typically less than ±20%, in part because analyte protectants were used in the LPGC-MS/MS analysis. The recoveries of polycyclic aromatic hydrocarbons and diverse pesticides were mostly 70-120%, whereas recoveries of nonpolar polybrominated diphenyl ethers and polychlorinated biphenyls were mostly lower than 70% through the cleanup procedure. With the use of internal standards, method validation results showed that 76-85 of the 117 analytes achieved satisfactory results (recoveries of 70-120% and RSD≤20%) in pork, avocado, and kale, while 53 analytes had satisfactory results in salmon. Detection limits were 5-10ng/g for all but a few analytes. EMR-Lipid is a new sample preparation tool that serves as another useful option for cleanup in multiresidue analysis, particularly of fatty foods. Published by Elsevier B.V.

All hazardous waste politics is local: Grass-roots advocacy and public participation in siting and cleanup decisions

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

Lowry, R.C.

1998-12-31

The combined effects of federalism and interest group pluralism pose particularly difficult problems for hazardous waste siting and cleanup decisions. Most national environmental groups have only limited involvement in local hazardous waste politics, while local grass-roots advocates have very different interests and sometimes are pitted against one another. Both the Environmental protection Agency and the Department of energy recently have begun to use site-specific citizen advisory boards at cleanup sites. This approach appears to improve communications at some sites, but does not address the issues of ``not in my back yard`` politics and alleged inequitable exposure to hazardous wastes.

Content Analysis of Vomit and Diarrhea Cleanup Procedures To Prevent Norovirus Infections in Retail and Food Service Operations.

PubMed

Chao, Morgan G; Dubé, Anne-Julie; Leone, Cortney M; Moore, Christina M; Fraser, Angela M

2016-11-01

Human noroviruses are the leading cause of foodborne disease in the United States, sickening 19 to 21 million Americans each year. Vomit and diarrhea are both highly concentrated sources of norovirus particles. For this reason, establishing appropriate cleanup procedures for these two substances is critical. Food service establishments in states that have adopted the 2009 or 2013 U.S. Food and Drug Administration Food Code are required to have a program detailing specific cleanup procedures. The aim of our study was to determine the alignment of existing vomit and diarrhea cleanup procedures with the 11 elements recommended in Annex 3 of the 2011 Supplement to the 2009 Food Code and to determine their readability and clarity of presentation. In July 2015, we located vomit and diarrhea cleanup procedures by asking Norovirus Collaborative for Outreach, Research, and Education stakeholders for procedures used by their constituency groups and by conducting a Google Advanced Search of the World Wide Web. We performed content analysis to determine alignment with the recommendations in Annex 3. Readability and clarity of presentation were also assessed. A total of 38 artifacts were analyzed. The mean alignment score was 7.0 ± 1.7 of 11 points; the mean clarity score was 6.7 ± 2.5 of 17 points. Only nine artifacts were classified as high clarity, high alignment. Vomit and diarrhea cleanup procedures should align with Annex 3 in the Food Code and should, as well, be clearly presented; yet, none of the artifacts completely met both conditions. To reduce the spread of norovirus infections in food service establishments, editable guidelines are needed that are aligned with Annex 3 and are clearly written, into which authors could insert their facility-specific information.

Power Sources Focus Group - Evaluation of Plasma Gasification for Waste-to-Energy Conversion

DTIC Science & Technology

2012-09-21

including paper , wood, plastic, food and agricultural waste. The system uses a shredder, dryer , and pelletizing preprocessor to fuel an in-house...limited information available, this paper does not attempt to determine the best way to use plasma in a gasifier. Instead, this paper makes general...Gasification Plasma gasification for the purposes of this paper includes any WTE system using plasma as part of the generation of syngas and/or cleanup

Establishing Final Cleanup Decisions for the Hanford Site River Corridor

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

Lerch, J.A.; Sands, J.P.

2007-07-01

A major challenge in the River Corridor Closure Contract is establishing final cleanup decisions for the source operable units in the Hanford Site river corridor. Cleanup actions in the river corridor began in 1994 and have been performed in accordance with a 'bias for action' approach adopted by the Tri-Parties - the U.S. Department of Energy, U.S. Environmental Protection Agency, and Washington State Department of Ecology. This approach enabled early application of cleanup dollars on actual remediation of contaminated waste sites. Consequently, the regulatory framework authorizing cleanup actions at source operable units in the river corridor consists largely of interimmore » action records of decision, which were supported by qualitative risk assessments. Obtaining final cleanup decisions for the source operable units is necessary to determine whether past cleanup actions in the river corridor are protective of human health and the environment and to identify any course corrections that may be needed to ensure that ongoing and future cleanup actions are protective. Because the cleanup actions are ongoing, it is desirable to establish the final cleanup decisions as early as possible to minimize the impacts of any identified course corrections to the present cleanup approach. Development of a strategy to obtain final cleanup decisions for the source operable units in a manner that is responsive to desires for an integrated approach with the groundwater and Columbia River components while maintaining the ability to evaluate each component on its own merit represents a significant challenge. There are many different options for grouping final cleanup decisions, and each involved party or stakeholder brings slightly different interests that shape the approach. Regardless of the selected approach, there are several specific challenges and issues to be addressed before making final cleanup decisions. A multi-agency and contractor working group has been established to address these issues and develop an endorsed strategy. Ultimately, it is anticipated that the Tri-Parties will establish a set of milestones to document pathway selection and define schedule requirements. (authors)« less

40 CFR 761.243 - Standard wipe sample method and size.

Code of Federal Regulations, 2010 CFR

2010-07-01

..., AND USE PROHIBITIONS Determining a PCB Concentration for Purposes of Abandonment or Disposal of Natural Gas Pipeline: Selecting Sample Sites, Collecting Surface Samples, and Analyzing Standard PCB Wipe.../Rinse Cleanup as Recommended by the Environmental Protection Agency PCB Spill Cleanup Policy,” dated...

Determination of perfluorinated compounds in mollusks by matrix solid-phase dispersion and liquid chromatography-tandem mass spectrometry.

PubMed

Villaverde-de-Sáa, Eugenia; Quintana, José Benito; Rodil, Rosario; Ferrero-Refojos, Raúl; Rubí, Elisa; Cela, Rafael

2012-01-01

Perfluorinated compounds (PFCs) have been used for over 40 years in different commercial and industrial applications mainly as surfactants and surface protectors and have become an important class of marine emerging pollutants. This study presents the development and validation of a new analytical method to determine the simultaneous presence of eight PFCs in different kinds of mollusks using matrix solid-phase dispersion (MSPD) followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Simplicity of the analytical procedure, low volume of solvent and quantity of sample required, low global price, and integration of extraction and clean-up into a single step, are the most important advantages of the developed methodology. Solvent, solid support (dispersing agent), clean-up sorbent, and their amounts were optimized by means of an experimental design. In the final method, 0.5 g of sample are dispersed with 0.2 g of diatomaceous earth and transferred into a polypropylene syringe containing 4 g of silica as clean-up sorbent. Then, analytes are eluted with 20 mL of acetonitrile. The extract is finally concentrated to a final volume of 0.5 mL in methanol, avoiding extract dryness in order to prevent evaporation losses and injected in the LC-MS/MS. The combination of this MSPD protocol with LC-MS/MS afforded detection limits from 0.05 to 0.3 ng g(-1). Also, a good linearity was established for the eight PFCs in the range from limit of quantification (LOQ) to 500 ng mL(-1) with R(2) > 0.9917. The recovery of the method was studied with three types of spiked mollusk and was in the 64-126% range. Moreover, a mussel sample was spiked and aged for more than 1 month and analyzed by the developed method and a reference method, ion-pair extraction, for comparison, producing both methods statistically equal concentration values. The method was finally applied to the determination of PFCs in different kinds of mollusks revealing concentrations up to 8.3 ng g(-1) for perfluoroundecanoic acid.

An Evaluation of Public Preferences for Superfund Site Cleanup, Volume 1: A Preliminary Assessment (1995)

EPA Pesticide Factsheets

The purpose of the project is to develop a methodology for determining the cleanup options for National Priority List (NPL) sites governed under Superfund legislation that are acceptable to the public. A survey instrument was developed for the study.

Simultaneous determination of 117 pesticides and 30 mycotoxins in raw coffee, without clean-up, by LC-ESI-MS/MS analysis.

PubMed

Reichert, Bárbara; de Kok, André; Pizzutti, Ionara Regina; Scholten, Jos; Cardoso, Carmem Dickow; Spanjer, Martien

2018-04-03

This paper describes the optimization and validation of an acetonitrile based method for simultaneous extraction of multiple pesticides and mycotoxins from raw coffee beans followed by LC-ESI-MS/MS determination. Before extraction, the raw coffee samples were milled and then slurried with water. The slurried samples were spiked with two separate standard solutions, one containing 131 pesticides and a second with 35 mycotoxins, which were divided into 3 groups of different relative concentration levels. Optimization of the QuEChERS approach included performance tests with acetonitrile acidified with acetic acid or formic acid, with or without buffer and with or without clean-up of the extracts before LC-ESI-MS/MS analysis. For the clean-up step, seven d-SPE sorbents and their various mixtures were evaluated. After method optimization a complete validation study was carried out to ensure adequate performance of the extraction and chromatographic methods. The samples were spiked at 3 concentrations levels with both mycotoxins and pesticides (with 6 replicates at each level, n = 6) and then submitted to the extraction procedure. Before LC-ESI-MS/MS analysis, the acetonitrile extracts were diluted 2-fold with methanol, in order to improve the chromatographic performance of the early-eluting polar analytes. Calibration standard solutions were prepared in organic solvent and in blank coffee extract at 7 concentration levels and analyzed 6 times each. The method was assessed for accuracy (recovery %), precision (RSD%), selectivity, linearity (r 2 ), limit of quantification (LOQ) and matrix effects (%). Copyright © 2017 Elsevier B.V. All rights reserved.

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

USDA-ARS?s Scientific Manuscript database

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...

Not ''just'' pump and treat

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

Angleberger, K; Bainer, R W

2000-12-12

The Lawrence Livermore National Laboratory (LLNL) has been consistently improving the site cleanup methods by adopting new philosophies, strategies and technologies to address constrained or declining budgets, lack of useable space due to a highly industrialized site, and significant technical challenges. As identified in the ROD, the preferred remedy at the LLNL Livermore Site is pump and treat, although LLNL has improved this strategy to bring the remediation of the ground water to closure as soon as possible. LLNL took the logical progression from a pump and treat system to the philosophy of ''Smart Pump and Treat'' coupled with themore » concepts of ''Hydrostratigraphic Unit Analysis,'' ''Engineered Plume Collapse,'' and ''Phased Source Remediation,'' which led to the development of new, more cost-effective technologies which have accelerated the attainment of cleanup goals significantly. Modeling is also incorporated to constantly develop new, cost-effective methodologies to accelerate cleanup and communicate the progress of cleanup to stakeholders. In addition, LLNL improved on the efficiency and flexibility of ground water treatment facilities. Ground water cleanup has traditionally relied on costly and obtrusive fixed treatment facilities. LLNL has designed and implemented various portable ground water treatment units to replace the fixed facilities; the application of each type of facility is determined by the amount of ground water flow and contaminant concentrations. These treatment units have allowed for aggressive ground water cleanup, increased cleanup flexibility, and reduced capital and electrical costs. After a treatment unit has completed ground water cleanup at one location, it can easily be moved to another location for additional ground water cleanup.« less

Estimate of the Potential Amount of Low-Level Waste from the Fukushima Prefecture - 12370

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

Hill, Carolyn; Olson, Eric A.J.; Elmer, John

2012-07-01

The amount of waste generated by the cleanup of the Fukushima Prefecture (Fukushima-ken) following the releases from the Fukushima Daiichi nuclear power plant accident (March 2011) is dependent on many factors, including: - Contamination amounts; - Cleanup levels determined for the radioisotopes contaminating the area; - Future land use expectations and human exposure scenarios; - Groundwater contamination considerations; - Costs and availability of storage areas, and eventually disposal areas for the waste; and - Decontamination and volume reduction techniques and technologies used. For the purposes of estimating these waste volumes, Fukushima-ken is segregated into zones of similar contamination level andmore » expected future use. Techniques for selecting the appropriate cleanup methods for each area are shown in a decision tree format. This approach is broadly applied to the 20 km evacuation zone and the total amounts and types of waste are estimated; waste resulting from cleanup efforts outside of the evacuation zone is not considered. Some of the limits of future use and potential zones where residents must be excluded within the prefecture are also described. The size and design of the proposed intermediate storage facility is also discussed and the current situation, cleanup, waste handling, and waste storage issues in Japan are described. The method for estimating waste amounts outlined above illustrates the large amount of waste that could potentially be generated by remediation of the 20 km evacuation zone (619 km{sup 2} total) if the currently proposed cleanup goals are uniformly applied. The Japanese environment ministry estimated in early October that the 1 mSv/year exposure goal would make the government responsible for decontaminating about 8,000 km{sup 2} within Fukushima-ken and roughly 4,900 km{sup 2} in areas outside the prefecture. The described waste volume estimation method also does not give any consideration to areas with localized hot spots. Land use and area dose rate estimates for the 20 km evacuation zone indicate there are large areas where doses to the public can be mitigated through methods other than removal and disposal of soil and other wastes. Several additional options for waste reduction can also be considered, including: - Recycling/reusing or disposing of as municipal waste material that can be unconditionally cleared; - Establishing additional precautionary (e.g., liners) and monitoring requirements for municipal landfills to dispose of some conditionally-cleared material; and - Using slightly-contaminated material in construction of reclamations, banks and roads. Waste estimates for cleanup will continue to evolve as decontamination plans are drafted and finalized. (authors)« less

Determination of Total Biotin by Liquid Chromatography Coupled with Immunoaffinity Column Cleanup Extraction: Multilaboratory Testing, Final Action 2016.02.

PubMed

Joseph, George; Devi, Ranjani; Marley, Elaine C; Leeman, David

2018-05-01

Single- and multilaboratory testing data have provided systematic scientific evidence that a simple, selective, accurate, and precise method can be used as a potential candidate reference method for dispute resolution in determining total biotin in all forms of infant, adult, and/or pediatric formula. Using LC coupled with immunoaffinity column cleanup extraction, the method fully meets the intended purpose and applicability statement in AOAC Standard Method Performance Requirement 2014.005. The method was applied to a cross-section of infant formula and adult nutritional matrixes, and acceptable precision and accuracy were established. The analytical platform is inexpensive, and the method can be used in almost any laboratory worldwide with basic facilities. The immunoaffinity column cleanup extraction is the key step to successful analysis.

Simultaneous and rapid determination of deoxynivalenol and its acetylate derivatives in wheat flour and rice by ultra high performance liquid chromatography with photo diode array detection.

PubMed

Xu, Jiao-Jiao; Zhou, Jian; Huang, Bai-Fen; Cai, Zeng-Xuan; Xu, Xiao-Min; Ren, Yi-Ping

2016-06-01

A simple and reliable method of ultra high performance liquid chromatography coupled with photo-diode array detection has been proposed for the simultaneous determination of deoxynivalenol and its acetylated derivatives in wheat flour and rice, especially focusing on the optimization of sample extraction, cleanup, and chromatographic separation conditions. Sample pretreatment consisted of a first step using a quick, easy, cheap, effective, rugged, and safe based extraction procedure and a subsequent cleanup step based on solid-phase extraction. The method was extensively validated in wheat flour and rice, obtaining satisfactory analytical performance with good linearity (R(2) ≥ 0.999), acceptable recoveries (80.0-104.4%), and repeatability (RSDs 1.3-10.7%). The limits of detection (21.7-57.4 μg/kg) and quantitation (72.3-191.4 μg/kg) for deoxynivalenols were lower than those usually permitted by various countries' legislation in these food matrices. The method was applied to 34 wheat and rice samples. The results were further compared with results of ultra high performance liquid chromatography with electrospray ionization tandem mass spectrometry. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of 21 antibiotics in sea cucumber using accelerated solvent extraction with in-cell clean-up coupled to ultra-performance liquid chromatography-tandem mass spectrometry.

PubMed

Zhu, Minghua; Zhao, Hongxia; Xia, Deming; Du, Juan; Xie, Huaijun; Chen, Jingwen

2018-08-30

An accelerated solvent extraction (ASE) with in-cell clean-up method coupled to ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed to determine 21 antibiotics in sea cucumber. The analytes include 10 sulfonamides, 4 fluoroquinolones, 3 amphenicols, 2 beta-lactams, 1 lincosamide and trimethoprim. Optimal parameters of ASE method were obtained at 80 °C, 1 static cycle of 5 min with methanol/acetonitrile (1/1, v/v) using 2 g of C18 as adsorbent. Recoveries at 50.1-129.2% were achieved with RSD under 20%. Method detection limits ranged from 0.03 to 2.9 μg kg -1 . Compared to the reported ultrasound-assisted extraction method, the proposed method offered comparable extraction efficiency for sulfonamides from sea cucumber, but higher for other categories of antibiotics. This validated method was then successfully applied to sea cucumber samples and 9 antibiotics were detected with the highest concentration up to 57.7 μg kg -1 for norfloxacin. Copyright © 2018 Elsevier Ltd. All rights reserved.

Liquid chromatographic determination of benzocaine and N-acetylbenzocaine in the edible fillet tissue from rainbow trout

USGS Publications Warehouse

Meinertz, J.R.; Stehly, G.R.; Hubert, T.D.; Bernardy, J.A.

1999-01-01

A method was developed for determining benzocaine and N-acetylbenzocaine concentrations in fillet tissue of rainbow trout. The method involves extracting the analytes with acetonitrile, removing lipids or hydrophobic compounds from the extract with hexane, and providing additional clean-up with solid-phase extraction techniques. Analyte concentrations are determined using reversed-phase high-performance liquid chromatographic techniques with an isocratic mobile phase and UV detection. The accuracy (range, 92 to 121%), precision (R.S.D., <14%), and sensitivity (method quantitation limit, <24 ng/g) for each analyte indicate the usefulness of this method for studies characterizing the depletion of benzocaine residues from fish exposed to benzocaine. Copyright (C) 1999.

40 CFR 280.65 - Investigations for soil and ground-water cleanup.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 28 2012-07-01 2012-07-01 false Investigations for soil and ground... Containing Petroleum or Hazardous Substances § 280.65 Investigations for soil and ground-water cleanup. (a) In order to determine the full extent and location of soils contaminated by the release and the...

40 CFR 280.65 - Investigations for soil and ground-water cleanup.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 27 2011-07-01 2011-07-01 false Investigations for soil and ground... Containing Petroleum or Hazardous Substances § 280.65 Investigations for soil and ground-water cleanup. (a) In order to determine the full extent and location of soils contaminated by the release and the...

40 CFR 280.65 - Investigations for soil and ground-water cleanup.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 27 2014-07-01 2014-07-01 false Investigations for soil and ground... Containing Petroleum or Hazardous Substances § 280.65 Investigations for soil and ground-water cleanup. (a) In order to determine the full extent and location of soils contaminated by the release and the...

40 CFR 280.65 - Investigations for soil and ground-water cleanup.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 28 2013-07-01 2013-07-01 false Investigations for soil and ground... Containing Petroleum or Hazardous Substances § 280.65 Investigations for soil and ground-water cleanup. (a) In order to determine the full extent and location of soils contaminated by the release and the...

40 CFR 280.65 - Investigations for soil and ground-water cleanup.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 26 2010-07-01 2010-07-01 false Investigations for soil and ground... Containing Petroleum or Hazardous Substances § 280.65 Investigations for soil and ground-water cleanup. (a) In order to determine the full extent and location of soils contaminated by the release and the...

40 CFR 761.283 - Determination of the number of samples to collect and sample collection locations.

Code of Federal Regulations, 2013 CFR

2013-07-01

... ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT POLYCHLORINATED BIPHENYLS (PCBs...-Implementing Cleanup and On-Site Disposal of Bulk PCB Remediation Waste and Porous Surfaces in Accordance With... locations for bulk PCB remediation waste and porous surfaces destined to remain at a cleanup site after...

40 CFR 761.283 - Determination of the number of samples to collect and sample collection locations.

Code of Federal Regulations, 2014 CFR

2014-07-01

... ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT POLYCHLORINATED BIPHENYLS (PCBs...-Implementing Cleanup and On-Site Disposal of Bulk PCB Remediation Waste and Porous Surfaces in Accordance With... locations for bulk PCB remediation waste and porous surfaces destined to remain at a cleanup site after...

Immunoaffinity column as clean-up tool for determination of trace amounts of microcystins in tap water.

PubMed

Tsutsumi, T; Nagata, S; Hasegawa, A; Ueno, Y

2000-07-01

Trace amounts of microcystins (MCs) in drinking water should be monitored because of their potential hazard for human health as an environmental tumor promoter. We describe here a new clean-up tool with immunoaffinity column (IAC) for determination of trace amounts of MCs (from pg to microg/litre) in tap water. The water samples were concentrated with IAC clean-up and MCs levels were determined by HPLC with UV detection or enzyme-linked immunosorbent assay (ELISA). In the combination with HPLC analysis, mean recovery of microcystin-LR (MCLR),-RR and-YR spiked to tap water were 91.8%, 77.3% and 86.4%, respectively, in the range 2.5-100 microg/litre. The chromatogram of MCs-spiked tap water sample cleaned up with IAC showed effective elimination of the impurities compared to that with octadecyl silanized cartridge, which had been cleaned up with a conventional method. Also, in the combination with highly sensitive ELISA, mean recovery of MCLR spiked to tap water was 80% in the range 0.1-1000 ng/litre. The combined methods developed here can detect pg to microg/litre of MCs in tap water. The overall results indicated that IAC will be suitable as a clean-up tool for trace amounts of MCs in tap water.

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.

Pesticide analysis in coffee leaves using a quick, easy, cheap, effective, rugged and safe approach and liquid chromatography tandem mass spectrometry: Optimization of the clean-up step.

PubMed

Trevisan, Maria Teresa Salles; Owen, Robert Wyn; Calatayud-Vernich, Pau; Breuer, Andrea; Picó, Yolanda

2017-08-25

An analytical method using a quick, easy, cheap, effective, rugged and safe (QuEChERS) procedure for multi-residue determination of 52 pesticides in coffee leaf extractshas been developed and validated according to SANTE/11945/2015 guidelines. Different sorbent combinations for dispersive solid phase extraction (d-SPE) clean-up as well as dispersive liquid-liquid microextraction (DLLME) were tested. The relative standard deviations (RSDs) for the recovery of 87-94% of pesticides added to coffee leaf extracts,was ≤20% for samples spiked at concentrations up to 50ng*g -1 depending on the clean-up procedures. However, samples spiked with a 100ng*g -1 pesticide mixture gave RSDs>20% for most pesticides when d-SPE was carried out adding Supelclean ENVI-Carb 120/400. To explain this fact,the secondary metabolic profile was analyzed in all the extraction and clean-up procedures. Only in the clean-up procedure with the addition of Supel QuE Z-Sep+, does caffeine show a constant adsorption between blank and spiked samples. In other clean-up procedures, the amount of caffeine was higher in those samples spiked with pesticides. This indicates competition between caffeine and pesticides for adsorption to the sorbent. Addition of Supel QuE Z-Sep+ to the procedure revealed only a 32% matrix effect, whereas using PSA+ C18 the matrix effect was close to 97%. The process efficiency is up to 54% with the addition of Supel QuE Z-Sep+ and just up to 7% for the other clean-up procedures. The method was successfully tested in coffee leaves from different types of cultivars. Pesticides were not detected in organic coffee leaf extracts, but thiametoxan was clearly detected in 50% of coffee leaf extracts harvested from coffee trees grown under traditional conditions as determined by UHPLC-TOFMSLC/QqTOF-MS/MS. Copyright © 2017 Elsevier B.V. All rights reserved.

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

USDA-ARS?s Scientific Manuscript database

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...

Risk Assessment Approach for the Hanford Site River Corridor Closure Project

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

Thomson, J.E.; Weiss, S.G.; Sands, J.P.

2007-07-01

The river corridor portion of the U.S. Department of Energy's (DOE) Hanford Site includes the 100 Area and 300 Area, which border the Columbia River and cover 565 km{sup 2} (218 mi{sup 2}). The River Corridor Closure (RCC) Project scope of work includes 486 contaminated facilities, 4 of 9 deactivated plutonium production reactors, and 370 waste disposal sites. DOE's cleanup actions in the river corridor were initiated in 1994 under the Comprehensive Environmental Response, Compensation, and Liability Act of 1981 (42 U.S.C. 9601, et seq.) (CERCLA) and included source and groundwater operable units (OUs). DOE's RCC Project, awarded to Washingtonmore » Closure Hanford (WCH) in 2005, focuses on source OUs and has allowed cleanup actions to continue in the 100 and 300 Areas with completion by 2013. The regulatory authorization for cleanup actions at source OUs in the river corridor consists primarily of interim action records of decision (RODs), which were supported by qualitative risk assessments and limited field investigations. A key to establishing final cleanup decisions and proceeding toward final CERCLA closeout is completion of quantitative baseline risk assessment activities. Baseline risk assessment is necessary to determine whether cleanup actions are protective of human health and the environment and to identify any course corrections needed to ensure that current and future cleanup actions are protective. Because cleanup actions are ongoing under interim action RODs, it is desirable to establish the final cleanup decision bases as early as possible to minimize the impacts of any identified course corrections to the cleanup approach. Risk assessment is being performed by WCH as the River Corridor Baseline Risk Assessment (RCBRA). The RCBRA uses a multi-step process that summarizes existing data; uses the data quality objectives process to identify both data gaps and unresolved issues through public workshops; and solicits input from regulators, trustees, and stakeholders. Sampling and analysis plans are then developed to document quality requirements and identify field sample collection approaches. After required data are collected, the risks to human health and the environment are assessed. Sampling of upland, riparian, and near-shore environments for the 100/300 Area Component was performed in 2005 and 2006. The 100/300 Area Component includes former operational/reactor areas. The results of these efforts will be incorporated into a mid-2007 draft risk assessment report for the 100/300 Area Component of the RCBRA. Adapting methodology developed from the 100/300 Area Component, the Inter-Areas risk assessment will be conducted for the riparian and near-shore environments. The Inter-Areas Component includes shoreline areas between former operational areas addressed in the 100/300 Area Component. The Inter-Areas risk assessment will supplement results from the 100/300 Area Component to provide a more complete analysis of residual risks in the river corridor. Plans for the final element of the RCBRA, the Columbia River Component, are being developed by DOE and currently is not part of the RCC Project. The Columbia River Component includes the reach of the Columbia River located adjacent to the Hanford Site and reaches downstream to an undetermined boundary. Recommendations for final cleanup decisions at source units within the river corridor, based in part on the risk assessment results, will be presented for future public review in a River Corridor Source Unit Proposed Plan. To form an integrated cleanup approach for the river corridor, the RCBRA results for the source units require integration with risk assessment results from groundwater cleanup actions managed by other contractors. WCH's risk assessment task includes development of an integration strategy for activities leading up to the final regulatory decisions for all OUs in the river corridor. (authors)« less

Determination of melamine in animal feed based on liquid chromatography tandem mass spectrometry analysis and dynamic microwave-assisted extraction coupled on-line with strong cation-exchange resin clean-up.

PubMed

Chen, Ligang; Zeng, Qinglei; Du, Xiaobo; Sun, Xin; Zhang, Xiaopan; Xu, Yang; Yu, Aimin; Zhang, Hanqi; Ding, Lan

2009-11-01

In this work, a new method was developed for the determination of melamine (MEL) in animal feed. The method was based on the on-line coupling of dynamic microwave-assisted extraction (DMAE) to strong cation-exchange (SCX) resin clean-up. The MEL was first extracted by 90% acidified methanol aqueous solution (v/v, pH = 3) under the action of microwave energy, and then the extract was cooled and passed through the SCX resin. Thus, the protonated MEL was retained on the resin through ion exchange interaction and the sample matrixes were washed out. Some obvious benefits were achieved, such as acceleration of analytical process, together with reduction in manual handling, risk of contamination, loss of analyte, and sample consumption. Finally, the analyte was separated by a liquid chromatograph with a SCX analytical column, and then identified and quantitatived by a tandem mass spectrometry with positive ionization mode and multiple-reaction monitoring. The DMAE parameters were optimized by the Box-Behnken design. The linearity of quantification obtained by analyzing matrix-matched standards is in the range of 50-5,000 ng g(-1). The limit of detection and limit of quantification obtained are 12.3 and 41.0 ng g(-1), respectively. The mean intra- and inter-day precisions expressed as relative standard deviations with three fortified levels (50, 250, and 500 ng g(-1)) are 5.1% and 7.3%, respectively, and the recoveries of MEL are in the range of 76.1-93.5%. The proposed method was successfully applied to determine MEL in different animal feeds obtained from the local market. MEL was detectable with the contents of 279, 136, and 742 ng g(-1) in three samples.

An automated online turboflow cleanup LC/MS/MS method for the determination of 11 plasticizers in beverages and milk.

PubMed

Ates, Ebru; Mittendorf, Klaus; Senyuva, Hamide

2013-01-01

An automated sample preparation technique involving cleanup and analytical separation in a single operation using an online coupled TurboFlow (RP-LC system) is reported. This method eliminates time-consuming sample preparation steps that can be potential sources for cross-contamination in the analysis of plasticizers. Using TurboFlow chromatography, liquid samples were injected directly into the automated system without previous extraction or cleanup. Special cleanup columns enabled specific binding of target compounds; higher MW compounds, i.e., fats and proteins, and other matrix interferences with different chemical properties were removed to waste, prior to LC/MS/MS. Systematic stepwise method development using this new technology in the food safety area is described. Selection of optimum columns and mobile phases for loading onto the cleanup column followed by transfer onto the analytical column and MS detection are critical method parameters. The method was optimized for the assay of 10 phthalates (dimethyl, diethyl, dipropyl, butyl benzyl, diisobutyl, dicyclohexyl, dihexyl, diethylhexyl, diisononyl, and diisododecyl) and one adipate (diethylhexyl) in beverages and milk.

Development of comprehensive remediation standards at San Francisco International Airport

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

Grosso, A.; Lawler, M.; Meek, S.

1995-12-31

An ongoing expansion at the San Francisco International Airport (Airport) will result in a 35 percent increase in both terminal square footage and passenger handling capability. Facility relocation and construction are set to begin in October, 1995. Appropriate cleanup of contaminated soil and groundwater must be completed prior to this activity. Remedial goals for this major industrial facility must be protective of both human health and the environment. A risk-based strategy for the development of recommended cleanup objectives has been developed with the support of state regulatory agencies. This strategy includes Remediation Management Zones (RMZs), distinct regions at the Airportmore » with different remedial goals based on the associated risk to water quality, human health, and the environment. The RMZs and the final cleanup objectives for the Airport will be finalized by mid-1995, and will be used to govern future cleanup efforts at the site. This presentation will describe the history of the project, the determination of human health and ecological buffer zones, and the integration of these two concepts to produce cleanup objectives fully supported by the state regulatory authority.« less

Experimental design for extraction and quantification of phenolic compounds and organic acids in white "Vinho Verde" grapes.

PubMed

Dopico-García, M S; Valentão, P; Guerra, L; Andrade, P B; Seabra, R M

2007-01-30

An experimental design was applied for the optimization of extraction and clean-up processes of phenolic compounds and organic acids from white "Vinho Verde" grapes. The developed analytical method consisted in two steps: first a solid-liquid extraction of both phenolic compounds and organic acids and then a clean-up step using solid-phase extraction (SPE). Afterwards, phenolic compounds and organic acids were determined by high-performance liquid chromatography (HPLC) coupled to a diode array detector (DAD) and HPLC-UV, respectively. Plackett-Burman design was carried out to select the significant experimental parameters affecting both the extraction and the clean-up steps. The identified and quantified phenolic compounds were: quercetin-3-O-glucoside, quercetin-3-O-rutinoside, kaempferol-3-O-rutinoside, isorhamnetin-3-O-glucoside, quercetin, kaempferol and epicatechin. The determined organic acids were oxalic, citric, tartaric, malic, shikimic and fumaric acids. The obtained results showed that the most important variables were the temperature (40 degrees C) and the solvent (acid water at pH 2 with 5% methanol) for the extraction step and the type of sorbent (C18 non end-capped) for the clean-up step.

Broad-spectrum immunoaffinity cleanup for the determination of aflatoxins B1, B2, G1, G2, M1, M2 in Ophiocordyceps sinensis and its pharmaceutical preparations by ultra performance liquid chromatography tandem mass spectrometry.

PubMed

Sun, Shujuan; Xie, Jie; Peng, Tao; Shao, Bing; Zhu, Kui; Sun, Yuanze; Yao, Kai; Gu, Qiang; Zhang, Jing; Fan, Chunlin; Chen, Ying; Jiang, Haiyang

2017-11-15

An ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the simultaneous determination of aflatoxins B 1 , B 2 , G 1 , G 2 , M 1 and M 2 (AFB 1 , AFB 2 , AFG 1 , AFG 2 , AFM 1 and AFM 2 ) in Ophiocordyceps sinensis and its pharmaceutical preparations. A rapid and reliable immunoaffinity column containing a broad-spectrum monoclonal antibody for six aflatoxins was used for sample cleanup. Under the optimized conditions, the home-made immunoaffinity column capacity were about 315, 319, 292, 102, 444 and 369ng/mL gel for AFB 1 , AFB 2 , AFG 1 , AFG 2 , AFM 1 and AFM 2 , respectively. Recoveries for all tested aflatoxins ranged from 79.28% to 103.42% with relative standard deviation less than 8%. The limits of quantitation were in the range of 0.008-0.045μg/kg. Among 31 real samples analyzed, one sample was contaminated with AFB 1 , AFB 2 and AFM 1 at levels of 0.483, 0.068 and 0.104μg/kg, respectively. The established method is simple, accurate, and can be effectively used to determine the aflatoxins in Ophiocordyceps sinensis and its pharmaceutical preparations. Copyright © 2017 Elsevier B.V. All rights reserved.

Pressurized solvent extraction followed by gas chromatography tandem mass spectrometry for the determination of benzotriazole light stabilizers in indoor dust.

PubMed

Carpinteiro, I; Abuín, B; Rodríguez, I; Ramil, M; Cela, R

2010-06-11

A novel and sensitive method for the determination of five benzotriazole compounds (commonly used as light stabilizers) in indoor dust is presented. Pressurized liquid extraction (PLE) and gas chromatography followed by tandem in time mass spectrometry (GC-MS/MS) were used as sample preparation and determination techniques, respectively. Extraction and clean-up were integrated on-line and, after an evaporative concentration step, the extract provided by the PLE instrument was injected directly in the GC-MS/MS system. Parameters affecting the performance of the sample preparation process were evaluated using experimental factorial designs. Under optimized conditions, analytes were recovered from 0.5g samples in 3 static extraction cycles of 10min, using a hexane:dichloromethane (7:3) mixture, at 90 degrees C. Silica (1g) was placed in the bottom of the extraction cells as clean-up sorbent. The recoveries of the method varied from 82 to 122%, with standard deviations below 13. The inter-day precision ranged from 9 to 12%, and the limits of quantification (LOQs) remained below 10ngg(-1) for all species. For the first time, four of the five investigated species were found in dust from indoor environments. Their mean concentrations ranged from 71 to 780ngg(-1). Copyright 2010 Elsevier B.V. All rights reserved.

A novel method for analysing key corticosteroids in polar bear (Ursus maritimus) hair using liquid chromatography tandem mass spectrometry.

PubMed

Weisser, Johan J; Hansen, Martin; Björklund, Erland; Sonne, Christian; Dietz, Rune; Styrishave, Bjarne

2016-04-01

This paper presents the development and evaluation of a methodology for extraction, clean-up and analysis of three key corticosteroids (aldosterone, cortisol and corticosterone) in polar bear hair. Such a methodology can be used to monitor stress biomarkers in polar bears and may provide as a useful tool for long-term and retrospective information. We developed a combined pressurized liquid extraction (PLE)-solid phase extraction (SPE) procedure for corticosteroid extraction and clean-up followed by high pressure liquid chromatography tandem mass spectrometry (HPLC-MS/MS) analysis. This procedure allows for the simultaneous determination of multiple steroids, which is in contrast to previous polar bear studies based on ELISA techniques. Absolute method recoveries were 81%, 75% and 60% for cortisol, corticosterone and aldosterone, respectively. We applied the developed method on a hair sample pooled from four East Greenland polar bears. Herein cortisol and corticosterone were successfully determined in levels of 0.32±0.02ng/g hair and 0.13±0.02ng/g hair, respectively. Aldosterone was below limit of detection (LOD<0.17ng/g). The cortisol hair concentration found in these East Greenland polar bears was consistent with cortisol levels previously determined in the Southern Hudson Bay and James Bay in Canada using ELISA kits. Copyright © 2016 Elsevier B.V. All rights reserved.

High-throughput analytical techniques for multiresidue, multiclass determination of 653 pesticides and chemical pollutants in tea--Part III: Evaluation of the cleanup efficiency of an SPE cartridge newly developed for multiresidues in tea.

PubMed

Pang, Guo-Fang; Fan, Chun-Lin; Chang, Qiao-Ying; Li, Yan; Kang, Jian; Wang, Wen-Wen; Cao, Jing; Zhao, Yan-Bing; Li, Nan; Li, Zeng-Yin; Chen, Zong-Mao; Luo, Feng-Jian; Lou, Zheng-Yun

2013-01-01

A comparative study was conducted over three stages on the cleanup efficiency of SPE cartridge Cleanert TPT, newly developed for multigroups of pesticide residues in tea. In Stage I, different SPE cartridges C18, graphite carbon black (GCB), primary secondary amine (PSA), and amino (NH2) were purchased and combined into 12 different sequences. Through the comparative test on cleanup efficiency of 84 representative pesticides in tea, Envi-Carb GCB + PSA with a good cleanup effect was selected. In Stage II, GC/MS test results from the comparative study of the extraction efficiency of 201 pesticides spiked into green tea and Woolong tea with Cleanert TPT and Envi-Carb + PSA SPE showed that average recoveries fell within 70-110% and RSD <20% for 193 and 184 pesticides, respectively, for green tea, accounting for 96.0 and 91.0% of the total number, respectively. GC/MS/MS test results also found 193 and 184 pesticides, respectively, meeting the recovery and RSD conditions, accounting for 96.0 and 91.5%, respectively, of the total number. For Woolong tea samples, GC/MS results showed that with Cleanert TPT and Envi-Carb + PSA SPE for cleanup, there were 192 and 177 pesticides, respectively, meeting the conditions, accounting for 95.5 and 88.1% of the total number, respectively. GC/MS/MS results demonstrated that there were 195 and 184 pesticides, respectively, meeting the conditions, accounting for 97.0 and 91.5% of the total number, respectively. It was seen that Cleanert TPT was superior to Envi-Carb + PSA in cleanup efficiency, whether for green or Woolong tea samples, or GC/MS or GC/MS/MS determination. In Stage III, 61104 results of the average content value of pesticides and RSD (two teas xtwo Youden pair concentrations x two kinds of SPE cartridges x two instruments x 19 tests x 201 pesticides) were derived from the 19 times stability tests over 3 months by paralleling three samples every 5 days via two instruments with two kinds of SPE cartridges for cleanup, respectively, against Youden Pair samples of the 201 incurred pesticides from green and Woolong teas. The statistical analysis found that detected values from the target pesticides of the incurred Youden pair samples showed no marked differences with cleanup by either Cleanert TPT or Envi-Carb + PSA, whether for green or Woolong tea, or G/IMS or G/IM/IMS. The test results using the two aforementioned kinds of SPE cleanup for above 93% pesticides had a tolerance less than 15%, which testifies that both cartridge cleanups met the requirement for pesticide residue analysis.

Determination of acrylamide in coffee and chocolate by pressurised fluid extraction and liquid chromatography-tandem mass spectrometry.

PubMed

Pardo, O; Yusà, V; Coscollà, C; León, N; Pastor, A

2007-07-01

A selective and sensitive procedure has been developed and validated for the determination of acrylamide in difficult matrices, such as coffee and chocolate. The proposed method includes pressurised fluid extraction (PFE) with acetonitrile, florisil clean-up purification inside the PFE extraction cell and detection by liquid chromatography (LC) coupled to atmospheric pressure ionisation in positive mode tandem mass spectrometry (APCI-MS-MS). Comparison of ionisation sources (atmospheric pressure chemical ionisation (APCI), atmospheric pressure photoionization (APPI) and the combined APCI/APPI) and clean-up procedures were carried out to improve the analytical signal. The main parameters affecting the performance of the different ionisation sources were previously optimised using statistical design of experiments (DOE). PFE parameters were also optimised by DOE. For quantitation, an isotope dilution approach was used. The limit of quantification (LOQ) of the method was 1 microg kg(-1) for coffee and 0.6 microg kg(-1) for chocolate. Recoveries ranged between 81-105% in coffee and 87-102% in chocolate. The accuracy was evaluated using a coffee reference test material FAPAS T3008. Using the optimised method, 20 coffee and 15 chocolate samples collected from Valencian (Spain) supermarkets, were investigated for acrylamide, yielding median levels of 146 microg kg(-1) in coffee and 102 microg kg(-1) in chocolate.

Fast determination of four polar contaminants in soy nutraceutical products by liquid chromatography coupled to tandem mass spectrometry.

PubMed

Domingos Alves, Renata; Romero-González, Roberto; López-Ruiz, Rosalía; Jiménez-Medina, M L; Garrido Frenich, Antonia

2016-11-01

An analytical method based on a modified QuPPe (quick polar pesticide) extraction procedure coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was evaluated for the determination of four polar compounds (chlorate, fosetyl-Al, maleic hydrazide, and perchlorate) in nutraceutical products obtained from soy. Experimental conditions including extraction such as solvent, acidification, time, and clean-up sorbents were varied. Acidified acetonitrile (1 % formic acid, v/v) was used as extraction solvent instead of methanol (conventional QuPPe), which provides a doughy mixture which cannot be injected into the LC. Clean-up or derivatization steps were avoided. For analysis, several stationary phases were evaluated and Hypercarb (porous graphitic carbon) provided the best results. The optimized method was validated and recoveries ranged between 46 and 119 %, and correction factors can be used for quantification purposes bearing in mind that inter-day precision was equal to or lower than 17 %. Limits of quantification (LOQs) ranged from 4 to 100 μg kg -1 . Soy-based nutraceutical products were analyzed and chlorate was detected in five samples at concentrations between 63 and 1642 μg kg -1 . Graphical Abstract Analysis of polar compounds in soy-based nutraceutical products.

Multi-residue method for the analysis of 85 current-use and legacy pesticides in bed and suspended sediments

USGS Publications Warehouse

Smalling, K.L.; Kuivila, K.M.

2008-01-01

A multi-residue method was developed for the simultaneous determination of 85 current-use and legacy organochlorine pesticides in a single sediment sample. After microwave-assisted extraction, clean-up of samples was optimized using gel permeation chromatography and either stacked carbon and alumina solid-phase extraction cartridges or a deactivated Florisil column. Analytes were determined by gas chromatography with ion-trap mass spectrometry and electron capture detection. Method detection limits ranged from 0.6 to 8.9 ??g/kg dry weight. Bed and suspended sediments from a variety of locations were analyzed to validate the method and 29 pesticides, including at least 1 from every class, were detected.

48 CFR 5119.1005 - Applicability.

Code of Federal Regulations, 2014 CFR

2014-10-01

... SMALL BUSINESS AND SMALL DISADVANTAGED BUSINESS CONCERNS Small Business Competitiveness Demonstration... (Dredging and Surface Cleanup Activities), limited to Federal Procurement Data Systems (FPDS) codes Y216 and...

48 CFR 5119.1005 - Applicability.

Code of Federal Regulations, 2011 CFR

2011-10-01

... SMALL BUSINESS AND SMALL DISADVANTAGED BUSINESS CONCERNS Small Business Competitiveness Demonstration... (Dredging and Surface Cleanup Activities), limited to Federal Procurement Data Systems (FPDS) codes Y216 and...

48 CFR 5119.1005 - Applicability.

Code of Federal Regulations, 2012 CFR

2012-10-01

... SMALL BUSINESS AND SMALL DISADVANTAGED BUSINESS CONCERNS Small Business Competitiveness Demonstration... (Dredging and Surface Cleanup Activities), limited to Federal Procurement Data Systems (FPDS) codes Y216 and...

48 CFR 5119.1005 - Applicability.

Code of Federal Regulations, 2013 CFR

2013-10-01

... SMALL BUSINESS AND SMALL DISADVANTAGED BUSINESS CONCERNS Small Business Competitiveness Demonstration... (Dredging and Surface Cleanup Activities), limited to Federal Procurement Data Systems (FPDS) codes Y216 and...

PETROCLEAN™

EPA Pesticide Factsheets

Technical product bulletin: this bioremediation agent is suitable for use in oil cleanups on hard surfaces with limited permeability such as concrete, permeable surfaces such as sand, and fresh or salt water.

Determination of formetanate hydrochloride in fruit samples using liquid chromatography-mass selective detection or -tandem mass spectrometry.

PubMed

Podhorniak, Lynda V; Kamel, Alaa; Rains, Diane M

2010-05-26

A rapid multiresidue method that captures residues of the insecticide formetanate hydrochloride (FHCl) in selected fruits is described. The method was used to provide residue data for dietary exposure determinations of FHCl. Using an acetonitrile extraction with a dispersive cleanup based on AOAC International method 2007.01, also known as QuEChERS, which was further modified and streamlined, thousands of samples were successfully analyzed for FHCl residues. FHCl levels were determined both by liquid chromatography-single-stage mass spectrometry (LC-MS) and ultraperformance liquid chromatography (UPLC)-tandem mass spectrometry (LC-MS/MS). The target limit of detection (LOD) and the limit of quantitation (LOQ) achieved for FHCl were 3.33 and 10 ng/g, respectively, with LC-MS and 0.1 and 0.3 ng/g, respectively, with LC-MS/MS. Recoveries at these previously unpublished levels ranged from 95 to 109%. A set of 20-40 samples can be prepared in one working day by two chemists.

Development of a rapid, simple and sensitive HPLC-FLD method for determination of rhodamine B in chili-containing products.

PubMed

Qi, Ping; Lin, Zhihao; Li, Jiaxu; Wang, ChengLong; Meng, WeiWei; Hong, Hong; Zhang, Xuewu

2014-12-01

In this work, a simple, rapid and sensitive analytical method for the determination of rhodamine B in chili-containing foodstuffs is described. The dye is extracted from samples with methanol and analysed without further cleanup procedure by high-performance liquid chromatography (HPLC) coupled to fluorescence detection (FLD). The influence of matrix fluorescent compounds (capsaicin and dihydrocapsaicin) on the analysis was overcome by the optimisation of mobile-phase composition. The limit of determination (LOD) and limit of quantification (LOQ) were 3.7 and 10 μg/kg, respectively. Validation data show a good repeatability and within-lab reproducibility with relative standard deviations <10%. The overall recoveries are in the range of 98-103% in chili powder and in the range of 87-100% in chili oil depending on the concentration of rhodamine B in foodstuffs. This method is suitable for the routine analysis of rhodamine B due to its sensitivity, simplicity, reasonable time and cost. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

Goltz, M.N.; Oxley, M.E.

Aquifer cleanup efforts at contaminated sites frequently involve operation of a system of extraction wells. It has been found that contaminant load discharged by extraction wells typically declines with time, asymptotically approaching a residual level. Such behavior could be due to rate-limited desorption of an organic contaminant from aquifer solids. An analytical model is presented which accounts for rate-limited desorption of an organic solute during cleanup of a contaminated site. Model equations are presented which describe transport of a sorbing contaminant in a converging radial flow field, with sorption described by (1) equilibrium, (2) first-order rate, and (3) Fickian diffusionmore » expressions. The model equations are solved in the Laplace domain and numerically inverted to simulate contaminant concentrations at an extraction well. A Laplace domain solution for the total contaminant mass remaining in the aquifer is also derived. It is shown that rate-limited sorption can have a significant impact upon aquifer remediation. Approximate equivalence among the various rate-limited models is also demonstrated.« less

Influence of orthodontic adhesives and clean-up procedures on the stain susceptibility of enamel after debonding.

PubMed

Joo, Hyun-Jin; Lee, Yong-Keun; Lee, Dong-Yul; Kim, Yae-Jin; Lim, Yong-Kyu

2011-03-01

To determine the influence of the type of orthodontic adhesive system, such as conventional acid-etching (CE) and self-etching primers (SEPs), on the stain susceptibility of enamel surface after debonding. Effects of clean-up procedures on the enamel surface were also determined. Two types and four brands of adhesive systems were investigated using 135 human premolars. Unbonded teeth were used as controls. Three-dimensional scanning of the enamel surface was performed before bracket bonding, after debonding, and after clean-up procedures. The color of each tooth was measured before bracket bonding and again after debonding and clean-up procedures. This was followed by methylene blue staining. The stain susceptibility of the enamel surface was measured after finishing only (F-condition) and after finishing/polishing (FP-condition). After debonding, the amount of residual adhesive resins in CE materials was greater than that in SEP materials. For the F-condition, staining color change in SEP materials was significantly higher than that in CE materials. For the FP-condition, staining color change in both CE and SEP materials was not different from those of the control. The SEP system would show less stain susceptibility if the thin residual adhesive resin layer after debonding is removed by polishing.

Determination of alkylphenols and 17beta-estradiol in fish homogenate. Extraction and clean-up strategies.

PubMed

Navarro, P; Bustamante, J; Vallejo, A; Prieto, A; Usobiaga, A; Arrasate, S; Anakabe, E; Puy-Azurmendi, E; Zuloaga, O

2010-09-17

The determination of target analytes such as nonyl- and octylphenols and 17beta-estradiol in fish homogenate require of solid-liquid extraction step. In this work microwave-assisted extraction (MAE) and focused-ultrasound liquid extraction (FUSLE) were studied as two different alternatives for extraction of the target compounds in zebrafish (Danio rerio) homogenate. In this work solid phase extraction (SPE) using 5-g and 10-g Florisil cartridges and gel permeation chromatography (GPC) were studied for the clean-up of the MAE and FUSLE extracts due to the non-selective extraction step. Although good recoveries were obtained both for SPE (106% and 126% range) and GPC (79% and 100% range) clean-up procedures, cleaner chromatograms were obtained after SPE and finally 5-g Florisil cartridges were tested since no improvement was observed when 10-g Florisil cartridges were used. Under optimized clean-up conditions, MAE and FUSLE provided comparable results for 4nOP and NP, while more accurate results were obtained for 4tOP and E2 after FUSLE. Finally, the method was applied to the determination of alkylphenols and 17beta-estradiol in zebrafish homogenate that had been exposed to known concentrations of the target analytes. In the case of alkylphenols two different isomers of nonyl- and octylphenol (4-(3',6'-dimethyl-3'-hepthyl)phenol, 363-NP, and 4-(3'-methyl-3'-hepthyl)phenol, 33-OP) were studied. 2010 Elsevier B.V. All rights reserved.

50 CFR 660.60 - Specifications and management measures.

Code of Federal Regulations, 2012 CFR

2012-10-01

... limits may be specified for the following species: longnose skate, big skate, California skate..., data collection, exploratory, health and safety, environmental cleanup, and/or hazard removal purposes...

ACT TERRA FIRMA

EPA Pesticide Factsheets

Technical product bulletin: this bioremediation agent is suitable for use in oil cleanups on hard surfaces with limited permeability such as concrete, permeable surfaces such as sand, and fresh or salt water.

Multi-class multi-residue analysis of veterinary drugs in meat using enhanced matrix removal lipid cleanup and liquid chromatography-tandem mass spectrometry.

PubMed

Zhao, Limian; Lucas, Derick; Long, David; Richter, Bruce; Stevens, Joan

2018-05-11

This study presents the development and validation of a quantitation method for the analysis of multi-class, multi-residue veterinary drugs using lipid removal cleanup cartridges, enhanced matrix removal lipid (EMR-Lipid), for different meat matrices by liquid chromatography tandem mass spectrometry detection. Meat samples were extracted using a two-step solid-liquid extraction followed by pass-through sample cleanup. The method was optimized based on the buffer and solvent composition, solvent additive additions, and EMR-Lipid cartridge cleanup. The developed method was then validated in five meat matrices, porcine muscle, bovine muscle, bovine liver, bovine kidney and chicken liver to evaluate the method performance characteristics, such as absolute recoveries and precision at three spiking levels, calibration curve linearity, limit of quantitation (LOQ) and matrix effect. The results showed that >90% of veterinary drug analytes achieved satisfactory recovery results of 60-120%. Over 97% analytes achieved excellent reproducibility results (relative standard deviation (RSD) < 20%), and the LOQs were 1-5 μg/kg in the evaluated meat matrices. The matrix co-extractive removal efficiency by weight provided by EMR-lipid cartridge cleanup was 42-58% in samples. The post column infusion study showed that the matrix ion suppression was reduced for samples with the EMR-Lipid cartridge cleanup. The reduced matrix ion suppression effect was also confirmed with <15% frequency of compounds with significant quantitative ion suppression (>30%) for all tested veterinary drugs in all of meat matrices. The results showed that the two-step solid-liquid extraction provides efficient extraction for the entire spectrum of veterinary drugs, including the difficult classes such as tetracyclines, beta-lactams etc. EMR-Lipid cartridges after extraction provided efficient sample cleanup with easy streamlined protocol and minimal impacts on analytes recovery, improving method reliability and consistency. Copyright © 2018 Elsevier B.V. All rights reserved.

Evaluation of beach cleanup effects using linear system analysis.

PubMed

Kataoka, Tomoya; Hinata, Hirofumi

2015-02-15

We established a method for evaluating beach cleanup effects (BCEs) based on a linear system analysis, and investigated factors determining BCEs. Here we focus on two BCEs: decreasing the total mass of toxic metals that could leach into a beach from marine plastics and preventing the fragmentation of marine plastics on the beach. Both BCEs depend strongly on the average residence time of marine plastics on the beach (τ(r)) and the period of temporal variability of the input flux of marine plastics (T). Cleanups on the beach where τ(r) is longer than T are more effective than those where τ(r) is shorter than T. In addition, both BCEs are the highest near the time when the remnants of plastics reach the local maximum (peak time). Therefore, it is crucial to understand the following three factors for effective cleanups: the average residence time, the plastic input period and the peak time. Copyright © 2014 Elsevier Ltd. All rights reserved.

46 CFR 68.25 - Purpose and scope.

Code of Federal Regulations, 2012 CFR

2012-10-01

... DOCUMENTATION OF VESSELS: EXCEPTIONS TO COASTWISE QUALIFICATION Documentation of Certain Vessels for Oil Spill... requirements are for the limited purposes of training for, implementing, and supporting oil spill cleanup...

46 CFR 68.25 - Purpose and scope.

Code of Federal Regulations, 2013 CFR

2013-10-01

... DOCUMENTATION OF VESSELS: EXCEPTIONS TO COASTWISE QUALIFICATION Documentation of Certain Vessels for Oil Spill... requirements are for the limited purposes of training for, implementing, and supporting oil spill cleanup...

46 CFR 68.25 - Purpose and scope.

Code of Federal Regulations, 2014 CFR

2014-10-01

... DOCUMENTATION OF VESSELS: EXCEPTIONS TO COASTWISE QUALIFICATION Documentation of Certain Vessels for Oil Spill... requirements are for the limited purposes of training for, implementing, and supporting oil spill cleanup...

Optimisation and validation of the analytical procedure for the determination of acrylamide in coffee by LC-MS/MS with SPE clean up.

PubMed

Gielecińska, Iwona; Mojska, Hanna

2013-01-01

Numerous studies have demonstrated acrylamide to be both neurotoxic and carcinogenic. At present it is widely recognised that acrylamide is mainly formed through the Maillard reaction from free asparagine and reducing sugars. The major sources of dietary acrylamide are potato products, processed cereals and coffee. To optimise and validate an analytical method for determining acrylamide in coffee by liquid chromatography and tandem mass spectrometry analysis (LC/MS/MS) using SPE clean-up. Analytical separation of acrylamide from roasted coffee was performed by liquid chromatography using a Hypercarb column followed by LC/MS/MS analysis, with 2,3,3-d3 acrylamide as an internal standard. The method was based on two purification steps: the first with hexane and Carrez solutions in order to remove of fat and to precipitate proteins, respectively; and the second with a solid-phase extraction (SPE) column which proved to be efficient in the elimination of the main chromatographic interferences. Limit of quantification (LOQ) for measuring acrylamide in coffee was 50 microg/kg. The described method demonstrates satisfactory precision (RSD = 2.5%), repeatability (RSD = 9.2%) and accuracy (mean recovery - 97.4%). Our results confirm that LC-MS/MS with SPE clean-up is selective and suitable for determination of acrylamide in coffee. Indeed, this method meets the criteria of EU Commission Recommendations (No. 2007/331/EC and No. 2010/307/EU), on the monitoring of acrylamide levels in food.

Matrix solid-phase dispersion followed by gas chromatography tandem mass spectrometry for the determination of benzotriazole UV absorbers in sediments.

PubMed

Carpinteiro, I; Abuín, B; Ramil, M; Rodríguez, I; Cela, R

2012-01-01

A cost-effective and low solvent consumption method, based on the matrix solid-phase dispersion (MSPD) technique, for the determination of six benzotriazole UV absorbers in sediments is presented. Sieved samples (0.5 g) were first mixed in a mortar with a solid sorbent and then transferred to a polypropylene syringe containing a layer of clean-up co-sorbent. Analytes were eluted with a suitable solvent and further determined by gas chromatography with tandem mass spectrometry (GC-MS/MS). Under final conditions, diatomaceous earth and silica, deactivated to 10%, were used as inert dispersant and clean-up co-sorbent, respectively. Analytes were recovered using just 5 mL of dichloromethane, and this extract was concentrated and exchanged to 1 mL of isooctane. Further removal of co-extracted sulphur was achieved adding activated copper powder to final extracts, which were stored overnight, before injection in the GC-MS/MS system. The accuracy of the method was assessed with river and marine sediment samples showing different carbon contents and spiked at different concentrations in the range from 40 to 500 ng g(-1). Recoveries varied between 78% and 110% with associated standard deviations below 14%. The limits of quantification of the method stayed between 3 and 15 ng g(-1). Levels of target compounds in sediment samples ranged from not detected up to a maximum of 56 ng g(-1) for Tinuvin 328.

A fully automated method for simultaneous determination of aflatoxins and ochratoxin A in dried fruits by pressurized liquid extraction and online solid-phase extraction cleanup coupled to ultra-high-pressure liquid chromatography-tandem mass spectrometry.

PubMed

Campone, Luca; Piccinelli, Anna Lisa; Celano, Rita; Russo, Mariateresa; Valdés, Alberto; Ibáñez, Clara; Rastrelli, Luca

2015-04-01

According to current demands and future perspectives in food safety, this study reports a fast and fully automated analytical method for the simultaneous analysis of the mycotoxins with high toxicity and wide spread, aflatoxins (AFs) and ochratoxin A (OTA) in dried fruits, a high-risk foodstuff. The method is based on pressurized liquid extraction (PLE), with aqueous methanol (30%) at 110 °C, of the slurried dried fruit and online solid-phase extraction (online SPE) cleanup of the PLE extracts with a C18 cartridge. The purified sample was directly analysed by ultra-high-pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for sensitive and selective determination of AFs and OTA. The proposed analytical procedure was validated for different dried fruits (vine fruit, fig and apricot), providing method detection and quantification limits much lower than the AFs and OTA maximum levels imposed by EU regulation in dried fruit for direct human consumption. Also, recoveries (83-103%) and repeatability (RSD < 8, n = 3) meet the performance criteria required by EU regulation for the determination of the levels of mycotoxins in foodstuffs. The main advantage of the proposed method is full automation of the whole analytical procedure that reduces the time and cost of the analysis, sample manipulation and solvent consumption, enabling high-throughput analysis and highly accurate and precise results.

Determination of polychlorinated biphenyls in fish: optimisation and validation of a method based on accelerated solvent extraction and gas chromatography-mass spectrometry.

PubMed

Ottonello, Giuliana; Ferrari, Angelo; Magi, Emanuele

2014-01-01

A simple and robust method for the determination of 18 polychlorinated biphenyls (PCBs) in fish was developed and validated. A mixture of acetone/n-hexane (1:1, v/v) was selected for accelerated solvent extraction (ASE). After the digestion of fat, the clean-up was carried out using solid phase extraction silica cartridges. Samples were analysed by GC-MS in selected ion monitoring (SIM) using three fragment ions for each congener (one quantifier and two qualifiers). PCB 155 and PCB 198 were employed as internal standards. The lowest limit of detection was observed for PCB 28 (0.4ng/g lipid weight). The accuracy of the method was verified by means of the Certified Reference Material EDF-2525 and good results in terms of linearity (R(2)>0.994) and recoveries (80-110%) were also achieved. Precision was evaluated by spiking blank samples at 4, 8 and 12ng/g. Relative standard deviation values for repeatability and reproducibility were lower than 8% and 16%, respectively. The method was applied to the determination of PCBs in 80 samples belonging to four Mediterranean fish species. The proposed procedure is particularly effective because it provides good recoveries with lowered extraction time and solvent consumption; in fact, the total time of extraction is about 12min per sample and, for the clean-up step, a total solvent volume of 13ml is required. Copyright © 2013 Elsevier Ltd. All rights reserved.

Cleanup/stimulation of a horizontal wellbore using propellants

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

Rougeot, J.E.; Lauterbach, K.A.

1993-01-01

This report documents the stimulation/cleanup of a horizontal well bore (Wilson 25) using propellants. The Wilson 25 is a Bartlesville Sand well located in the Flatrock Field, Osage County, Oklahoma. The Wilson 25 was drilled to determine if horizontal drilling could be used as a means to economically recover primary oil that had been left in place in a mostly abandoned oil field because of the adverse effects of water coning. Pump testing of the Wilson 25 horizontal well bore before cleanup or stimulation produced 6 barrels of oil and .84 barrels of water per day. The high percentage ofmore » daily oil production to total daily fluid production indicated that the horizontal well bore had accessed potentially economical oil reserves if the fluid production rate could be increased by performing a cleanup/stimulation treatment. Propellants were selected as an inexpensive means to stimulate and cleanup the near well bore area in a uniform manner. The ignition of a propellant creates a large volume of gas which penetrates the formation, creating numerous short cracks through which hydrocarbons can travel into the well bore. More conventional stimulation/cleanup techniques were either significantly more expensive, less likely to treat uniformly, or could not be confined to the near well bore area. Three different propellant torpedo designs were tested with a total of 304' of horizontal well bore being shot and producible. The initial test shot caused 400' of the horizontal well bore to become plugged off, and subsequently it could not be production tested. The second and third test shots were production tested, with the oil production being increased 458% and 349%, respectively, on a per foot basis. The Wilson 25 results indicate that a propellant shot treatment is an economically viable means to cleanup/stimulate a horizontal well bore.« less

Technical support for the EPA cleanup rule on radioactively contaminated sites

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

Hull, H.B.; Newman, A.; Wolbarst, A.B.

1995-12-31

The U.S. Environmental Protection Agency (EPA) is developing a radiation site cleanup regulation for the protection of the public from radionuclide contamination at sites that are to be cleaned up and released for public use. The regulation will apply to sites under the control of Federal agencies, and to sites licensed by the Nuclear Regulatory Commission (NRC) or NRC Agreement States. The agency is therefore conducting a comprehensive technical analysis aimed at developing information that will be used to support the rule. This presentation describes the regulation and the approach developed to determine how radiological health impacts and volumes ofmore » soil requiring remediation vary as functions of the possible cleanup dose or risk level.« less

Regression Analysis as a Cost Estimation Model for Unexploded Ordnance Cleanup at Former Military Installations

DTIC Science & Technology

2002-06-01

fits our actual data . To determine the goodness of fit, statisticians typically use the following four measures: R2 Statistic. The R2 statistic...reviewing instruction, searching existing data sources, gathering and maintaining the data needed, and completing and reviewing the collection of...mathematical model is developed to better estimate cleanup costs using historical cost data that could be used by the Defense Department prior to placing

Characterization and reclamation assessment for the Central Shops Diesel Storage Facility, Savannah River Site, Aiken, South Carolina

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

Fliermans, C.B.; Hazen, T.C.; Bledsoe, H.

1993-10-01

The contamination of subsurface terrestrial environments by organic contaminants is a global phenomenon. The remediation of such environments requires innovative assessment techniques and strategies for successful clean-ups. Central Shops Diesel Storage Facility at Savannah River Site was characterized to determine the extent of subsurface diesel fuel contamination using innovative approaches and effective bioremediation techniques for clean-up of the contaminant plume have been established.

U-PLANT GEOGRAPHIC ZONE CLEANUP PROTOTYPE

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

ROMINE, L.D.

2006-02-01

The U Plant geographic zone (UPZ) occupies 0.83 square kilometers on the Hanford Site Central Plateau (200 Area). It encompasses the U Plant canyon (221-U Facility), ancillary facilities that supported the canyon, soil waste sites, and underground pipelines. The UPZ cleanup initiative coordinates the cleanup of the major facilities, ancillary facilities, waste sites, and contaminated pipelines (collectively identified as ''cleanup items'') within the geographic zone. The UPZ was selected as a geographic cleanup zone prototype for resolving regulatory, technical, and stakeholder issues and demonstrating cleanup methods for several reasons: most of the area is inactive, sufficient characterization information is availablemore » to support decisions, cleanup of the high-risk waste sites will help protect the groundwater, and the zone contains a representative cross-section of the types of cleanup actions that will be required in other geographic zones. The UPZ cleanup demonstrates the first of 22 integrated zone cleanup actions on the Hanford Site Central Plateau to address threats to groundwater, the environment, and human health. The UPZ contains more than 100 individual cleanup items. Cleanup actions in the zone will be undertaken using multiple regulatory processes and decision documents. Cleanup actions will include building demolition, waste site and pipeline excavation, and the construction of multiple, large engineered barriers. In some cases, different cleanup actions may be taken at item locations that are immediately adjacent to each other. The cleanup planning and field activities for each cleanup item must be undertaken in a coordinated and cohesive manner to ensure effective execution of the UPZ cleanup initiative. The UPZ zone cleanup implementation plan (ZCIP) was developed to address the need for a fundamental integration tool for UPZ cleanup. As UPZ cleanup planning and implementation moves forward, the ZCIP is intended to be a living document that will provide a focal point for integrating UPZ actions, including field cleanup activities, waste staging and handling, and post-cleanup monitoring and institutional controls.« less

46 CFR 68.33 - Privileges of a limited coastwise endorsement.

Code of Federal Regulations, 2014 CFR

2014-10-01

... Certain Vessels for Oil Spill Cleanup § 68.33 Privileges of a limited coastwise endorsement. (a) A vessel...) To recover oil discharged into the water. (2) To transport oil discharged into the water. (3) To transport and deploy equipment, supplies, and personnel for recovering and transporting oil discharged into...

46 CFR 68.33 - Privileges of a limited coastwise endorsement.

Code of Federal Regulations, 2012 CFR

2012-10-01

... Certain Vessels for Oil Spill Cleanup § 68.33 Privileges of a limited coastwise endorsement. (a) A vessel...) To recover oil discharged into the water. (2) To transport oil discharged into the water. (3) To transport and deploy equipment, supplies, and personnel for recovering and transporting oil discharged into...

46 CFR 68.33 - Privileges of a limited coastwise endorsement.

Code of Federal Regulations, 2013 CFR

2013-10-01

... Certain Vessels for Oil Spill Cleanup § 68.33 Privileges of a limited coastwise endorsement. (a) A vessel...) To recover oil discharged into the water. (2) To transport oil discharged into the water. (3) To transport and deploy equipment, supplies, and personnel for recovering and transporting oil discharged into...

Impact of pH on the stability and the cross-reactivity of ochratoxin A and citrinin.

PubMed

Bazin, Ingrid; Faucet-Marquis, Virginie; Monje, Marie-Carmen; El Khoury, Micheline; Marty, Jean-Louis; Pfohl-Leszkowicz, Annie

2013-11-28

Mycotoxins are secondary metabolites produced by several fungi contaminating crops. In several countries, the maximum permitted levels of mycotoxins are found in foodstuffs and feedstuffs. The common strategy of mycotoxin analysis involves extraction, clean-up and quantification by chromatography. In this paper, we analyzed the reasons of underestimation of ochratoxin A (OTA) content in wine, and overestimation of OTA in wheat, depending on the pH of the clean-up step and the simultaneous presence of citrinin (CIT). We demonstrated that the increase of pH by adding polyethylene glycol (PEG) to wine led to an underestimation of OTA by conversion of OTA into open ring ochratoxin A OP-OA. In comparing three methods of extraction and clean-up for the determination of OTA and CIT in wheat--(i) an inter-laboratory validated method for OTA in cereals using immunoaffinity column clean-up (IAC) and extraction by acetonitrile/water; (ii) a validated method using IAC and extraction with 1% bicarbonate Na; and (iii) an in-house validated method based on acid liquid/liquid extraction--we observed an overestimation of OTA after immunoaffinity clean-up when CIT is also present in the sample, whereas an underestimation was observed when OTA was alone. Under neutral and alkaline conditions, CIT was partially recognized by OTA antibodies.

Impact of pH on the Stability and the Cross-Reactivity of Ochratoxin A and Citrinin

PubMed Central

Bazin, Ingrid; Faucet-Marquis, Virginie; Monje, Marie-Carmen; El Khoury, Micheline; Marty, Jean-Louis; Pfohl-Leszkowicz, Annie

2013-01-01

Mycotoxins are secondary metabolites produced by several fungi contaminating crops. In several countries, the maximum permitted levels of mycotoxins are found in foodstuffs and feedstuffs. The common strategy of mycotoxin analysis involves extraction, clean-up and quantification by chromatography. In this paper, we analyzed the reasons of underestimation of ochratoxin A (OTA) content in wine, and overestimation of OTA in wheat, depending on the pH of the clean-up step and the simultaneous presence of citrinin (CIT). We demonstrated that the increase of pH by adding polyethylene glycol (PEG) to wine led to an underestimation of OTA by conversion of OTA into open ring ochratoxin A OP-OA. In comparing three methods of extraction and clean-up for the determination of OTA and CIT in wheat—(i) an inter-laboratory validated method for OTA in cereals using immunoaffinity column clean-up (IAC) and extraction by acetonitrile/water; (ii) a validated method using IAC and extraction with 1% bicarbonate Na; and (iii) an in-house validated method based on acid liquid/liquid extraction—we observed an overestimation of OTA after immunoaffinity clean-up when CIT is also present in the sample, whereas an underestimation was observed when OTA was alone. Under neutral and alkaline conditions, CIT was partially recognized by OTA antibodies. PMID:24287570

Hollow fibre liquid phase micro-extraction by facilitated anionic exchange for the determination of flavonoids in faba beans (Vicia faba L.).

PubMed

Chaieb, Nadia; López-Mesas, Montserrat; Luis González, Johannes; Mars, Messaoud; Valiente, Manuel

2015-01-01

Flavonoids are polyphenolic compounds found ubiquitously in foods of plant origin. They are commonly extracted from plant materials with ethanol, methanol, water, their combination or even with acidified extracting solutions. The disadvantages of these methods are the use of high quantity of organic solvent, the possible loss of analytes in the different steps and the laborious process of the techniques. In addition, the complexity of the phenolic mixtures present in plant materials requires a preliminary clean-up and fractionation of the crude extracts. To develop a hollow fibre liquid phase micro-extraction (HF-LPME) method for a one step clean-up and pre-concentration of flavonoids. Two flavonoids (catechin and rutin) has been extracted by HF-LPME and analysed by HPLC. The related driving force for the liquid membrane has been studied by means of facilitated and non-facilitated transport. Different ionic and non-ionic water insoluble compounds [trioctylamine (TOA), tributyl phosphate (TBP), trioctylphosphine oxide (TOPO) and methyltrioctylammonium chloride (aliquat 336)] were used as carriers. The liquid membrane was constituted by a solution of n-decanol in the presence or absence of carriers. Maximum enrichment factors were obtained with n-decanol/aliquat 336 (20%) as organic liquid membrane, sodium hydroxide (NaOH) (0.1 M) as donor solution, sodium chloride (NaCl) (2 M) as acceptor solution and 3 h as extraction time. Under these conditions, good results for validation parameters were obtained [for linearity, limit of detection (LOD), limit of quantitation (LOQ) and repeatability]. The developed method is simple, effective and has been successfully applied to determine catechin and rutin in ethanolic extracts of faba beans. Copyright © 2015 John Wiley & Sons, Ltd.

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(-1) in a pear sample. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of parabens and endocrine-disrupting alkylphenols in soil by gas chromatography-mass spectrometry following matrix solid-phase dispersion or in-column microwave-assisted extraction: a comparative study.

PubMed

Pérez, R A; Albero, B; Miguel, E; Sánchez-Brunete, C

2012-03-01

Two rapid methods were evaluated for the simultaneous extraction of seven parabens and two alkylphenols from soil based on matrix solid-phase dispersion (MSPD) and microwave-assisted extraction (MAE). Soil extracts were derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide and analyzed by gas chromatography with mass spectrometry. Extraction and clean-up of samples were carried out by both methods in a single step. A glass sample holder, inside the microwave cell, was used in MAE to allow the simultaneous extraction and clean-up of samples and shorten the MAE procedure. The detection limits achieved by MSPD were lower than those obtained by MAE because the presence of matrix interferences increased with this extraction method. The extraction yields obtained by MSPD and MAE for three different types of soils were compared. Both procedures showed good recoveries and sensitivity for the determination of parabens and alkylphenols in two of the soils assayed, however, only MSPD yielded good recoveries with the other soil. Finally, MSPD was applied to the analysis of soils collected in different sites of Spain. In most of the samples analyzed, methylparaben and butylparaben were detected at levels ranging from 1.21 to 8.04 ng g(-1) dry weight and 0.48 to 1.02 ng g(-1) dry weight, respectively.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry

USGS Publications Warehouse

Furlong, E.T.; Vaught, D.G.; Merten, L.M.; Foreman, W.T.; Gates, Paul M.

1996-01-01

A method for the determination of 79 semivolatile organic compounds (SOCs) and 4 surrogate compounds in soils and bottom sediment is described. The SOCs are extracted from bottom sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography (GPC). The SOCs then are qualitatively identified and quantitative concentrations determined by capillary-column gas chromatography/mass spectrometry (GC/MS). This method also is designed for an optional simultaneous isolation of polychlorinated biphenyls (PCBs) and organochlorine (OC) insecticides, including toxaphene. When OCs and PCBs are determined, an additional alumina- over-silica column chromatography step follows GPC cleanup, and quantitation is by dual capillary- column gas chromatography with electron-capture detection (GC/ECD). Bottom-sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethane. The extract is concentrated, centrifuged, and then filtered through a 0.2-micrometer polytetrafluoro-ethylene syringe filter. Two aliquots of the sample extract then are quantitatively injected onto two polystyrene- divinylbenzene GPC columns connected in series. The SOCs are eluted with dichloromethane, a fraction containing the SOCs is collected, and some coextracted interferences, including elemental sulfur, are separated and discarded. The SOC-containing GPC fraction then is analyzed by GC/MS. When desired, a second aliquot from GPC is further processed for OCs and PCBs by combined alumina-over-silica column chromatography. The two fractions produced in this cleanup then are analyzed by GC/ECD. This report fully describes and is limited to the determination of SOCs by GC/MS.

Validation of a Chiral Liquid Chromatographic Method for the Degradation Behavior of Flumequine Enantiomers in Mariculture Pond Water.

PubMed

Wang, Yan-Fei; Gao, Xiao-Feng; Jin, Huo-Xi; Wang, Yang-Guang; Wu, Wei-Jian; Ouyang, Xiao-Kun

2016-09-01

In this work, flumequine (FLU) enantiomers were separated using a Chiralpak OD-H column, with n-hexane-ethanol (20:80, v/v) as the mobile phase at a flow rate of 0.6 mL/min. Solid phase extraction (SPE) was used for cleanup and enrichment. The limit of detection, limit of quantitation, linearity, precision, and intra/interday variation of the chiral high-performance liquid chromatography (HPLC) method were determined. The developed method was then applied to investigate the degradation behavior of FLU enantiomers in mariculture pond water samples. The results showed that the degradation of FLU enantiomers under natural, sterile, or dark conditions was not enantioselective. Chirality 28:649-655, 2016. © 2016 Wiley Periodicals, Inc. © 2016 Wiley Periodicals, Inc.

VERU-SOLVE™ MARINE 200 HP

EPA Pesticide Factsheets

Technical product bulletin: this surface washing agent used in oil spill cleanups separates the oil and water from the sand or soiled surface. Suitable for treating shorelines, beaches, rocks, marshes, sensitive environments, and access limited areas.

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.

Rapid gas chromatography with flame photometric detection of multiple organophosphorus pesticides in Salvia miltiorrhizae after ultrasonication assisted one-step extraction.

PubMed

Zhang, Shanshan; Liu, Xiaofei; Qin, Jia'an; Yang, Meihua; Zhao, Hongzheng; Wang, Yong; Guo, Weiying; Ma, Zhijie; Kong, Weijun

2017-11-15

A simple and rapid gas chromatography-flame photometric detection (GC-FPD) method was developed for the determination of 12 organophosphorus pesticides (OPPs) in Salvia miltiorrhizae by using ultrasonication assisted one-step extraction (USAE) without any clean-up steps. Some crucial parameters such as type of extraction solvent were optimized to improve the method performance for trace analysis. Any clean-up steps were negligent as no interferences were detected in the GC-FPD chromatograms for sensitive detection. Under the optimized conditions, limits of detection (LODs) and quantitation (LOQs) for all pesticides were in the range of 0.001-0.002mg/kg and 0.002-0.01mg/kg and 0.002-0.01mg/kg, respectively, which were all below the regulatory maximum residue limits suggested. RSDs for method precision (intra- and inter-day variations) were lower than 6.8% in approval with international regulations. Average recovery rates for all pesticides at three fortification levels (0.5, 1.0 and 5.0mg/kg) were in the range of 71.2-101.0% with relative standard deviations (RSDs) <13%. The developed method was evaluated for its feasibility in the simultaneous pre-concentration and determination of 12 OPPs in 32 batches of real S. miltiorrhizae samples. Only one pesticide (dimethoate) out of the 12 targets was simultaneously detected in four samples at concentrations of 0.016-0.02mg/kg. Dichlorvos and omethoate were found in the same sample from Sichuan province at 0.004 and 0.027mg/kg, respectively. Malathion and monocrotophos were determined in the other two samples at 0.014 and 0.028mg/kg, respectively. All the positive samples were confirmed by LC-MS/MS. The simple, reliable and rapid USAE-GC-FPD method with many advantages over traditional techniques would be preferred for trace analysis of multiple pesticides in more complex matrices. Copyright © 2017 Elsevier B.V. All rights reserved.

PERCHLORATE: Occurrence is Widespread but at Varying Levels; Federal Agencies Have Taken Some Actions to Respond to and Lessen Releases

DTIC Science & Technology

2010-08-01

Massachusetts Military Reservation Army/Air Force Active Groundwater Soil 770 8,060 Remediation under way MA Fort Devens Army Active Groundwater 133...cleanup, known as a remedial action . • CERCLA itself does not establish cleanup standards. Rather, the remedial action chosen by a federal agency...perchlorate contaminated areas, which could determine the need for and feasibility of remedial action . • Edwards Air Force Base. In 1997 and 1998

Screening method for the determination of tetracyclines and fluoroquinolones in animal drinking water by liquid chromatography with diode array detector.

PubMed

Patyra, E; Kowalczyk, E; Grelik, A; Przeniosło-Siwczyńska, M; Kwiatek, K

2015-01-01

A liquid chromatography - diode array detector (HPLC-DAD) procedure has been developed for the determination of oxytetracycline (OTC), tetracycline (TC), chlorotetracycline (CTC), doxycycline (DC), enrofloxacin (ENR), ciprofloxacin (CIP), sarafloxacin (SAR) and flumequine (FLU) residues in animal drinking water. This method was applied to animal drinking water. Solid-phase extraction (SPE) clean-up on an Oasis HLB cartridge allowed an extract suitable for liquid chromatographic analysis to be obtained. Chromatographic separation was carried out on a C18 analytical column, using gradient elution with 0.1% trifluoroacetic acid - acetonitrile - methanol at 30°C. The flow-rate was 0.7 mL/min and the eluate was analysed at 330 nm. The whole procedure was evaluated according to the requirements of the Commission Decision 2002/657/EC, determining specificity, decision limit (CCα), detection capacity (CCβ), limit of detection (LOD), limit of quantification (LOQ), precision and accuracy during validation of the method. The recoveries of TCs and FQs from spiked samples at the levels of 10, 100 and 1000 μg/L were higher than 82%. The developed method based on HPLC-DAD has been applied for the determination of four tetracyclines and four fluoroquinolones in animal drinking water samples.

A modified extraction and clean-up procedure for the detection and determination of parathion-methyl and chlorpyrifos residues in tea.

PubMed

Shanker, A; Sood, C; Kumar, V; Ravindranath, S D

2001-05-01

Recent advances in methodology and instrumentation have made possible the detection and determination of pesticides at microgram kg-1 (ppb) levels. The sensitivity of a method of analysis depends greatly on the efficient extraction of the pesticide and the subsequent clean-up of the extract. The extract from green tea leaves is a mixture of aroma components, polyphenols and caffeine. The preparation of made tea from green tea leaves adds to this complexity by concentrating these coextractives. Conventional clean-up techniques provide poor recoveries for parathion-methyl and chlorpyrifos from both green tea leaves and made tea. This arises from interference by caffeine during gas chromatography, as it has a similar retention time to the two pesticides and peaks overlap. A modification to the protocol based on a solvent partitioning process using dichloromethane and subsequent washing of the extracts with warm water removed the caffeine, and pigments were removed by column chromatography. Recoveries ranging from 80 to 90% were then obtained for both pesticides.

Doses of Ukrainian female clean-up workers with diagnosed breast cancer.

PubMed

Chumak, Vadim V; Klymenko, Sergiy V; Zitzelsberger, Horst; Wilke, Christina; Rybchenko, Lyudmila A; Bakhanova, Elena V

2018-05-01

The Chernobyl reactor accident in 1986 has caused significant exposure to ionizing radiation of the Ukrainian population, in particular clean-up workers and evacuees from the exclusion zones. A study aiming at the discovery of radiation markers of the breast cancer was conducted from 2008 to 2015 within a collaborative project by HZM, LMU, and NRCRM. In this study, post-Chernobyl breast cancer cases both in radiation-exposed female patients diagnosed at age less than 60 from 1992 to 2014 and in non-exposed controls matched for residency, tumor type, age at diagnosis, TNM classification as well as tumor grading were investigated for molecular changes with special emphasis to copy number alterations and miRNA profiles. Cancer registry and clinical archive data were used to identify 435 breast cancer patients among female clean-up workers and 14 among evacuees from highly contaminated territories as candidates for the study. Of these, 129 breast cancer patients fit study inclusion criteria and were traced for individual reconstruction of the target organ (breast) doses. The doses were estimated for 71 exposed cases (clean-up workers and evacuees from which biomaterial was available for molecular studies and who agreed to participate in a dosimetric interview) by the use of the well-established RADRUE method, which was adjusted specifically for the assessment of breast doses. The results of 58 female clean-up workers showed a large inter-individual variability of doses in a range of about five orders of magnitude: from 0.03 to 929 mGy, with median of 5.8 mGy. The study provides the first quantitative estimate of exposures received by female clean-up workers, which represent a limited but very important group of population affected by the Chernobyl accident. The doses of 13 women evacuated after the accident who did not take part in the clean-up activities (from 4 to 45 mGy with median of 19 mGy) are in line with the previous estimates for the evacuees from Pripyat and the 30-km zone.

Development and validation of a solid-phase extraction method coupled to liquid chromatography with fluorescence detection for the determination of fluoroquinolone residues in powdered infant formulae. Application to the analysis of samples from the Spanish and Latin American market.

PubMed

Rodriguez, E; Moreno-Bondi, M C; Marazuela, M D

2008-10-31

This paper describes a new method for the effective extraction, clean-up and chromatographic analysis of residues of four fluoroquinolones (ciprofloxacin, enrofloxacin, danofloxacin and sarafloxacin) in powdered infant formulae and follow-on preparations. Samples were reconstituted following the manufacturer's recommendations and treated with trichloroacetic acid in methanol 10% (w/v) for deproteinization. Two solid-phase extraction cartridges have been evaluated for sample clean-up and preconcentration, Strata Screen A and Strata X and the later provided the best recoveries for all the analytes tested. Chromatographic analysis has been carried out using a polar endcapped column (AQUA C(18)) and fluorescence detection, with lomefloxacin (LOME) as internal standard. Method validation has been performed according to European Commission Decision 2002/657/EC criteria, in terms of linearity, recovery, precision, specificity, decision limit (CC(alpha)) and detection capability (CC(beta)). Typical recoveries ranged between 70 and 110% at levels below and above the maximum residue limits of the target analytes in bovine milk, with an excellent intralab reproducibility (RSDs<7%). Matrix effects did not significantly affect method accuracy, as evidenced by analyzing different brands of milk. The method has been successfully applied to the analysis of 100 samples of infant and follow-on formulae of the Spanish and Latin American market, using LC-MS/MS as confirmatory technique.

Validation of an Analytical Method for the Determination of Pesticide Residues in Vine Leaves by GC-MS/MS.

PubMed

Maestroni, Britt; Abu Alnaser, Amer; Ghanem, Iyad; Islam, Marivil; Cesio, Veronica; Heinzen, Horacio; Kelly, Simon; Cannavan, Andrew

2018-06-27

A modified and miniaturized SweEt/QuEChERS method for pesticide residue analysis applied to vine leaves is presented. The deep-frozen plant material was cryogenically processed. A 2 g analytical portion was hydrated for 30 min and extracted with acidified ethyl acetate after buffering with NaHCO 3 and adding Na 2 SO 4 . A dispersive solid-phase (d-SPE) cleanup step with primary-secondary amine (PSA) was performed. The pesticide residues were determined using GC-MS/MS. The whole procedure was validated for 54-59 pesticides at 0.01, 0.02, 0.1, and 0.2 mg/kg in fresh vine leaves ( Vitis vinifera). The key method performance parameters investigated were specificity, linearity, trueness, within laboratory repeatability and reproducibility, limit of detection, limit of quantitation, and matrix effects. Recoveries for the 59 pesticides tested ranged from 60 to 110%, and the RSDs were lower than 20% for the majority of the pesticides studied.

A generic method for the determination of acrylamide in thermally processed foods.

PubMed

Gökmen, Vural; Senyuva, Hamide Z

2006-07-07

A generic sample preparation method for the determination of acrylamide in foods was developed. The method entails extraction with methanol, purification with Carrez I and II solutions, evaporation and solvent change to water, and cleanup with Oasis HLB solid-phase extraction (SPE) cartridge. The final extract was analyzed by liquid chromatography-mass spectrometry (LC-MS) for quantitation. The chromatographic separation was performed on ODS-3 column using the isocratic mixture of 0.01 mM acetic acid in 0.2% aqueous solution of formic acid at a flow rate of 0.6 ml/min at 25 degrees C. The recoveries of acrylamide from potato chips, biscuits and coffee ranged between 92.8 and 101.5% with relative standard deviations of 4.1% or less. The limit of detection (LOD) and the limit of quantitation (LOQ) were 2 ng/g and 6 ng/g in the basis of signal to noise ratios of 3:1 and 9:1, respectively.

Micro-solid-phase extraction (µ-SPE) of organophosphorous pesticides from wheat followed by LC-MS/MS determination.

PubMed

Della Pelle, Flavio; Di Crescenzo, Maria Chiara; Sergi, Manuel; Montesano, Camilla; Di Ottavio, Francesca; Scarpone, Rossana; Scortichini, Giampiero; Compagnone, Dario

2016-01-01

A rapid, selective and effective method of extraction, clean-up and concentration of organophosphorous pesticides from wheat followed by electrospray (ESI) LC-MS/MS analysis was developed. The μ-SPE (micro-solid-phase extraction) procedure resulted in good analytical performance and reduced at the same time matrix effects, analysis time and solvent consumption. Limits of detection (LODs) and quantification (LOQs) were in the range of 0.3-10 and 1-30 μg kg(-1), respectively, with good reproducibility (RSD ≤ 13.8) and recoveries between 75% and 109%. Coefficients of determination (r(2)) were greater than 0.996 for the studied pesticides. Despite the reduced sorbent bed mass of μ-SPE tips (4.2 mg), the analytical data showed that no saturation phenomena occurs in the tested range of concentration both for single compounds and mixtures. Several real samples were analysed and the concentrations of the selected pesticides were found to be below the respective maximum residue limit (MRLs).

Specific determination of bromate in bread by ion chromatography with ICP-MS.

PubMed

Akiyama, Takumi; Yamanaka, Michiko; Date, Yukiko; Kubota, Hiroki; Nagaoka, Megumi Hamano; Kawasaki, Yoko; Yamazaki, Takeshi; Yomota, Chikako; Maitani, Tamio

2002-12-01

A sensitive method for detecting bromate in bread by ion chromatography with inductively-coupled plasma mass spectrometry (IC/ICP-MS) was developed. Bromate was extracted from bread with water. The clean-up procedure included a 0.2 micron filter, a C18 cartridge for defatting, a silver cartridge to remove halogen anions, a centrifugal ultrafiltration unit to remove proteins, and a cation-exchange cartridge to remove silver ions. A 500 microL sample solution was applied to IC/ICP-MS. The detection limit and the quantitation limit of bromate in the solution were 0.3 ng/mL and 1.0 ng/mL, expressed as HBrO3, respectively, which corresponded to 2 ng/g and 5 ng/g, respectively, in bread. Recovery of bromate was about 90%, and the CV was about 2%. Based on the detection limit in solution and recovery from bread, the detection limit of bromate in bread was estimated to be 2 ng/g.

Refined methodology for the determination of neonicotinoid pesticides and their metabolites in honey bees and bee products by liquid chromatography-tandem mass spectrometry (LC-MS/MS).

PubMed

Kamel, Alaa

2010-05-26

An analytical method was refined for the extraction and determination of neonicotinoid pesticide residues and their metabolites in honey bees and bee products. Samples were extracted with 2% triethylamine (TEA) in acetonitrile (ACN) followed by salting out, solid phase extraction (SPE) cleanup, and detection using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method was validated in triplicate at three fortification concentrations in each matrix. Good recoveries were observed for most analytes and ranged between 70 and 120% with relative standard deviations between replicates of <20% in most cases. The method limits of detection were 0.2 ng/g for the parent neonicotinoid pesticides and ranged between 0.2 and 15 ng/g for the neonicotinoid metabolites. This refined method provides lower detection limits and improved recovery of neonicotinoids and their metabolites, which will help researchers evaluate subchronic effects of these pesticides, address data gaps related to colony collapse disorder (CCD), and determine the role of pesticides in pollinator decline.

Liquid chromatographic determination of urinary 5-methyl-2'-deoxycytidine and pseudouridine as potential biological markers for leukaemia.

PubMed

Zambonin, C G; Aresta, A; Palmisano, F; Specchia, G; Liso, V

1999-12-01

A simple reversed-phase liquid chromatographic (LC) method for the determination of urinary 5-methyl-2'-deoxycytidine (m5dCyd), recently claimed (on the basis of an imuno-technique) to be a potential marker for leukaemia, has been developed. Sample pre-treatment is based on a microcolumn clean-up step with an average recovery of 79% and a RSD of 3%. Detection limit was 0.2 microg/ml which is about tenfold lower than levels previously measured by an ELISA method in urine of healthy individuals. The creatinine (Cre) excretion, necessary for normalising the m5dCyd excretion, was evaluated by ion-pair liquid chromatography which permitted the simultaneous determination of pseudouridine (psi), a modified nucleoside also potentially useful as a marker for leukaemia. The described LC procedures were applied to the analysis of urine samples from healthy individuals and leukaemia patients. While the urinary psi/Cre ratio was found significantly increased for leukaemia patients, the urinary m5dCyd levels in healthy individuals were below the detection limits and did not increase in presence of the malignant disease.

Application of an activated carbon-based support for magnetic solid phase extraction followed by spectrophotometric determination of tartrazine in commercial beverages.

PubMed

Rodríguez, José A; Escamilla-Lara, Karen A; Guevara-Lara, Alfredo; Miranda, Jose M; Páez-Hernández, Ma Elena

2015-01-01

A method is presented for magnetic solid phase extraction of tartrazine from nonalcoholic beverages. The method involves the extraction and clean-up by activated carbon covered with magnetite dispersed in the sample, followed by the magnetic isolation and desorption of the analyte by basified methanol. The tartrazine eluted from the magnetic support was determined by spectrophotometry. Under optimal conditions, the linear range of the calibration curve ranges from 3 to 30 mg L(-1), with a limit of detection of 1 mg L(-1). The method was validated by comparing the results with those obtained by HPLC. A precision of <5.0% was obtained in all cases and no significant differences were observed (P < 0.05).

Application of an Activated Carbon-Based Support for Magnetic Solid Phase Extraction Followed by Spectrophotometric Determination of Tartrazine in Commercial Beverages

PubMed Central

Rodríguez, José A.; Escamilla-Lara, Karen A.; Guevara-Lara, Alfredo; Miranda, Jose M.

2015-01-01

A method is presented for magnetic solid phase extraction of tartrazine from nonalcoholic beverages. The method involves the extraction and clean-up by activated carbon covered with magnetite dispersed in the sample, followed by the magnetic isolation and desorption of the analyte by basified methanol. The tartrazine eluted from the magnetic support was determined by spectrophotometry. Under optimal conditions, the linear range of the calibration curve ranges from 3 to 30 mg L−1, with a limit of detection of 1 mg L−1. The method was validated by comparing the results with those obtained by HPLC. A precision of <5.0% was obtained in all cases and no significant differences were observed (P < 0.05). PMID:25873965

Determination of pesticides in sewage sludge from an agro-food industry using QuEChERS extraction followed by analysis with liquid chromatography-tandem mass spectrometry.

PubMed

Ponce-Robles, Laura; Rivas, Gracia; Esteban, Belen; Oller, Isabel; Malato, Sixto; Agüera, Ana

2017-10-01

An analytical method was developed and validated for the determination of ten pesticides in sewage sludge coming from an agro-food industry. The method was based on the application of Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction for solid sewage sludge and SPE extraction for sludge aqueous phase, followed by liquid chromatography (LC) coupled to hybrid quadrupole/linear ion trap mass spectrometry (QqLIT-MS). The QuEChERS method was reported 14 years ago and nowadays is mainly applied to the analysis of pesticides in food. More recent applications have been reported in other matrices as sewage sludge, but the complexity of the matrix makes necessary the optimization of the cleanup step to improve the efficiency of the analysis. With this aim, several dispersive solid-phase extraction cleanup sorbents were tested, choosing C18 + PSA as a d-SPE sorbent. The proposed method was satisfactorily validated for most compounds investigated, showing recoveries higher than 80% in most cases, with the only exception of prochloraz (71%) at low concentration level. Limits of quantification were lower than 40 ng l -1 in the aqueous phase and below 40 ng g -1 in the solid phase for the majority of the analytes. The method was applied to solid sludge and the sludge aqueous phase coming from an agro-food industry which processes fruits and vegetables. Graphical abstract Application of LC/MS/MS advanced analytical techniques for determination of pesticides contained in sewage sludge.

Primary secondary amine as a sorbent material in dispersive solid-phase extraction clean-up for the determination of indicator polychlorinated biphenyls in environmental water samples by gas chromatography with electron capture detection.

PubMed

Guo, Yuanming; Hu, Hongmei; Li, Tiejun; Xue, Lijian; Zhang, Xiaoning; Zhong, Zhi; Zhang, Yurong; Jin, Yanjian

2017-08-01

A simple, rapid, and novel method has been developed and validated for determination of seven indicator polychlorinated biphenyls in water samples by gas chromatography with electron capture detection. 1 L of water samples containing 30 g of anhydrous sodium sulfate was first liquid-liquid extracted with an automated Jipad-6XB vertical oscillator using n-hexane/dichloromethane (1:1, v/v). The concentrated extract was cleaned up by dispersive solid-phase extraction with 100 mg of primary secondary amine as sorbent material. The linearity of this method ranged from 1.25 to 100 μg/L, with regression coefficients ranging between 0.9994 and 0.9999. The limits of detection were in the ng/L level, ranging between 0.2 and 0.3 ng/L. The recoveries of seven spiked polychlorinated biphenyls with external calibration method at different concentration levels in tap water, lake water, and sea water were in the ranges of 85-112, 76-116, and 72-108%, respectively, and with relative standard deviations of 3.3-4.5, 3.4-5.6, and 3.1-4.8% (n = 5), respectively. The performance of the proposed method was compared with traditional liquid-liquid extraction and solid-phase extraction clean-up methods, and comparable efficiencies were obtained. It is concluded that this method can be successfully applied for the determination of polychlorinated biphenyls in different water samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Multiresidue determination of pesticides in malt beverages by capillary gas chromatography with mass spectrometry and selected ion monitoring.

PubMed

Wong, Jon W; Webster, Michael G; Bezabeh, Dawit Z; Hengel, Mathew J; Ngim, Kenley K; Krynitsky, Alexander J; Ebeler, Susan E

2004-10-20

A method was developed to determine pesticides in malt beverages using solid phase extraction on a polymeric cartridge and sample cleanup with a MgSO4-topped aminopropyl cartridge, followed by capillary gas chromatography with electron impact mass spectrometry in the selected ion monitoring mode [GC-MS(SIM)]. Three GC injections were required to analyze and identify organophosphate, organohalogen, and organonitrogen pesticides. The pesticides were identified by the retention times of peaks of the target ion and qualifier-to-target ion ratios. GC detection limits for most of the pesticides were 5-10 ng/mL, and linearity was determined from 50 to 5000 ng/mL. Fortification studies were performed at 10 ng/mL for three malt beverages that differ in properties such as alcohol content, solids, and appearance. The recoveries from the three malt beverages were greater than 70% for 85 of the 142 pesticides (including isomers) studied. The data showed that the different malt beverage matrixes had no significant effect on the recoveries. This method was then applied to the screening and analysis of malt beverages for pesticides, resulting in the detection of the insectide carbaryl and the fungicide dimethomorph in real samples. The study indicates that pesticide levels in malt beverages are significantly lower than the tolerance levels set by the United States Environmental Protection Agency for malt beverage starting ingredients. The use of the extraction/cleanup procedure and analysis by GC-MS(SIM) proved effective in screening malt beverages for a wide variety of pesticides. Copyright 2004 American Chemical Society

Cleanup/stimulation of a horizontal wellbore using propellants. Final report

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

Rougeot, J.E.; Lauterbach, K.A.

1993-01-01

This report documents the stimulation/cleanup of a horizontal well bore (Wilson 25) using propellants. The Wilson 25 is a Bartlesville Sand well located in the Flatrock Field, Osage County, Oklahoma. The Wilson 25 was drilled to determine if horizontal drilling could be used as a means to economically recover primary oil that had been left in place in a mostly abandoned oil field because of the adverse effects of water coning. Pump testing of the Wilson 25 horizontal well bore before cleanup or stimulation produced 6 barrels of oil and .84 barrels of water per day. The high percentage ofmore » daily oil production to total daily fluid production indicated that the horizontal well bore had accessed potentially economical oil reserves if the fluid production rate could be increased by performing a cleanup/stimulation treatment. Propellants were selected as an inexpensive means to stimulate and cleanup the near well bore area in a uniform manner. The ignition of a propellant creates a large volume of gas which penetrates the formation, creating numerous short cracks through which hydrocarbons can travel into the well bore. More conventional stimulation/cleanup techniques were either significantly more expensive, less likely to treat uniformly, or could not be confined to the near well bore area. Three different propellant torpedo designs were tested with a total of 304` of horizontal well bore being shot and producible. The initial test shot caused 400` of the horizontal well bore to become plugged off, and subsequently it could not be production tested. The second and third test shots were production tested, with the oil production being increased 458% and 349%, respectively, on a per foot basis. The Wilson 25 results indicate that a propellant shot treatment is an economically viable means to cleanup/stimulate a horizontal well bore.« less

46 CFR 68.29 - Citizenship requirements for limited coastwise endorsement.

Code of Federal Regulations, 2013 CFR

2013-10-01

... Documentation of Certain Vessels for Oil Spill Cleanup § 68.29 Citizenship requirements for limited coastwise... issued to a vessel owned by— (1) A not-for-profit oil spill response cooperative if the vessel meets the requirements of paragraph (b) of this section; or (2) A member or members of a not-for-profit oil spill...

46 CFR 68.29 - Citizenship requirements for limited coastwise endorsement.

Code of Federal Regulations, 2014 CFR

2014-10-01

... Documentation of Certain Vessels for Oil Spill Cleanup § 68.29 Citizenship requirements for limited coastwise... issued to a vessel owned by— (1) A not-for-profit oil spill response cooperative if the vessel meets the requirements of paragraph (b) of this section; or (2) A member or members of a not-for-profit oil spill...

46 CFR 68.31 - Vessel eligibility requirements for limited coastwise endorsement.

Code of Federal Regulations, 2013 CFR

2013-10-01

... Documentation of Certain Vessels for Oil Spill Cleanup § 68.31 Vessel eligibility requirements for limited... vessel was formerly owned by a not-for-profit oil spill response cooperative or by one or more members of a not-for-profit oil spill response cooperative and the vessel meets the criteria of § 68.29. [CGD...

46 CFR 68.31 - Vessel eligibility requirements for limited coastwise endorsement.

Code of Federal Regulations, 2012 CFR

2012-10-01

... Documentation of Certain Vessels for Oil Spill Cleanup § 68.31 Vessel eligibility requirements for limited... vessel was formerly owned by a not-for-profit oil spill response cooperative or by one or more members of a not-for-profit oil spill response cooperative and the vessel meets the criteria of § 68.29. [CGD...

46 CFR 68.29 - Citizenship requirements for limited coastwise endorsement.

Code of Federal Regulations, 2012 CFR

2012-10-01

... Documentation of Certain Vessels for Oil Spill Cleanup § 68.29 Citizenship requirements for limited coastwise... issued to a vessel owned by— (1) A not-for-profit oil spill response cooperative if the vessel meets the requirements of paragraph (b) of this section; or (2) A member or members of a not-for-profit oil spill...

46 CFR 68.31 - Vessel eligibility requirements for limited coastwise endorsement.

Code of Federal Regulations, 2014 CFR

2014-10-01

... Documentation of Certain Vessels for Oil Spill Cleanup § 68.31 Vessel eligibility requirements for limited... vessel was formerly owned by a not-for-profit oil spill response cooperative or by one or more members of a not-for-profit oil spill response cooperative and the vessel meets the criteria of § 68.29. [CGD...

Comparison of methods and optimisation of the analysis of fumonisins B₁ and B₂ in masa flour, an alkaline cooked corn product.

PubMed

De Girolamo, A; Pascale, M; Visconti, A

2011-05-01

A comparison study of different extraction and clean-up procedures for the liquid chromatographic analysis of fumonisins B(1) (FB(1)) and B(2) (FB(2)) in corn masa flour was performed. The procedures included extraction (heat or room temperature) with acidic conditions or EDTA-containing solvents, and clean-up by immunoaffinity or C18 solid-phase extraction columns. Thereafter an analytical method was optimised using extraction with an acidic mixture of methanol-acetonitrile-citrate/phosphate buffer, clean-up through the immunoaffinity column and determination of fumonisins by liquid chromatography with automated pre-column derivatisation with o-phthaldialdehyde reagent. Recovery experiments performed on yellow, white and blue masa flours at spiking levels of 400, 800 and 1200 µg kg(-1) FB(1) and of 100, 200 and 300 µg kg(-1) FB(2) gave overall mean recoveries of 99% (±6%) for FB(1) and 88% (±6%) for FB(2). Good recoveries (higher than 90% for both FB(1) and FB(2)) were also obtained with corn tortilla chips. The limits of quantification of the method (signal-to-noise ratio of 10) were 25 µg kg(-1) for FB(1) and 17 µg kg(-1) for FB(2). The method was tested on different commercial corn masa flours as well as on white and yellow corn tortilla chips, showing fumonisin contamination levels (FB(1) + FB(2)) up to 1800 µg kg(-1) (FB(1) + FB(2)) in masa flour and 960 µg kg(-1) in tortilla chips. Over 30% of masa flours originating from Mexico exceeded the European Union maximum permitted level.

A sensitive and efficient method for routine pesticide multiresidue analysis in bee pollen samples using gas and liquid chromatography coupled to tandem mass spectrometry.

PubMed

Vázquez, P Parrilla; Lozano, A; Uclés, S; Ramos, M M Gómez; Fernández-Alba, A R

2015-12-24

Several clean-up methods were evaluated for 253 pesticides in pollen samples concentrating on efficient clean-up and the highest number of pesticides satisfying the recovery and precision criteria. These were: (a) modified QuEChERS using dSPE with PSA+C18; (b) freeze-out prior to QuEChERS using dSPE with PSA+C18; (c) freeze-out prior to QuEChERS using dSPE with PSA+C18+Z-Sep; and (d) freeze-out followed by QuEChERS using dSPE with PSA+C18 and SPE with Z-Sep. Determinations were made using LC-MS/MS and GC-MS/MS. The modified QuEChERS protocol applying a freeze-out followed by dSPE with PSA+C18 and SPE clean-up with Z-Sep was selected because it provided the highest number of pesticides with mean recoveries in the 70-120% range, as well as relative standard deviations (RSDs) typically below 20% (12.2% on average) and ensured much better removal of co-extracted matrix compounds of paramount importance in routine analysis. Limits of quantification at levels as low as 5μgkg(-1) were obtained for the majority of the pesticides. The proposed methodology was applied to the analysis of 41 pollen bee samples from different areas in Spain. Pesticides considered potentially toxic to bees (DL50<2μg/bee) were detected in some samples with concentrations up to 72.7μgkg(-1), which could negatively affect honeybee health. Copyright © 2015 Elsevier B.V. All rights reserved.

Development and validation of a solid phase extraction sample cleanup procedure for the recovery of trace levels of nitro-organic explosives in soil.

PubMed

Thomas, Jennifer L; Donnelly, Christopher C; Lloyd, Erin W; Mothershead, Robert F; Miller, Mark L

2018-03-01

An improved cleanup method has been developed for the recovery of trace levels of 12 nitro-organic explosives in soil, which is important not only for the forensic community, but also has environmental implications. A wide variety of explosives or explosive-related compounds were evaluated, including nitramines, nitrate esters, nitroaromatics, and a nitroalkane. Fortified soil samples were extracted with acetone, processed via solid phase extraction (SPE), and then analyzed by gas chromatography with electron capture detection. The following three SPE sorbents in cartridge format were compared: Empore™ SDB-XC, Oasis ® HLB, and Bond Elut NEXUS cartridges. The NEXUS cartridges provided the best overall recoveries for the 12 explosives in potting soil (average 48%) and the fastest processing times (<30min). It also rejected matrix components from spent motor oil on potting soil. The SPE method was validated by assessing limit of detection (LOD), processed sample stability, and interferences. All 12 compounds were detectable at 0.02μg explosive/gram of soil or lower in the three matrices tested (potting soil, sand, and loam) over three days. Seven explosives were stable up to seven days at 2μg/g and three were stable at 0.2μg/g, both in processed loam, which was the most challenging matrix. In the interference study, five interferences above the determined LOD for soil were detected in matrices collected across the United States and in purchased all-purpose sand, potting soil, and loam. This represented a 3.2% false positive rate for the 13 matrices processed by the screening method for interferences. The reported SPE cleanup method provides a fast and simple extraction process for separating organic explosives from matrix components, facilitating sample throughput and reducing instrument maintenance. In addition, a comparison study of the validated SPE method versus conventional syringe filtration was completed and highlighted the benefits of sample cleanup for removing matrix interferences, while also providing lower supply cost, order of magnitude lower LODs for most explosives, higher percent recoveries for complex matrices, and fewer instrument maintenance issues. Published by Elsevier B.V.

A new approach in sample treatment combined with UHPLC-MS/MS for the determination of multiclass mycotoxins in edible nuts and seeds.

PubMed

Arroyo-Manzanares, Natalia; Huertas-Pérez, José F; Gámiz-Gracia, Laura; García-Campaña, Ana M

2013-10-15

A sensitive, simple and rapid method for the determination of fourteen mycotoxins in nuts and seeds (including almonds, peanuts, sunflower seeds, pumpkin seeds, walnuts, macadamia nuts, pistachios, hazelnuts and pine nuts) has been developed using ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). The sample treatment comprises a first step based on QuEChERS procedure for the determination of fumonisin B1, fumonisin B2, deoxynivalenol, fusarenon-X, T-2 and HT-2 toxin, citrinin, sterigmatocystin, zearalenone and ochratoxin A. A subsequent clean-up step based on the dispersive liquid-liquid microextraction (DLLME) was necessary for the determination of aflatoxins (B1, B2, G1 and G2), since their determination was not possible applying only the QuEChERS-based extraction. The method was validated for peanuts as representative matrix and was subsequently evaluated for the other eight matrices. Quantification limits obtained for aflatoxins, the unique mycotoxins legislated on these matrices, were lower than the maximum levels allowed by the current legislation, while quantification limits obtained for the other mycotoxins were lower than the limits usually permitted by the legislation in other food matrices. Precision of the method was always lower than 11%, and recoveries ranged between 60.7% and 104.3%. © 2013 Elsevier B.V. All rights reserved.

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

PubMed

Oellig, Claudia

2016-05-06

Propolis is a very complex mixture of substances that is produced by honey bees and is known to be a rather challenging matrix for residue analysis. Besides resins, flavonoids and phenols, high amount of wax is co-extracted resulting in immense matrix effects. Therefore a suitable clean-up is crucial and indispensable. In this study, a reliable solid phase extraction (SPE) clean-up was developed for pesticide residue analysis in propolis. The clean-up success was quickly and easily monitored by high-performance thin-layer chromatography with different detection possibilities. The final method consists of the extraction of propolis with acetonitrile according to the QuEChERS method followed by an effective extract purification on dual-layer SPE cartridges with spherical hydrophobic polystyrene-divinylbenzene resin/primary secondary amine as sorbent and a mixture of toluene/acetone (95:5, v/v) for elution. Besides fat-soluble components like waxes, flavonoids, and terpenoids, more polar compounds like organic acids, fatty acids, sugars and anthocyanins were also removed to large extent. Method performance was assessed by recovery experiments at spiking levels of 0.5 and 1mg/kg (n=5) for fourteen pesticides that are relevant for propolis. Mean recoveries determined by HPLC-MS against solvent standards were between 40 and 101%, while calculation against matrix-matched standards provided recoveries of 79-104%. Precision of recovery, assessed by relative standard deviations, were below 9%. Thus, the developed dual-layer SPE clean-up enables the reliable pesticide residue analysis in propolis and provides a suitable alternative to time-consuming clean-up procedures proposed in literature. Copyright © 2016 Elsevier B.V. All rights reserved.

Hydrophilic chromatographic determination of carnosine, anserine, balenine, creatine, and creatinine.

PubMed

Mora, Leticia; Sentandreu, Miguel Angel; Toldrá, Fidel

2007-06-13

A new HPLC procedure based on hydrophilic interaction chromatography (HILIC) has been developed for the simultaneous determination of carnosine, anserine, balenine, creatine, and creatinine in meat. This is the first time that HILIC has been directly applied to the study of meat components, having the advantage of not requiring complex cleanup and/or sample derivatization procedures. The chromatographic separation has been developed using a silica column (4.6 x 150 mm, 3 microm), and the proposed methodology is simple, reliable, and fast (<13 min per sample). The method has been validated in terms of linearity, repeatability, reproducibility, and recovery and represents an interesting alternative to methods currently in use for determining the mentioned compounds and other polar substances. The detection limits are 5.64, 8.23, 3.66, 3.99, and 0.06 microg/mL for carnosine, anserine, balenine, creatine, and creatinine, respectively.

Determination of active components of Ginkgo biloba in human urine by capillary high-performance liquid chromatography/mass spectrometry with on-line column-switching purification.

PubMed

Ding, Shujing; Dudley, Ed; Chen, Lijuan; Plummer, Sue; Tang, Jiandong; Newton, Russell P; Brenton, A Gareth

2006-01-01

Ginkgo biloba is one of the most popular herbal nutritional supplements, with terpene lactones and flavonoids being the two major active components. An on-line purification high-performance liquid chromatography/mass spectrometry (HPLC/MS) method was successfully developed for the quantitative determination of flavonoids and terpene lactones excreted in human urine after ingesting the herbal supplement. Satisfactory separation was obtained using a C18 capillary column made in-house with sample clean-up and pre-concentration achieved using a C18 pre-column with column switching. High selectivity and limits of detection of 1-18 ng/mL were achieved using a selected ion monitoring (SIM) scan in negative ion mode; the on-line solid-phase extraction (SPE) recovery of the active components in Ginkgo biloba determined in this study was greater than 75%. Copyright 2006 John Wiley & Sons, Ltd.

Determination of organophosphate flame retardants in soil and fish using ultrasound-assisted extraction, solid-phase clean-up, and liquid chromatography with tandem mass spectrometry.

PubMed

Lorenzo, María; Campo, Julián; Picó, Yolanda

2018-03-22

A solid-liquid extraction method in combination with high-performance liquid chromatography and tandem mass spectrometry was developed and optimized for extraction and analysis of organophosphorus flame retardants in soil and fish. Methanol was chosen as the optimum extraction solvent, not only in terms of extraction efficiency, but also for its broader analyte coverage. The subsequent clean-up by solid-phase extraction is required to eliminate matrix coextractives and reduce matrix effects. Recoveries of the optimized method were 50-121% for soil and 47-123% for biota, both with high precision (RSDs <12% in soil and <23% in biota). The method limits of detection ranged from 0.06 to 0.20 ng/g dry weight and between 0.02 and 0.30 ng/g wet weight for soil and biota samples, respectively. However, samples with a high lipid content produce several problems as solid-phase extraction cartridge clogging that increase variability and analysis time. The method was successfully applied for the determination of organophosphorus flame retardants in soil and fish from L'Albufera Natural Park (Valencia, Spain). Target compounds were detected in all soil and fish samples with values varying from 13.8 to 89.7 ng/g dry weight and from 3.3 to 53.0 ng/g wet weight, respectively. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Using geostatistics to evaluate cleanup goals

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

Marcon, M.F.; Hopkins, L.P.

1995-12-01

Geostatistical analysis is a powerful predictive tool typically used to define spatial variability in environmental data. The information from a geostatistical analysis using kriging, a geostatistical. tool, can be taken a step further to optimize sampling location and frequency and help quantify sampling uncertainty in both the remedial investigation and remedial design at a hazardous waste site. Geostatistics were used to quantify sampling uncertainty in attainment of a risk-based cleanup goal and determine the optimal sampling frequency necessary to delineate the horizontal extent of impacted soils at a Gulf Coast waste site.

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

Anderson, L.M.

This paper describes the role of the Monsanto Chemical Company in the cleanup of a Superfund site in Galveston, Texas. Although other companies had sent waste to the site over an extended period of time, Monsanto was charged with the entire cost. Monsanto responded by identifying other site users and determining the extent of their liability through chemical analysis of the wastes. They took the lead in organizing the other users and developing an effective cleanup process at a cost much less than the EPA's estimates. They also helped to improve industry's relations with the community.

Potential Environmental and Environmental-Health Implications of the SAFRR Tsunami Scenario in California: Chapter F in The SAFRR (Science Application for Risk Reduction) Tsunami Scenario

USGS Publications Warehouse

Plumlee, Geoffrey S.; Morman, Suzette A.; San Juan, Carma

2013-01-01

If human populations are successfully evacuated prior to the tsunami arrival, there would be no or limited numbers of drownings, other casualties, or related injuries, wounds, and infections. Immediately after the tsunami, human populations away from the inundation zone could be transiently exposed to airborne gases, smoke, and ash from tsunamigenic fires. Cleanup and disposal, particularly of hazardous materials, would pose substantial logistical challenges and economic costs. Given the high value of the coastal residential and commercial properties in the inundation zone, it can be postulated that there would be substantial insurance claims for environmental restoration, mold mitigation, disposal of debris that contains hazardous materials, and costs of litigation related to environmental liability. Post-tsunami cleanup, if done with appropriate mitigation (for example, dust control), personal protection, and disposal measures, would help reduce the potential for cleanup-worker and resident exposures to toxicants and pathogens in harbor waters, debris, soils, ponded waters, and buildings. A number of other steps can be taken by governments, businesses, and residents to help reduce the environmental impacts of tsunamis and to recover more quickly from these environmental impacts. For example, development of State and local policies that foster rapid assessment of potential contamination, as well as rapid decision making for disposal options should hazardous debris or sediment be identified, would help enhance recovery by speeding cleanup.

A sustainable approach to controlling oil spills.

PubMed

Al-Majed, Abdul Aziz; Adebayo, Abdulrauf Rasheed; Hossain, M Enamul

2012-12-30

As a result of the huge economic and environmental destruction from oil spills, studies have been directed at improving and deploying natural sorbents which are not only the least expensive but also the safest means of spill control. This research reviews the limitations and environmental impact of existing cleanup methods. It also justifies the need for concerted research effort on oil spill control using natural and sustainable technology concepts. The article proposes future guidelines for the development of a sustainable cleanup technology. Finally, guidelines for the development of a new technology for the Middle East are proposed, which is the use of an abundant resource--date palm fibers--for such techniques. Copyright © 2012 Elsevier Ltd. All rights reserved.

Livermore study says oil leaks not severe

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

Patrick, L.

The Petroleum Marketers Association of America (PMAA), which is working to reform the federal Leaking Underground Storage Tank program, got some strong ammunition last month. A study that the Lawrence Livermore National Laboratory performed for the California State Water Resources Control Board has found that the environmental threat of leaks is not as severe as formerly thought. The study said: such leaks rarely jeopardize drinking water; fuel hydrocarbons have limited impacts on health, the environment, and groundwater; and cleanups often are done contrary to the knowledge and experience gained from prior remediations. As a result of the study, Gov. Petemore » Wilson ordered California cleanups halted at sites more than 250 feet from drinking water supplies.« less

A novel method for the rapid detection of benzo(a)pyrene in liquid milk by dimethyl sulfoxide selectively enhanced synchronous fluorescence spectrometry.

PubMed

Lin, Li-Rong; Luo, He-Dong; Li, Xiu-Ying; Li, Na; Zhou, Na; Jia, Yu-Zhu; Liu, Yi-Hong; Li, Yao-Qun

2014-01-01

Based on the high solubility efficiency and strong fluorescence response of benzo(a)pyrene (BaP) in dimethyl sulfoxide in combination with the high-performance derivative constant-energy synchronous fluorescence spectroscopic (DCESFS) technique, a simple, sensitive and economic method was developed for the determination of BaP in liquid milk. This method comprises ultrasound-assisted solvent extraction, solvent replacement and DCESFS detection. No saponification or other tedious clean-up procedures were needed. The recoveries of BaP in different milk samples were greater than 82%. Detection limits in full- and low-fat milk were 0.03 and 0.04 μg kg(-1), respectively.

Cleanups in My Community Data

EPA Pesticide Factsheets

Cleanups in My Community (CIMC) enables you to map and list hazardous waste cleanup locations and grant areas, and drill down to details about those cleanups and grants and other, related information.

Clean-up of aqueous acetone vegetable extracts by solid-matrix partition for pyrethroid residue determination by gas chromatography-electron-capture detection.

PubMed

Di Muccio, A; Barbini, D A; Generali, T; Pelosi, P; Ausili, A; Vergori, F; Camoni, I

1997-03-21

Disposable, ready-to-use cartridges filled with macroporous diatomaceous material are used to carry out a partition clean-up that, in a single step, is capable of transferring pesticide residues from aqueous acetone extracts into light petroleum-dichloromethane (75:25, v/v). This procedure takes the place of some functions (such as separatory-funnel partition, drying over anhydrous sodium sulphate and partial adsorption clean-up) usually performed by separate steps in classical schemes. Fourteen pyrethroid pesticides, including tefluthrin, tetramethrin, cyphenothrin, cyfluthrin, flucythrinate, tau-fluvalinate, deltamethrin, bioallethrin, fenpropathrin, lambda-cyhalothrin, permethrin, alpha-cypermethrin, esfenvalerate and tralomethrin were determined using the described procedure with satisfactory recoveries for most of them, at spiking levels ranging from 0.08 to 0.82 mg/kg for the different compounds. Crops subjected to the described procedure included strawberry, apple, and orange gave extracts containing a mass of co-extractives that was between 5 and 30 mg. Compared with classical schemes, the described procedure is simple, less labour intensive, allows parallel handling of several extracts and does not require the preparation and maintenance of equipment. Troublesome emulsions such as those frequently observed in separation funnel partitioning do not occur.

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

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

Clegg, B.

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.

Mold: Cleanup and Remediation

MedlinePlus

... National Center for Environmental Health (NCEH) Cleanup and Remediation Recommend on Facebook Tweet Share Compartir On This ... CDC and EPA on mold cleanup, removal and remediation. Cleanup information for you and your family Homeowner’s ...

Determination of perfluoroalkyl carboxylic, sulfonic, and phosphonic acids in food.

PubMed

Ullah, Shahid; Alsberg, Tomas; Vestergren, Robin; Berger, Urs

2012-11-01

A sensitive and accurate method was developed and validated for simultaneous analysis of perfluoroalkyl carboxylic acids, sulfonic acids, and phosphonic acids (PFPAs) at low picograms per gram concentrations in a variety of food matrices. The method employed extraction with acetonitrile/water and cleanup on a mixed-mode co-polymeric sorbent (C8 + quaternary amine) using solid-phase extraction. High-performance liquid chromatographic separation was achieved on a C18 column using a mobile phase gradient containing 5 mM 1-methyl piperidine for optimal chromatographic resolution of PFPAs. A quadrupole time-of-flight high-resolution mass spectrometer operating in negative ion mode was used as detector. Method detection limits were in the range of 0.002 to 0.02 ng g(-1) for all analytes. Sample preparation (extraction and cleanup) recoveries at a spiking level of 0.1 ng g(-1) to a baby food composite were in the range of 59 to 98 %. A strong matrix effect was observed in the analysis of PFPAs in food extracts, which was tentatively assigned to sorption of PFPAs to the injection vial in the solvent-based calibration standard. The method was successfully applied to a range of different food matrices including duplicate diet samples, vegetables, meat, and fish samples.

REGULATORY STRATEGIES TO MINIMIZE GENERATION OF REGULATED WASTES FROM CLEANUP, CONTINUED USE OR DECOMMISSIONING OF NUCLEAR FACILITIES CONTAMINATED WITH POLYCHLORINATED BIPHENYLS (PCBS) - 11198

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

Lowry, N.

Disposal costs for liquid PCB radioactive waste are among the highest of any category of regulated waste. The high cost is driven by the fact that disposal options are extremely limited. Toxic Substances Control Act (TSCA) regulations require most liquids with PCBs at concentration of {ge} 50 parts-per-million to be disposed by incineration or equivalent destructive treatment. Disposal fees can be as high as $200 per gallon. This figure does not include packaging and the cost to transport the waste to the disposal facility, or the waste generator's labor costs for managing the waste prior to shipment. Minimizing the generationmore » of liquid radioactive PCB waste is therefore a significant waste management challenge. PCB spill cleanups often generate large volumes of waste. That is because the removal of PCBs typically requires the liberal use of industrial solvents followed by a thorough rinsing process. In a nuclear facility, the cleanup process may be complicated by the presence of radiation and other occupational hazards. Building design and construction features, e.g., the presence of open grating or trenches, may also complicate cleanup. In addition to the technical challenges associated with spill cleanup, selection of the appropriate regulatory requirements and approach may be challenging. The TSCA regulations include three different sections relating to the cleanup of PCB contamination or spills. EPA has also promulgated a separate guidance policy for fresh PCB spills that is published as Subpart G of 40 CFR 761 although it is not an actual regulation. Applicability is based on the circumstances of each contamination event or situation. Other laws or regulations may also apply. Identification of the allowable regulatory options is important. Effective communication with stakeholders, particularly regulators, is just as important. Depending on the regulatory path that is taken, cleanup may necessitate the generation of large quantities of regulated waste. Allowable options must be evaluated carefully in order to reduce compliance risks, protect personnel, limit potential negative impacts on facility operations, and minimize the generation of wastes subject to TSCA. This paper will identify critical factors in selecting the appropriate TSCA regulatory path in order to minimize the generation of radioactive PCB waste and reduce negative impacts to facilities. The importance of communicating pertinent technical issues with facility staff, regulatory personnel, and subsequently, the public, will be discussed. Key points will be illustrated by examples from five former production reactors at the DOE Savannah River Site. In these reactors a polyurethane sealant was used to seal piping penetrations in the biological shield walls. During the intense neutron bombardment that occurred during reactor operation, the sealant broke down into a thick, viscous material that seeped out of the piping penetrations over adjacent equipment and walls. Some of the walls were painted with a PCB product. PCBs from the paint migrated into the degraded sealant, creating PCB 'spill areas' in some of these facilities. The regulatory cleanup approach selected for each facility was based on its operational status, e.g., active, inactive or undergoing decommissioning. The selected strategies served to greatly minimize the generation of radioactive liquid PCB waste. It is expected that this information would be useful to other DOE sites, DOD facilities, and commercial nuclear facilities constructed prior to the 1979 TSCA ban on most manufacturing and uses of PCBs.« less

[Analysis of sulfonamide residues in pork and chicken by high performance liquid chromatography coupled with solid-phase extraction using multiwalled carbon nanotubes as adsorbent].

PubMed

Zhao, Haixiang; Liu, Haiping; Yan, Zaoying

2014-03-01

A multi-residue analytical method based on solid-phase extraction (SPE) with multiwalled carbon nanotubes (MWCNTs) as sorbent was developed. The determination of the sulfonamides (SAs) in pork and chicken was carried out by high performance liquid chromatography-ultraviolet detection (HPLC-UV). The clean-up conditions were optimized. The analytes were extracted by acetonitril and cleaned-up by MWCNTs SPE cartridge. The extract was redissolved with the Na2HPO4 buffer (pH 5.5-6.0) for loading, and was washed with acetone-hexane (5:95, v/v), then eluted with acetone-dichloromethane (1:1, v/v) from the column. The mobile phase used in the chromatographic separation consisted of a binary mixture of acetonitrile and 50 mmol/L NaH2PO4 with the volume ratio of 7:3. A wide linear range was 0.01-1.00 mg/L with the correlation coefficients above 0.998. The limits of detection (S/N = 3) were 0.003 mg/L, and the limits of quantification (S/N = 10) were 0.01 mg/L. The average recoveries were over 70% for the nine SAs in the spiked range of 0.02-0.2 mg/kg, with the relative standard deviations (RSDs) lower than 8%. This study indicated that the MWCNTs SPE cartridge is efficient for the clean-up of the SAs in animal tissues or products, and the method is simple, accurate and suitable for the quantification of the SAs residues.

Application Of Monitored Natural Attenuation For Cleanup Of Radionuclides In Groundwater

EPA Science Inventory

A retrospective analysis was conducted to evaluate the unsuccessful performance of an MNA remedy for uranium contamination in groundwater at a Superfund site in Richland, Washington. The primary factors that limited the accuracy of contaminant transport model projections at this...

Cleanups in My Community

EPA Pesticide Factsheets

Cleanups In My Community is a web app of hazardous waste cleanups for which EPA collects information, on maps and in lists, and to access additional information about those cleanups. This page describes and links to the application.

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. Copyright © 2015 Elsevier B.V. All rights reserved.

Multi-residue determination of 47 organic compounds in water, soil, sediment and fish-Turia River as case study.

PubMed

Carmona, Eric; Andreu, Vicente; Picó, Yolanda

2017-11-30

A sensitive and reliable method based on solid-liquid extraction (SLE) using McIlvaine-Na 2 EDTA buffer (pH=4.5)-methanol and solid-phase extraction (SPE) clean up prior to ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) was applied to determine 47 organic contaminants in fish, soil and sediments. The SPE procedure to clean-up the extracts was also used as extraction method to determine these compounds in water. Recoveries ranged from 38 to 104% for all matrices with RSDs<30%. Limits of Quantification for the target compounds were in the range of 10-50ng/g for soil, 2-40ng/g for sediment, 5-30ng/g for fish and 0.3-26ng/L for water. Furthermore, the proposed method was compared to QuEChERS (widely used for environmental matrices) that involves extraction with buffered acetonitrile (pH 5.5) and dispersive SPE clean-up. The results obtained (recoveries>50% for 36 compounds in front of 9, matrix effect<20% for 31 compounds against 21, and LOQs <25ngg -1 for 38 compounds against 22) indicates that the proposed method is more efficient than QuEChERS, The method was applied to monitoring these compounds along the Turia River. In river waters, Paracetamol (175ngL -1 ), ibuprofen (153ngL -1 ) and bisphenol A (41ngL -1 ) were the compounds most frequently detected while in sediments were vildagliptin (7ngg -1 ) and metoprolol (31ngg -1 ) and in fish, bisphenol A (33ngg -1 ) or sulfamethoxazole (13ngg -1 ). Copyright © 2017 Elsevier B.V. All rights reserved.

Development of "one-pot" method for multi-class compounds in porcine formula feed by multi-function impurity adsorption cleaning followed ultra-performance liquid chromatography-tandem mass spectrometry detection.

PubMed

Wang, Peilong; Wang, Xiao; Zhang, Wei; Su, Xiaoou

2014-02-01

A novel and efficient determination method for multi-class compounds including β-agonists, sedatives, nitro-imidazoles and aflatoxins in porcine formula feed based on a fast "one-pot" extraction/multifunction impurity adsorption (MFIA) clean-up procedure has been developed. 23 target analytes belonging to four different class compounds could be determined simultaneously in a single run. Conditions for "one-pot" extraction were studied in detail. Under the optimized conditions, the multi-class compounds in porcine formula feed samples were extracted and purified with methanol contained ammonia and absorbents by one step. The compounds in extracts were purified by using multi types of absorbent based on MFIA in one pot. The multi-walled carbon nanotubes were employed to improved clean-up efficiency. Shield BEH C18 column was used to separate 23 target analytes, followed by tandem mass spectrometry (MS/MS) detection using an electro-spray ionization source in positive mode. Recovery studies were done at three fortification levels. Overall average recoveries of target compounds in porcine formula feed at each levels were >51.6% based on matrix fortified calibration with coefficients of variation from 2.7% to 13.2% (n=6). The limit of determination (LOD) of these compounds in porcine formula feed sample matrix was <5.0 μg/kg. This method was successfully applied in screening and confirmation of target drugs in >30 porcine formula feed samples. It was demonstrated that the integration of the MFIA protocol with the MS/MS instrument could serve as a valuable strategy for rapid screening and reliable confirmatory analysis of multi-class compounds in real samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Development and validation of a hydrophilic interaction chromatography-mass spectrometry assay for taurine and methionine in matrices rich in carbohydrates.

PubMed

de Person, Marine; Hazotte, Aurélie; Elfakir, Claire; Lafosse, Michel

2005-07-22

A new procedure based on hydrophilic interaction chromatography coupled to tandem mass spectrometry (ionisation process by pneumatically assisted electrospray in negative ion mode), is developed and validated for the simultaneous determination of underivatised taurine and methionine in beverages rich in carbohydrates such as energy drinks. No initial clean-up procedure and no sample derivatisation are required. Satisfactory analysis was obtained on an Astec apHera NH2 (150 mm x 4.6 mm; 5 microm) column with methanol-water (60/40) as mobile phase. The method was validated in terms of specificity, detection limits, linearity, accuracy, precision and stability, using threonine as internal standard. The potential effects of matrix and endogenous amino acid content were also examined. The limits of detection in the beverage varied from 20 microg L(-1) for taurine to 50 micro L(-1) for methionine.

Determination of aflatoxins B1, B2, G1 and G2 in spices using a multifunctional column clean-up.

PubMed

Akiyama, H; Goda, Y; Tanaka, T; Toyoda, M

2001-10-12

A rapid and simple method using a multifunctional column, which contains lipophilic and charged active sites, was developed to analyse aflatoxins B1, B2, G1 and G2 in various spices, such as red pepper and nutmeg. After extraction by acetonitrile:water (9:1) and clean-up using MultiSep #228 column, the aflatoxins and aflatoxin-TFA derivatives are determined using LC with fluorescence detection. Recoveries of each aflatoxin B1, B2, G1 and G2 spiked to red pepper, white pepper, black pepper, nutmeg and tear grass at the level of 10 ng/g were over 80-85% in all instances. The minimum detectable concentration for aflatoxins in red pepper was 0.5 ng/g.

Simultaneous determination of multiclass pesticide residues in human plasma using a mini QuEChERS method.

PubMed

Srivastava, Anshuman; Rai, Satyajeet; Kumar Sonker, Ashish; Karsauliya, Kajal; Pandey, Chandra Prabha; Singh, Sheelendra Pratap

2017-06-01

Blood is one of the most assessable matrices for the determination of pesticide residue exposure in humans. Effective sample preparation/cleanup of biological samples is very important in the development of a sensitive, reproducible, and robust method. In the present study, a simple, cost-effective, and rapid gas chromatography-tandem mass spectrometry method has been developed and validated for simultaneous analysis of 31 multiclass (organophosphates, organochlorines, and synthetic pyrethroids) pesticide residues in human plasma by means of a mini QuEChERS (quick, easy, cheap, effective, rugged, and safe) method. We have adopted a modified version of the QuEChERS method, which is primarily used for pesticide residue analysis in food commodities. The QuEChERS method was optimized by use of different extraction solvents and different amounts and combinations of salts and sorbents (primary-secondary amines and C 18 ) for the dispersive solid-phase extraction step. The results show that a combination of ethyl acetate with 2% acetic acid, magnesium sulfate (0.4 g), and solid-phase extraction for sample cleanup with primary-secondary amines (50 mg) per 1-mL volume of plasma is the most suitable for generating acceptable results with high recoveries for all multiclass pesticides from human plasma. The mean recovery ranged from 74% to 109% for all the analytes. The limit of quantification and limit of detection of the method ranged from 0.12 to 13.53 ng mL -1 and from 0.04 to 4.10 ng mL -1 respectively. The intraday precision and the interday precision of the method were 6% or less and 11% or less respectively. This method would be useful for the analysis of a wide range of pesticides of interest in a small volume of clinical and/or forensic samples to support biomonitoring and toxicological applications. Graphical Abstract Pesticide residues analysis in human plasma using mini QuEChERS method.

Simultaneous determination of residues of emamectin and its metabolites, and milbemectin, ivermectin, and abamectin in crops by liquid chromatography with fluorescence detection.

PubMed

Yoshii, K; Kaihara, A; Tsumura, Y; Ishimitsu, S; Tonogai, Y

2001-01-01

A liquid chromatographic (LC) method was developed for the determination of emamectin and its metabolites (8,9-Z-isomer, N-demethylated, N-formylated, and N-methylformylated emamectin) in various crops. The analytes were extracted with acetone, cleaned up on cartridge columns (C18 and NH2), derivatized with trifluoroacetic anhydride and 1-methylimidazole, and determined by LC with fluorescence detection. Because radish inhibited the formation of the fluorescent derivatives, an additional Bond Elut PRS cartridge was used in the cleanup of Japanese radish samples. During sample preparation, N-formylated emamectin partially degraded to emamectin B1b and emamectin B1a, and the 8,9-Z-isomer partially degraded to N-demethylated emamectin. Therefore, emamectin and its metabolites were determined as total emamectin, i.e., their sum was estimated as emamectin benzoate. Their recoveries from most crops were approximately 80-110% with the developed method. The detection limits for the analytes in vegetables were 0.1-0.3 parts per trillion (ppt). The results for these compounds were confirmed by LC/mass spectrometry (LC/MS; electrospray ionization mode). Because the fluorescent derivative of emamectin was undetectable by LC/MS, the results for the analyte were confirmed by using a sample solution without derivatization. Limits of detection by LC/MS were similar to the fluorescence detection limits, 0.1-0.3 ppt in vegetables. In addition to the emamectins, milbemectin, ivermectin, and abamectin were also determined by the developed method.

Multi-residue determination of 171 pesticides in cowpea using modified QuEChERS method with multi-walled carbon nanotubes as reversed-dispersive solid-phase extraction materials.

PubMed

Han, Yongtao; Song, Le; Zou, Nan; Chen, Ronghua; Qin, Yuhong; Pan, Canping

2016-09-15

A rapid and sensitive method for the determination of 171 pesticides in cowpea was developed using multi-walled carbon nanotubes (MWCNTs) as reversed-dispersive solid-phase (r-DSPE) extraction materials. The clean-up performance of MWCNTs was proved to be obviously superior to PSA and GCB. This method was validated on cowpea spiked at 0.01 and 0.1mgkg(-1) with five replicates. The mean recoveries for 169 pesticides ranged from 74% to 129% with relative standard deviations (RSDs) (n=5) lower than 16.4%, except diflufenican and quizalofop-ethyl. Good linearity for all pesticides was obtained with the calibration curve coefficients (R(2)) larger than 0.9970. The limit of detection (LODs) and limit of quantification (LOQs) for the 171 pesticides ranged from 0.001 to 0.003mgkg(-1) and from 0.002 to 0.009mgkg(-1), respectively. The method was demonstrated to be reliable and sensitive for the routine monitoring of the 171 pesticides in cowpea samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Multifamily determination of pesticide residues in soya-based nutraceutical products by GC/MS-MS.

PubMed

Páleníková, Agneša; Martínez-Domínguez, Gerardo; Arrebola, Francisco Javier; Romero-González, Roberto; Hrouzková, Svetlana; Frenich, Antonia Garrido

2015-04-15

An analytical method based on a modified QuEChERS extraction coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) was evaluated for the determination of 177 pesticides in soya-based nutraceutical products. The QuEChERS method was optimised and different extraction solvents and clean-up approaches were tested, obtaining the most efficient conditions with a mixture of sorbents (PSA, C18, GBC and Zr-Sep(+)). Recoveries were evaluated at 10, 50 and 100 μg/kg and ranged between 70% and 120%. Precision was expressed as relative standard deviation (RSD), and it was evaluated for more than 160 pesticides as intra and inter-day precision, with values always below 20% and 25%, respectively. Limits of detection (LODs) ranged from 0.1 to 10 μg/kg, whereas limits of quantification (LOQs) from 0.5 to 20 μg/kg. The applicability of the method was proved by analysing soya-based nutraceuticals. Two pesticides were found in these samples, malathion and pyriproxyfen, at 11.1 and 1.5 μg/kg respectively. Copyright © 2014 Elsevier Ltd. All rights reserved.

An updated ciguatoxin extraction method and silica cleanup for use with HPLC-MS/MS for the analysis of P-CTX-1, PCTX-2 and P-CTX-3.

PubMed

Meyer, Lauren; Carter, Steve; Capper, Angela

2015-12-15

Ciguatera fish poisoning is a debilitating human neuro-intoxication caused by consumption of tropical marine organisms, contaminated with bioaccumulated ciguatoxins (CTXs). The growing number of cases coupled with the high toxicity of CTXs makes their reliable detection and quantification of paramount importance. Three commonly occurring ciguatoxins, P-CTX-1, 2 and 3 from five different ciguatoxic Spanish mackerel (Scomberomorus commerson), were used to assess the effectiveness of different extraction techniques: homogenization (high powered blending vs. ultrasonication); C-18 column sizes (500 mg vs. 900 mg); and a novel HILIC SPE cleanup. Despite minor differences, blending and sonication proved equally effective. Larger 900 mg columns offered a greater extraction efficiency, increasing detected P-CTX-1 by 37% (P < 0.001). The newly adapted cleanup was highly effective at reducing co-eluting phospholipids thereby reducing matrix effects and increasing detectable CTXs by HPLC-MS/MS. Silica cleanup extraction efficiencies were also compared between the highly effective and validated ciguatoxin rapid extraction method (CREM) and current best practice extraction method employed by Queensland Health (QH). Overall, the QH protocol proved more effective, especially when paired with the newly adapted cleanup, as this increased the amount of extracted P-CTX-1 by 46% (P < 0.01), P-CTX-2 by 10% and P-CTX-3 by 71% (P = 0.001). This study suggests the QH protocol utilizing a 900 mg C-18 column and newly adapted HILIC SPE cleanup was most effective at extracting P-CTX-1, -2, -3. Specifically P-CTX-1, the primary ciguatoxin congener of concern due to its extremely high potency and an ability to cause CFP at 0.1 μg/kg following consumption of carnivorous fish flesh. Despite being more time intensive (an additional 85 min per batch of 12 samples), this will be especially effective for assessing lower toxin burdens, which may be near the limit of detection. Copyright © 2015 Elsevier Ltd. All rights reserved.

Brownfield site development -- The Ontario context

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

Phillips, D.B.

The provincial government of Ontario recently promulgated new guidelines to deal with contamination on sites. One of the purposes of the guideline was to bolster development of contaminated sites by clarifying the regulatory process for redeveloping a contaminated site and to provide several clean-up options based on newer scientific information. These clean-up options include stratified clean-ups and site specific risk based criteria. The applications of the previous guideline were at times cumbersome for industries and land developers which may have impeded development of the Brownfield. This paper compares the changes between the old and the new regulatory clean-up guidelines andmore » presents the differences in approach. This paper also presents the results from interviews with several industries and property developers and assesses their view on the regulatory change as well as their desire to develop Brownfields in Ontario. This information determines if the change in regulatory process has really encouraged development. Results from the interviews with proponents indicated that the new guidelines are a much better approach but still contain barriers such as liability issues. Furthermore, the regulatory approval process has been transferred from the provincial government to the local governments. As a result the local governments are applying the guidelines differently across the province.« less

Fast-Track Cleanup at Closing DoD Installations

EPA Pesticide Factsheets

The Fast-Track Cleanup program strives to make parcels available for reuse as quickly as possible by the transfer of uncontaminated or remediated parcels, the lease of contaminated parcels where cleanup is underway, or the 'early transfer' of contaminated property undergoing cleanup.

HANFORD SITE CENTRAL PLATEAU CLEANUP COMPLETION STRATEGY

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

BERGMAN TB

2011-01-14

Cleanup of the Hanford Site is a complex and challenging undertaking. The U.S. Department of Energy (DOE) has developed a comprehensive vision for completing Hanford's cleanup mission including transition to post-cleanup activities. This vision includes 3 principle components of cleanup: the {approx}200 square miles ofland adjacent to the Columbia River, known as the River Corridor; the 75 square miles of land in the center of the Hanford Site, where the majority of the reprocessing and waste management activities have occurred, known as the Central Plateau; and the stored reprocessing wastes in the Central Plateau, the Tank Wastes. Cleanup of themore » River Corridor is well underway and is progressing towards completion of most cleanup actions by 2015. Tank waste cleanup is progressing on a longer schedule due to the complexity of the mission, with construction of the largest nuclear construction project in the United States, the Waste Treatment Plant, over 50% complete. With the progress on the River Corridor and Tank Waste, it is time to place increased emphasis on moving forward with cleanup of the Central Plateau. Cleanup of the Hanford Site has been proceeding under a framework defmed in the Hanford Federal Facility Agreement and Consent Order (Tri-Party Agreement). In early 2009, the DOE, the State of Washington Department of Ecology, and the U.S. Environmental Protection Agency signed an Agreement in Principle in which the parties recognized the need to develop a more comprehensive strategy for cleanup of the Central Plateau. DOE agreed to develop a Central Plateau Cleanup Completion Strategy as a starting point for discussions. This DOE Strategy was the basis for negotiations between the Parties, discussions with the State of Oregon, the Hanford Advisory Board, and other Stakeholder groups (including open public meetings), and consultation with the Tribal Nations. The change packages to incorporate the Central Plateau Cleanup Completion Strategy were signed by the Parties on October 26,2010, and are now in the process of being implemented.« less

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. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of Polychlorinated Biphenyls in Soil and Sediment by Selective Pressurized Liquid Extraction with Immunochemical Detection

EPA Science Inventory

A selective liquid pressurized extraction (SPLE) method was developed as a streamlined sample preparation/cleanup procedure for determining Aroclors and coplanar polychlorinated biphenyls (PCBs) in soil and sediment matrices. The SPLE method was coupled with an enzyme-linked imm...

EVALUATION OF ANALYTICAL METHODS FOR DETERMINING PESTICIDES IN BABY FOOD AND ADULT DUPLICATE-DIET SAMPLES

EPA Science Inventory

Determinations of pesticides in food are often complicated by the presence of fats and require multiple cleanup steps before analysis. Cost-effective analytical methods are needed for conducting large-scale exposure studies. We examined two extraction methods, supercritical flu...

Determination of sulfonamides in animal tissues by modified QuEChERS and liquid chromatography tandem mass spectrometry.

PubMed

Wen, Ching-Hsuan; Lin, Shu-Ling; Fuh, Ming-Ren

2017-03-01

In this study, the salting-out solvent extraction and dispersive solid-phase extraction (dSPE) clean-up steps in QuEChERS (quick, easy, cheap, effective, rugged, and safe) method were optimized to reduce matrix effect and efficiently extract target sulfonamides from a variety of edible animal tissues. The extracted sulfonamides were then analyzed using liquid chromatography tandem mass spectrometry (LC-MS/MS). Good extraction recoveries (74.0-100.3% in five different sources of animal tissues; n=3) with acceptable matrix effect (<10%, except for liver samples) were obtained using the proposed method. For the first time, a commercial ND-lipids cartridge was used to remove hydrophobic matrix components from fat-rich animal tissues in the clean-up step of QuEChERS. In addition, good linearity (0.125-12.5ngg -1 ) was observed using matrix-matched calibration (in beef). Limits of detection (LODs) were estimated at 0.01-0.03ngg -1 in beef, pork, and chicken samples. For beef tripe and pig liver samples, the LODs were in the range of 0.02-0.04ngg -1 . Good intra-day/inter-day precision (1.0-10.5%/0.4-8.0%) and accuracy (95.2-107.2%/97.8-102.1%) were also achieved using the modified QuEChERS for sample pretreatment. The applicability of the modified QuEChERS-LC-MS/MS method was demonstrated by determining the occurrence of target sulfonamides in various edible animal tissues for potential food safety analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

Simultaneous determination of 1- and 2-naphthol in human urine using on-line clean-up column-switching liquid chromatography-fluorescence detection.

PubMed

Preuss, Ralf; Angerer, Jürgen

2004-03-05

We developed a new 3-D HPLC method for on-line clean-up and simultaneous quantification of two important naphthalene metabolites, 1-naphthol and 2-naphthol, in human urine. Except an enzymatic hydrolysis no further sample pre-treatment is necessary. The metabolites are stripped from urinary matrix by on-line extraction on a restricted access material pre-column (RAM RP-8), transferred in backflush mode onto a silica-based CN-(cyano)phase column for further purification from interfering substances. By another successive column switching step both analytes are transferred with a minimum of overlapping interferences onto a C12 bonded reversed phase column with trimethylsilyl endcapping where the final separation is carried out. The entire arrangement is software controlled. Eluting analytes are quantified by fluorescence detection (227/430 nm) after an external calibration. Within a total run time of 40 min we can selectively quantify both naphthols with detection limits in the lower ppb range (1.5 and 0.5 microg/l for 1- and 2-naphthol, respectively) with excellent reliability (ensured by precision, accuracy, matrix-independency and FIOH quality assurance program participation). First results on a collective of 53 occupationally non exposed subjects showed mean levels of 11.0 microg/l (1-naphthol) and 12.9 microg/l (2-naphthol). Among smokers (n=21) a significantly elevated mean level of urinary naphthols was determined (1-naphthol: 19.2 microg/l and 2-naphthol: 23.7 microg/l) in comparison to non smokers (n=32; 1-naphthol: 5.6 microg/l, 2-naphthol: 5.6 microg/l).

IDENTIFICATION OF COMPOUNDS IN SOUTH AFRICAN STREAM SAMPLES USING ION COMPOSITION ELUCIDATION (ICE)

EPA Science Inventory

Analytical methods for target compounds usually employ clean-up procedures to remove potential mass interferences and utilize selected ion recording (SIR) to provide low detection limits. Such an approach, however, could overlook non-target compounds that might be present and tha...

Amounts and activity concentrations of radioactive wastes from the cleanup of large areas contaminated in nuclear accidents

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

Lehto, J.; Ikaeheimonen, T.K.; Salbu, B.

The fallout from a major nuclear accident at a nuclear plant may result in a wide-scale contamination of the environment. Cleanup of contaminated areas is of special importance if these areas are populated or cultivated. All cleanup measures generate high amounts of radioactive waste, which have to be treated and disposed of in a safe manner. Scenarios assessing the amounts and activity concentrations of radioactive wastes for various cleanup measures after severe nuclear accidents have been worked out for urban, forest and agricultural areas. These scenarios are based on contamination levels and ares of contaminated lands from a model accident,more » which simulates a worst case accident at a nuclear power plant. Amounts and activity concentrations of cleanup wastes are not only dependent on the contamination levels and areas of affected lands, but also on the type of deposition, wet or dry, on the time between the deposition and the cleanup work, on the season, at which the deposition took place, and finally on the level of cleanup work. In this study practically all types of cleanup wastes were considered, whether or not the corresponding cleanup measures are cost-effective or justified. All cleanup measures are shown to create large amounts of radioactive wastes, but the amounts, as well as the activity concentrations vary widely from case to case.« less

Biodegradation of oil refinery wastes under OPA and CERCLA

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

Gamblin, W.W.; Banipal, B.S.; Myers, J.M.

1995-12-31

Land treatment of oil refinery wastes has been used as a disposal method for decades. More recently, numerous laboratory studies have been performed attempting to quantify degradation rates of more toxic polycyclic aromatic hydrocarbon compounds (PAHs). This paper discusses the results of the fullscale aerobic biodegradation operations using land treatment at the Macmillan Ring-Free Oil refining facility. The tiered feasibility approach of evaluating biodegradation as a treatment method to achieve site-specific cleanup criteria, including pilot biodegradation operations, is discussed in an earlier paper. Analytical results of biodegradation indicate that degradation rates observed in the laboratory can be met and exceededmore » under field conditions and that site-specific cleanup criteria can be attained within a proposed project time. Also prevented are degradation rates and half-lives for PAHs for which cleanup criteria have been established. PAH degradation rates and half-life values are determined and compared with the laboratory degradation rates and half-life values which used similar oil refinery wastes by other in investigators (API 1987).« less

Chitosan from shrimp shells: A renewable sorbent applied to the clean-up step of the QuEChERS method in order to determine multi-residues of veterinary drugs in different types of milk.

PubMed

Arias, Jean Lucas de Oliveira; Schneider, Antunielle; Batista-Andrade, Jahir Antonio; Vieira, Augusto Alves; Caldas, Sergiane Souza; Primel, Ednei Gilberto

2018-02-01

Clean extracts are essential in LC-MS/MS, since the matrix effect can interfere in the analysis. Alternative materials which can be used as sorbents, such as chitosan in the clean-up step, are cheap and green options. In this study, chitosan from shrimp shell waste was evaluated as a sorbent in the QuEChERS method in order to determine multi-residues of veterinary drugs in different types of milk, i. e., fatty matrices. After optimization, the method showed correlation coefficients above 0.99, LOQs ranged between 1 and 50μgkg -1 and recoveries ranged between 62 and 125%, with RSD<20% for all veterinary drugs in all types of milk under study. The clean-up step which employed chitosan proved to be effective, since it reduced both the matrix effect (from values between -40 and -10% to values from -10 to +10%) and the extract turbidity (up to 95%). When the proposed method was applied to different milk samples, residues of albendazole (49μgkg -1 ), sulfamethazine (

AUTOMATED PRESSURIZED FLUID EXTRACTION WITH IN-LINE CLEAN-UP FOR DETERMINATION OF PESTICIDES IN COMPOSITE DIETS.

EPA Science Inventory

USEPA's National Exposure Research Laboratory conducts research to measure the exposure of individuals to chemical pollutants through the diet, as well as other media. In support of this research, methods are being evaluated for determination of organophosphate pesticides in co...

Determination of phenolic xenoestrogens in water by liquid chromatography with coulometric-array detection.

PubMed

Inoue, Koichi; Yoshie, Yuriko; Kondo, Sachiko; Yoshimura, Yoshihiro; Nakazawa, Hiroyuki

2002-02-08

A sensitive method for the simultaneous determination of phenolic xenoestrogens such as bisphenol A, 2,4-dichlorophenol, 4-tert,-butylphenol, 4-n2-pentylphenol, 4-n-hexylphenol, 4-n-heptylphenol, 4-octylphenol, 4-nonylphenol was developed using reversed-phase LC and coulometric-array detection. Stepwise gradient elution with phosphoric acid in water-acetonitrile was used. The calibration curves were linear in the range of 5.0 (or 10.0)-1000 ng ml(-1) with correlation coefficients of 0.9978-0.9999, the limits of detection were 0.01-0.02 ng ml(-1). Sample clean-up was performed by solid-phase extraction (SPE) using 3M Empore extraction disks. Three commercial sorbents, C18, SDB-XD (styrene-divinylbenzene polymer) and SDB-RPS (sulfonated styrene-divinylbenzene polymer) were compared. The highest recoveries were obtained with SDB-RPS. They were above 70% with a relative standard deviation of less than 15%. The proposed method was applied to the determination of phenolic xenoestrogens in various water samples.

[Determination of emamectin benzoate residue in vegetables by high performance liquid chromatography with fluorescence detection].

PubMed

Zhang, Yan; Wu, Yinliang; Hu, Jiye; Wang, Hongwei; Pan, Canping; Liu, Fengmao

2008-01-01

A method was developed for the determination of emamectin benzoate residue in cabbage and mushroom using solid-phase extraction (SPE) and high performance liquid chromatography (HPLC) with fluorescence detection. The sample was extracted with ethyl acetate. Further cleanup was performed on a propylsulfonic acid solid phase extraction cartridge, followed by the derivatization with trifluoroacetic anhydride in the presence of N-methylimidazole. The amount of derivatized emamectin benzoate was determined by fluorescence detector after separation by HPLC. The detection limit was 0.10 microg/kg for cabbage and mushroom samples. The recoveries of emamectin benzoate in cabbage and mushroom samples were 78.6%-84.9%. The inter-day relative standard deviation (RSD) and intra-day RSD were 2.7%-6.0% and 3.1%-8.9%, respectively, at the fortified levels of 1.0-20.0 microg/kg. The calibration curve of emamectin benzoate in vegetables at the concentration range of 0.002 mg/L to 0.10 mg/L was linear (r = 0.9999).

Determination of nicotianamine in soy sauce and other plant-based foods by LC-MS/MS.

PubMed

Yamaguchi, Hitomi; Uchida, Riichiro

2012-10-10

Nicotianamine is a nonproteinogenic amino acid, known to be an important metal chelator in plants. Recently, the antihypertensive effect of nicotianamine was discovered. In this study, a simple method to determine nicotianamine was developed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) with a multimode ODS column. This method does not need derivatizing or ion-pairing reagents to retain nicotianamine, which is known for its poor retention on reversed-phase columns because of its high polarity. Moreover, this method showed a sufficient limit of detection (0.5 ng/mL), so it was found to be suitable for the analysis of nicotianamine in soy sauce and other foods, without cleanup. To subtract the matrix effect during LC-MS/MS analysis, a standard addition method was used. The levels of nicotianamine in soy sauce ranged from <0.25 to 71 μg/g. Nicotianamine was also determined in other foods, including soy milk, vegetable juice, fruit juice, and bottled tea.

[Determination of phthalate plasticizers in foods by high performance liquid chromatography with gel permeation chromatographic clean-up].

PubMed

Zhang, Chunyu; Wang, Hui; Zhang, Xiaohui; Ma, Zhongqiang; Deng, Wanmei; Hu, Ke; Ding, Mingyu

2011-12-01

A method of gel permeation chromatography-high performance liquid chromatography (GPC-HPLC) was established for the simultaneous determination of 5 main phthalate plasticizers in foods (edible oil, instant noodles, fried pastries, Saqima, etc.). The samples were extracted with petroleum ether in an ultrasonator, purified by a GPC column, and analyzed by HPLC. The chromatographic separation was achieved on a Labtech-C18 column (250 mm x 4.6 mm, 5 microm) using acetonitrile and water mixture as the mobile phases in a gradient elution mode. The developed method exhibited a linear correlation coefficient of more than 0.997 and the detection limits of 3.25 - 13.4 microg/L. The spike recoveries were between 70.4% and 113.6% with the relative standard deviations (RSDs, n = 3) of 0.3% - 5.8% at the spiked level of 50 mg/L. This method is simple, rapid and practical, and can be used for the simultaneous determination of PAEs in grease food samples.

Simultaneous determination of 20 pharmacologically active substances in cow's milk, goat's milk, and human breast milk by gas chromatography-mass spectrometry.

PubMed

Azzouz, Abdelmonaim; Jurado-Sánchez, Beatriz; Souhail, Badredine; Ballesteros, Evaristo

2011-05-11

This paper reports a systematic approach to the development of a method that combines continuous solid-phase extraction and gas chromatography-mass spectrometry for the simultaneous determination of 20 pharmacologically active substances including antibacterials (chloramphenicol, florfenicol, pyrimethamine, thiamphenicol), nonsteroideal anti-inflammatories (diclofenac, flunixin, ibuprofen, ketoprofen, naproxen, mefenamic acid, niflumic acid, phenylbutazone), antiseptic (triclosan), antiepileptic (carbamazepine), lipid regulator (clofibric acid), β-blockers (metoprolol, propranolol), and hormones (17α-ethinylestradiol, estrone, 17β-estradiol) in milk samples. The sample preparation procedure involves deproteination of the milk, followed by sample enrichment and cleanup by continuous solid-phase extraction. The proposed method provides a linear response over the range of 0.6-5000 ng/kg and features limits of detection from 0.2 to 1.2 ng/kg depending on the particular analyte. The method was successfully applied to the determination of pharmacologically active substance residues in food samples including whole, raw, half-skim, skim, and powdered milk from different sources (cow, goat, and human breast).

Fast determination of pyrethroid pesticides in tobacco by GC-MS-SIM coupled with modified QuEChERS sample preparation procedure.

PubMed

Gao, Yan; Sun, Ying; Jiang, Chunzhu; Yu, Xi; Wang, Yuanpeng; Zhang, Hanqi; Song, Daqian

2013-01-01

An analytical method was developed for the extraction and determination of pyrethroid pesticide residues in tobacco. The modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method was applied for preparing samples. In this study, methyl cyanide (MeCN)-saturated salt aqueous was used as the two-phase extraction solvent for the first time, and a vortex shaker was used for the simultaneous shaking and concentration of the analytes. The effects of experimental parameters on extraction and clean-up efficiency were investigated and optimized. The analytes were determined by gas chromatography-mass spectrometry-selected ion monitoring (GC-MS-SIM). The obtained recoveries of the analytes at three different fortification levels were 76.85-114.1% and relative standard deviations (RSDs) were lower than 15.7%. The limits of quantification (LOQs) were from 1.28 to 26.6 μg kg(-1). This method was also applied to the analysis of actual commercial tobacco products and the analytical results were satisfactory.

An HPLC method for determination of azadirachtin residues in bovine muscle.

PubMed

Gai, María Nella; Álvarez, Christian; Venegas, Raúl; Morales, Javier

2011-04-01

A high-performance liquid chromatography (HPLC) method for the determination of azadirachtin (A and B) residues in bovine muscle has been developed. Azadirachtin is a neutral triterpene and chemotherapeutic agent effective in controlling some pest flies in horses, stables, horns and fruit. The actual HPLC method uses an isocratic elution and UV detection. Liquid-liquid extraction and solid-phase purification was used for the clean-up of the biological matrix. The chromatographic determination of these components is achieved using a C18 analytical column with water-acetonitrile mixture (27.5:72.5, v/v) as mobile phase, 1 mL/min as flow rate, 45 °C column temperature and UV detector at 215 nm. The azadirachtin peaks are well resolved and free of interference from matrix components. The extraction and analytical method developed in this work allows the quantitation of azadirachtin with precision and accuracy, establishing a lower limit of quantitation of azadirachtin, extracted from the biological matrix.

ESTIMATING THE EXPOSURE POINT CONCENTRATION TERM USING PROUCL, VERSION 3.0

EPA Science Inventory

In superfund and RCRA Projects of the U.S. EPA, cleanup, exposure, and risk assessment decisions are often made based upon the mean concentrations of the contaminants of potential concern (COPC). A 95% upper confidence limit (UCL) of the population mean is used to estimate the e...

Risk based requirements for long term stewardship: A proof-of-principle analysis of an analytic method tested on selected Hanford locations

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

Jarvis, T.T.; Andrews, W.B.; Buck, J.W.

1998-03-01

Since 1989, the Department of Energy`s (DOE) Environmental Management (EM) Program has managed the environmental legacy of US nuclear weapons production, research and testing at 137 facilities in 31 states and one US territory. The EM program has conducted several studies on the public risks posed by contaminated sites at these facilities. In Risks and the Risk Debate [DOE, 1995a], the Department analyzed the risks at sites before, during, and after remediation work by the EM program. The results indicated that aside from a few urgent risks, most hazards present little inherent risk because physical and active site management controlsmore » limit both the releases of site contaminants, and public access to these hazards. Without these controls, these sites would pose greater risks to the public. Past risk reports, however, provided little information about post-cleanup risk, primarily because of uncertainty about future site uses and site characteristics at the end of planned cleanup activities. This is of concern because in many cases current cleanup technologies, and remedies, will last a shorter period of time than the waste itself and the resulting contamination will remain hazardous.« less

Development of a high performance liquid chromatography method and a liquid chromatography-tandem mass spectrometry method with the pressurized liquid extraction for the quantification and confirmation of sulfonamides in the foods of animal origin.

PubMed

Yu, Huan; Tao, Yanfei; Chen, Dongmei; Wang, Yulian; Huang, Lingli; Peng, Dapeng; Dai, Menghong; Liu, Zhenli; Wang, Xu; Yuan, Zonghui

2011-09-01

The residues of sulfonamides (SAs) in the foods of animal origin are of the major concern because they are harmful to the consumer's health and could induce pathogens to develop resistance. Rapid and efficient determination methods are urgently in need. A quantitative high performance liquid chromatography method (HPLC) and a confirmative liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of 18 sulfonamides such as sulfamidinum, sulfanilamide, sulfisomidine, sulfadiazine, sulfapyridine, sulfathiazole, sulfamerazine, sulfadimidine, sulfamethoxypyridazine, sulfamethoxydiazine, sulfisoxazole, sulfachloropyridazine, sulfamethoxazole, sulfamonomethoxine, sulfadoxine, sulfaclozine, sulfadimethoxine, sulfaquinoxaline in the muscles, livers and kidneys of swine, bovine and chicken were developed and validated. The sample preparation procedures included a pressurized liquid extraction (PLE) with acetonitrile conducted at elevated temperature (70°C) and pressure (1400 psi). After clean-up with hydrophilic-lipophilic balance cartridge, the extraction solution was concentrated and analyzed by HPLC and LC-MS/MS analysis. 18 SAs were separated by the HPLC with a Zorbax SB-Aq-C18 column and the mobile phase of methanol/acetonitrile/1% acetic acid with a gradient system. The wavelength of UV for the HPLC detection was set at 285 nm. The LC-MS/MS analysis was achieved with a Hypersil Golden column and the mobile phase of acetonitrile and 0.1% formic acid aqueous solution with two gradient systems. The Limits of detection (LOD) and the limits of quantitation (LOQ) were 3 μg/kg and 10 μg/kg, respectively, for both of the HPLC and LC-MS/MS. Linearity was obtained with an average coefficient of determination (R) higher than 0.9980 over a dynamic range from the LOQ value up to 5000 μg/kg. The recoveries of the methods range from 71.1% to 118.3% with the relative standard derivation less than 13%. The peaks of interest with no interferences were observed throughout the chromatographic run. The sample pretreatment provided efficient extraction and cleanup that enables a sensitive and rugged determination of 18 SAs, the obtained results revealed that PLE, in comparison with other sample preparation methods applied, has significantly higher efficacy for SAs isolation from animal tissues. Copyright © 2011 Elsevier B.V. All rights reserved.

EPRR

Science.gov Websites

Electronic Public Reading Room Operational Reading Room & Environmental Cleanup through April 2018 Los Alamos Legacy Cleanup Electronic Public Reading Room Environmental Cleanup from May 2018

33 CFR 165.1329 - Regulated Navigation Area; Thea Foss and Wheeler-Osgood Waterways EPA Superfund Cleanup Site...

Code of Federal Regulations, 2014 CFR

2014-07-01

... Foss and Wheeler-Osgood Waterways EPA Superfund Cleanup Site, Commencement Bay, Tacoma, WA. 165.1329... Area; Thea Foss and Wheeler-Osgood Waterways EPA Superfund Cleanup Site, Commencement Bay, Tacoma, WA... (EPA) and others in the Thea Foss and Wheeler-Osgood Waterways EPA superfund cleanup site. Vessels may...

33 CFR 165.1329 - Regulated Navigation Area; Thea Foss and Wheeler-Osgood Waterways EPA Superfund Cleanup Site...

Code of Federal Regulations, 2011 CFR

2011-07-01

... Foss and Wheeler-Osgood Waterways EPA Superfund Cleanup Site, Commencement Bay, Tacoma, WA. 165.1329... Area; Thea Foss and Wheeler-Osgood Waterways EPA Superfund Cleanup Site, Commencement Bay, Tacoma, WA... (EPA) and others in the Thea Foss and Wheeler-Osgood Waterways EPA superfund cleanup site. Vessels may...

33 CFR 165.1329 - Regulated Navigation Area; Thea Foss and Wheeler-Osgood Waterways EPA Superfund Cleanup Site...

Code of Federal Regulations, 2013 CFR

2013-07-01

... Foss and Wheeler-Osgood Waterways EPA Superfund Cleanup Site, Commencement Bay, Tacoma, WA. 165.1329... Area; Thea Foss and Wheeler-Osgood Waterways EPA Superfund Cleanup Site, Commencement Bay, Tacoma, WA... (EPA) and others in the Thea Foss and Wheeler-Osgood Waterways EPA superfund cleanup site. Vessels may...

33 CFR 165.1329 - Regulated Navigation Area; Thea Foss and Wheeler-Osgood Waterways EPA Superfund Cleanup Site...

Code of Federal Regulations, 2012 CFR

2012-07-01

... Foss and Wheeler-Osgood Waterways EPA Superfund Cleanup Site, Commencement Bay, Tacoma, WA. 165.1329... Area; Thea Foss and Wheeler-Osgood Waterways EPA Superfund Cleanup Site, Commencement Bay, Tacoma, WA... (EPA) and others in the Thea Foss and Wheeler-Osgood Waterways EPA superfund cleanup site. Vessels may...

Cleanups in My Community

EPA Pesticide Factsheets

Cleanups in My Community (CIMC) is a public web application that enables integrated access through maps, lists and search filtering to site-specific information EPA has across all cleanup programs. CIMC taps into data publicly available from EPA's EnviroFacts (RCRA Corrective Action facilities, Brownfields properties and grant areas, Superfund NPL sites, other facility data) and web services (water monitoring stations, impaired waters, emergency responses, tribal boundaries, congressional districts, etc.) and connects to other applications (e.g., Superfund's CPAD) to provide easy seamless access to site-specific cleanup information with explanatory text and within the context of related data. Data can be filtered by cleanup program, geography, environmental indicators, controls, and cleanup stage. CIMC also provides some web services that integrate these data for others to use in their applications.

Analysis of coffee for the presence of acrylamide by LC-MS/MS.

PubMed

Andrzejewski, Denis; Roach, John A G; Gay, Martha L; Musser, Steven M

2004-04-07

A variety of popular instant, ground, and brewed coffees were analyzed using a modified liquid chromatography-tandem mass spectrometry (LC-MS/MS) method specifically developed for the determination of acrylamide in foods. Coffee test portions were spiked with 13C3-labeled acrylamide as an internal standard prior to their extraction and cleanup. Ground coffees (1 g) and instant coffees (0.5 g) were extracted by shaking with 9 mL of water for 20 min. Brewed coffee test portions (9 mL) were taken through the cleanup procedure without further dilution with extraction solvent. Coffee test portions were cleaned up by passing 1.5 mL first through an Oasis HLB (hydrophilic/lipophilic copolymer sorbent) solid phase extraction (SPE) cartridge and then a Bond Elut-Accucat (cation and anion exchange sorbent) SPE cartridge. The cleaned up extracts were analyzed by positive ion electrospray LC-MS/MS. The MS/MS data was used to detect, confirm, and quantitate acrylamide. The limit of quantitation of the method was 10 ng/g for ground and instant coffees and 1.0 ng/mL for brewed coffee. The levels of acrylamide ranged from 45 to 374 ng/g in unbrewed coffee grounds, from 172 to 539 ng/g in instant coffee crystals, and from 6 to 16 ng/mL in brewed coffee.

CERCLIS Non-NPL Removal Sites in US EPA Region 3

EPA Pesticide Factsheets

This data layer contains point locations of waste sites throughout EPA Region 3 that have come under the jurisdiction of CERCLA. Congress passed the Comprehensive Environmental Response, Compensation, and Liability Act of 1980 (CERCLA, also known as Superfund) in response to a growing national concern about the release of hazardous substances from abandoned waste sites. Under CERCLA, Congress gave the federal government broad authority to regulate hazardous substances, to respond to hazardous substance emergencies, and to develop long-term solutions for the Nation's most serious hazardous waste problems. The 1980 law requires the parties responsible for the contamination to conduct or pay for the cleanup. If the Environmental Protection Agency's (EPA's) efforts to take an enforcement action for the cleanup are not successful, the federal government can clean up a site using the CERCLA Trust Fund. If the Superfund program conducts the cleanup, the government can take court action against responsible parties to recover up to three times the cleanup costs. These sites do not meet the requirements for the National Priority List, but are still part of the CERCLA list. The National Priority List is intended primarily to guide the EPA in determining which sites warrant further investigation. Some of these waste sites are also known as removal sites, where waste and/or soils are transported away from the site. This point location data was extracted by US EPA Region 3 pe

Determination of quinolones and fluoroquinolones, tetracyclines and sulfonamides in bovine, swine and poultry liver using LC-MS/MS.

PubMed

Martins, Magda Targa; Barreto, Fabiano; Hoff, Rodrigo Barcelos; Jank, Louise; Arsand, Juliana Bazzan; Feijó, Tiago Correa; Schapoval, Elfrides Eva Scherman

2015-01-01

Antibacterials are widely used in veterinary medicine. Residues of these drugs can remain in food of animal origin, including bovine liver. This paper describes a fast and simple analytical method for the determination of quinolones and fluoroquinolones, tetracyclines and sulfonamides in bovine liver samples. Deuterated enrofloxacin, sulfapyridine and demeclocycline were used as internal standards. The homogenised liver samples were extracted with acidified acetonitrile. Steps of non-solid-phase extraction (SPE) clean-up and concentration were used in the presented method. The final extracts were analysed by sensitive and selective detection of all components in a single run using LC-MS/MS. Acceptable recoveries between 66% and 110% were obtained. Good linearity (r(2)) above 0.96, considering three different days, for all drugs was achieved in concentrations ranging from 0.0 to 2.0 × the maximum residue limit (MRL). Intraday precision with coefficient of variation (CV%) (n = 6) lower than 14.7% and inter-day precision lower than 18.8% in agreement with European Commission Decision 2002/657/EC were obtained in concentrations ranging from 0.5 to 1.5 MRL. Accuracy was between 86% and 110%. Limits of detection and quantitation, as well as decision limit (CCα) and detection capability (CCβ), were also evaluated.

Mental health and alcohol problems among Estonian cleanup workers 24 years after the Chernobyl accident.

PubMed

Laidra, Kaia; Rahu, Kaja; Tekkel, Mare; Aluoja, Anu; Leinsalu, Mall

2015-11-01

To study the long-term mental health consequences of the 1986 Chernobyl nuclear accident among cleanup workers from Estonia. In 2010, 614 Estonian Chernobyl cleanup workers and 706 geographically and age-matched population-based controls completed a mail survey that included self-rated health, the Posttraumatic Stress Disorder Checklist (PCL), alcohol symptoms (AUDIT), and scales measuring depressive, anxiety, agoraphobia, fatigue, insomnia, and somatization symptoms. Respondents were dichotomized into high (top quartile) and low symptom groups on each measure. Logistic regression analysis detected significant differences between cleanup workers and controls on all measures even after adjustment for ethnicity, education, marital status, and employment status. The strongest difference was found for somatization, with cleanup workers being three times more likely than controls to score in the top quartile (OR = 3.28, 95% CI 2.39-4.52), whereas for alcohol problems the difference was half as large (OR = 1.52, 95% CI 1.16-1.99). Among cleanup workers, arrival at Chernobyl in 1986 (vs. later) was associated with sleep problems, somatization, and symptoms of agoraphobia. The toll of cleanup work was evident 24 years after the Chernobyl accident among Estonian cleanup workers indicating the need for focused mental health interventions.

Determination of polycyclic aromatic hydrocarbons in biochar and biochar amended soil

USDA-ARS?s Scientific Manuscript database

A method for the determination of the 16 USEPA polycyclic aromatic hydrocarbons (PAHs) in biochar and soil amended with biochar was developed. Samples were Soxhlet extracted with acetone:cyclohexane 1:1, and PAHs were analysed by GC-MS after silica gel clean-up. In a comparative study based on reflu...

The ecological impact of land restoration and cleanup. Technical report

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

Not Available

1978-08-01

The report is concerned with the ecological impacts of specific cleanup treatment on the land where they were carried out. The cleanup procedures given apply equally to chemical or radioactive materials. Guidance is provided for cleanup procedures likely to be suggested by government, industry, or environmental groups. The basic types of cleanup procedures for removing or deactiving spilled contamination involve moving people and animals from the affected area, scraping and grading the contaminated soil into windrows, plowing the contamination under, or digging up the contamination and hauling it away. The report describes and evaluates the various land-type cleanup effects inmore » terms of impact of the techniques on the environment. Part I defines several natural ecosystems and some of their natural derivations. Part II presents managed ecosystems which are imposed on natural ecosystems and are no longer bound by the initial native ecosystem balances. Part III deals with avion and mammilian wild life displaced by cleanup.« less

Greener Cleanups

EPA Pesticide Factsheets

OSWER’s goal is to reduce the environmental footprint of cleanup activities at contaminated sites to the maximum extent possible. This website shares policies, tools and practices to achieve that goal across cleanup programs.

[Determination of short-chain chlorinated paraffins in ambient air using high-volume sampling combined with high resolutimi gas chromatography-electron capture negative ion-low resolution mass spectrometry].

PubMed

Shi, Loimeng; Gao, Yuan; Hou, Xiaohong; Zhang, Haijun; Zhang, Yichi; Chen, Jiping

2016-02-01

An analytical method for quantifying short-chain chlorinated paraffins (SCCPs) in ambient air using high-volume sampling combined with high resolution gas chromatography-electron capture negative ion-low resolution mass spectrometry ( HRGC-ECNI-LRMS) was developed. An acidified silica gel column and a basic alumina column were used to optimize the cleanup procedures. The results showed a good linearity (R2>0. 99) between the total response factors and the degree of chlorination of SCCPs in the content range of 58. 1%-63. 3%. The limits of detection (S/N ≥3) and the limits of quantification (S/N ≥ 10) were 4. 2 and 12 µg, respectively. The method detection limit (MDL) for SCCPs was 0. 34 ng/m3 (n = 7). The recoveries of SCCPs in air samples were in the range of 81. 9% to 94. 2%. It is demonstrated that the method is suitable for the quantitative analysis of SCCPs in air samples.

Determination of siloxanes in silicone products and potential migration to milk, formula and liquid simulants.

PubMed

Zhang, Kai; Wong, Jon W; Begley, Timothy H; Hayward, Douglas G; Limm, William

2012-08-01

A pressurised solvent extraction procedure coupled with a gas chromatography-mass spectrometry-selective ion monitoring (GC-MS-SIM) method was developed to determine three cyclic siloxanes, octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), dodecamethylcyclohexasiloxane (D6) and three linear siloxanes, octamethyltrisiloxane (L3), decamethyltetrasiloxane (L4), dodecamethylpentasiloxane (L5), in silicone products. Additionally, two different extraction methods were developed to measure these siloxanes migrating into milk, infant formula and liquid simulants (50 and 95% ethanol in water). The limits of quantification (LOQs) of the six siloxanes ranged from 6 ng/g (L3) to 15 ng/g (D6). Silicone nipples and silicone bakewares were extracted using pressurised solvent extraction (PSE) and analysed using the GC-MS-SIM method. No linear siloxanes were detected in the silicone nipple samples analysed. The three cyclic siloxanes (D4, D5 and D6) were detected in all silicone nipple samples with concentrations ranging from 0.5 to 269 µg/g. In the bakeware samples, except for L3, the other five siloxanes were detected with concentrations ranging from 0.2 µg/g (L4) to 7030 µg/g (D6). To investigate the potential migration of the six siloxanes from silicone nipples to milk and infant formula, a liquid extraction and dispersive clean-up procedure was developed for the two matrices. The procedure used a mix of hexane and ethyl acetate (1 : 1, v/v) as extraction solvent and C₁₈ powder as the dispersive clean-up sorbent. For the liquid simulants, extraction of the siloxanes was achieved using hexane without any salting out or clean-up procedures. The recoveries of the six siloxanes from the milk, infant formula and simulants fortified at 50, 100, 200, 500 and 1000 µg/l ranged from 70 to 120% with a relative standard derivation (RSD) of less than 15% (n = 4). Migration tests were performed by exposing milk, infant formula and the liquid simulants to silicone baking sheets with known concentrations of the six siloxanes at 40°C. No siloxanes were detected in milk or infant formula after 6 h of direct contact with the silicone baking sheet plaques, indicating insignificant migration of the siloxanes to milk or infant formula. Migration tests in the two simulants lasted up to 72 h and the three cyclic siloxanes were detected in 50% ethanol after an 8-h exposure and after 2 h in 95% ethanol. The highest detected concentrations of D4, D5 and D6 were 42, 36 and 155 ng/ml, respectively, indicating very limited migration of D4, D5 or D6 into the two simulants.

United States v. M/V Big Sam: preserving a niche for the federal common law of maritime tort of oil pollution

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

Murway, A.

1984-07-01

When the M/V Big Sam tugboat struck an oil-carrying barge in 1975, the district court held that no tort action existed, and limited the government's claim for cleanup compensation to the Federal Water Pollution Control Act (FWPCA) and a potential yield of only $15,500. The author traces the foundations of the defendant's claim that Congress intended the FWPCA to be the government's exclusive means of recovery oil cleanup costs and, citing prior case law, discusses the arguments and applies the exclusivity test to the Fifth Circuit's decision in M/V Big Sam. She concludes that the courts viewed Congress' major goalsmore » under the FWPCA to be the elimination of oil pollution and the protection of the merchant marine from potentially uninsurable risks arising out of the nation's growing environmental consciousness. Although a potential threat to the shipping and insurance companies, the court limited its ruling to third-party vessels already protected from unlimited liability. 91 references.« less

Evaluation of direct analysis in real time for the determination of highly polar pesticides in lettuce and celery using modified Quick Polar Pesticides Extraction method.

PubMed

Lara, Francisco J; Chan, Danny; Dickinson, Michael; Lloyd, Antony S; Adams, Stuart J

2017-05-05

Direct analysis in real time (DART) was evaluated for the determination of a number of highly polar pesticides using the Quick Polar Pesticides Extraction (QuPPe) method. DART was hyphenated to high resolution mass spectrometry (HRMS) in order to get the required selectivity that allows the determination of these compounds in complex samples such as lettuce and celery. Experimental parameters such as desorption temperature, scanning speed, and distances between the DART ion source and MS inlet were optimized. Two different mass analyzers (Orbitrap and QTOF) and two accessories for sample introduction (Dip-it ® tips and QuickStrip™ sample cards) were evaluated. An extra clean-up step using primary-secondary amine (PSA) was included in the QuPPe method to improve sensitivity. The main limitation found was in-source fragmentation, nevertheless QuPPe-DART-HRMS proved to be a fast and reliable tool with quantitative capabilities for at least seven compounds: amitrole, cyromazine, propamocarb, melamine, diethanolamine, triethanolamine and 1,2,4-triazole. The limits of detection ranged from 20 to 60μg/kg. Recoveries for fortified samples ranged from 71 to 115%, with relative standard deviations <18%. Copyright © 2017 Elsevier B.V. All rights reserved.

Analytical method for the evaluation of the outdoor air contamination by emerging pollutants using tree leaves as bioindicators.

PubMed

Barroso, Pedro José; Martín, Julia; Santos, Juan Luis; Aparicio, Irene; Alonso, Esteban

2018-01-01

In this work, an analytical method, based on sonication-assisted extraction, clean-up by dispersive solid-phase extraction and determination by liquid chromatography-tandem mass spectrometry, has been developed and validated for the simultaneous determination of 15 emerging pollutants in leaves from four ornamental tree species. Target compounds include perfluorinated organic compounds, plasticizers, surfactants, brominated flame retardant, and preservatives. The method was optimized using Box-Behnken statistical experimental design with response surface methodology and validated in terms of recovery, accuracy, precision, and method detection and quantification limits. Quantification of target compounds was carried out using matrix-matched calibration curves. The highest recoveries were achieved for the perfluorinated organic compounds (mean values up to 87%) and preservatives (up to 88%). The lowest recoveries were achieved for plasticizers (51%) and brominated flame retardant (63%). Method detection and quantification limits were in the ranges 0.01-0.09 ng/g dry matter (dm) and 0.02-0.30 ng/g dm, respectively, for most of the target compounds. The method was successfully applied to the determination of the target compounds on leaves from four tree species used as urban ornamental trees (Citrus aurantium, Celtis australis, Platanus hispanica, and Jacaranda mimosifolia). Graphical abstract Analytical method for the biomonitorization of emerging pollutants in outdoor air.

Voluntary Guidelines for Methamphetamine Laboratory Cleanup - Document

EPA Pesticide Factsheets

provides technical guidance for state and local personnel responsible for meth lab cleanup, based on an extensive review of the best available science and practices, and addresses general cleanup activities, specific items/materials, sampling.

Multi-pesticides residue analysis of grains using modified magnetic nanoparticle adsorbent for facile and efficient cleanup.

PubMed

Liu, Zhenzhen; Qi, Peipei; Wang, Xiangyun; Wang, Zhiwei; Xu, Xiahong; Chen, Wenxue; Wu, Liyu; Zhang, Hu; Wang, Qiang; Wang, Xinquan

2017-09-01

A facile, rapid sample pretreatment method was developed based on magnetic nanoparticles for multi-pesticides residue analysis of grains. Magnetite (Fe 3 O 4 ) nanoparticles modified with 3-(N,N-diethylamino)propyltrimethoxysilane (Fe 3 O 4 -PSA) and commercial C18 were selected as the cleanup adsorbents to remove the target interferences of the matrix, such as fatty acids and non-polar compounds. Rice was used as the representative grain sample for method optimization. The amount of Fe 3 O 4 -PSA and C18 were systematically investigated for selecting the suitable purification conditions, and the simultaneous determination of 50 pesticides and 8 related metabolites in rice was established by liquid chromatography-tandem mass spectrometry. Under the optimal conditions, the method validation was performed including linearity, sensitivity, matrix effect, recovery and precision, which all satisfy the requirement for pesticides residue analysis. Compared to the conventional QuEChERS method with non-magnetic material as cleanup adsorbent, the present method can save 30% of the pretreatment time, giving the high throughput analysis possible. Copyright © 2017 Elsevier Ltd. All rights reserved.

Delineating high-density areas in spatial Poisson fields from strip-transect sampling using indicator geostatistics: application to unexploded ordnance removal.

PubMed

Saito, Hirotaka; McKenna, Sean A

2007-07-01

An approach for delineating high anomaly density areas within a mixture of two or more spatial Poisson fields based on limited sample data collected along strip transects was developed. All sampled anomalies were transformed to anomaly count data and indicator kriging was used to estimate the probability of exceeding a threshold value derived from the cdf of the background homogeneous Poisson field. The threshold value was determined so that the delineation of high-density areas was optimized. Additionally, a low-pass filter was applied to the transect data to enhance such segmentation. Example calculations were completed using a controlled military model site, in which accurate delineation of clusters of unexploded ordnance (UXO) was required for site cleanup.

Occurrence of ochratoxin A in wine and beer samples from China.

PubMed

Wu, Jianwei; Tan, Yinfeng; Wang, Yuqi; Xu, Rong

2011-01-01

A total of 125 wine and beer samples, including 42 white, 63 red wine and 20 beer samples, originating from several areas of China were analyzed for ochratoxin A (OTA). An analytical method based on immunoaffinity column (IAC) for clean-up and high performance liquid chromatography with fluorescence detection (HPLC-FD) was used to determine OTA. Positive results were further confirmed by LC-MS-MS. OTA was detected in 22 (17.6%) samples at levels of 0.02-1.18 ng/ml, which were below the EU maximum limit. The mean OTA concentration in red wine was slightly higher than in white wine. This study showed that OTA occurs in wine and beer in China but at levels that pose no danger of significant human exposure to OTA from this source.

Ion-exchange solid-phase extraction combined with liquid chromatography-tandem mass spectrometry for the determination of veterinary drugs in organic fertilizers.

PubMed

Zhao, Zhiyong; Zhang, Yanmei; Xuan, Yanfang; Song, Wei; Si, Wenshuai; Zhao, Zhihui; Rao, Qinxiong

2016-06-01

The analysis of veterinary drugs in organic fertilizers is crucial for an assessment of potential risks to soil microbial communities and human health. We develop a robust and sensitive method to quantitatively determine 19 veterinary drugs (amantadine, sulfonamides and fluoroquinolones) in organic fertilizers. The method involved a simple solid-liquid extraction step using the combination of acetonitrile and McIlvaine buffer as extraction solvent, followed by cleanup with a solid-phase extraction cartridge containing polymeric mixed-mode anion-exchange sorbents. Ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was used to separate and detect target analytes. We particularly focused on the optimization of sample clean-up step: different diluents and dilution factors were tested. The developed method was validated in terms of linearity, recovery, precision, sensitivity and specificity. The recoveries of all the drugs ranged from 70.9% to 112.7% at three concentration levels, with the intra-day and inter-day relative standard deviation lower than 15.7%. The limits of quantification were between 1.0 and 10.0μg/kg for all the drugs. Matrix effect was minimized by matrix-matched calibration curves. The analytical method was successfully applied for the survey of veterinary drugs contamination in 20 compost samples. The results indicated that fluoroquinolones had higher incidence rate and mean concentration levels ranging from 31.9 to 308.7μg/kg compared with other drugs. We expect the method will provide the basis for risk assessment of veterinary drugs in organic fertilizers. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of T-2 toxin, HT-2 toxin, and three other type A trichothecenes in layer feed by high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS)--comparison of two sample preparation methods.

PubMed

Bernhardt, Katrin; Valenta, Hana; Kersten, Susanne; Humpf, Hans-Ulrich; Dänicke, Sven

2016-05-01

A sensitive method for the simultaneous determination of T-2 toxin, HT-2 toxin, neosolaniol, T-2 triol, and T-2 tetraol in layer feed using high-performance liquid chromatography coupled to triple quadrupole mass spectrometry in the positive ionization mode (LC-ESI-MS/MS) is described. Two fast and easy clean-up methods-with BondElut Mycotoxin and MycoSep 227 columns, respectively-were tested. The separation of the toxins was conducted on a Pursuit XRs Ultra 2.8 HPLC column using 0.13 mM ammonium acetate as eluent A and methanol as eluent B. Detection of the mycotoxins was carried out in the multiple reaction monitoring (MRM) mode using ammonium adducts as precursor ions. Quantification of all analytes was performed with d3-T-2 toxin as an internal standard. The clean-up method with MycoSep 227 columns gave slightly better results for layer feed compared to the method using BondElut Mycotoxin columns (MycoSep 227: recovery between 50 and 63%, BondElut Mycotoxin: recovery between 32 and 67%) and was therefore chosen as the final method. The limits of detection ranged between 0.9 and 7.5 ng/g depending on the mycotoxin. The method was developed for the analysis of layer feed used at carry-over experiments with T-2 toxin in laying hens. For carry-over experiments, it is necessary that the method includes not only T-2 toxin but also the potential metabolites in animal tissues HT-2 toxin, neosolaniol, T-2 triol, and T-2 tetraol which could naturally occur in cereals used as feed stuff as well.

Simple determination of betaine, l-carnitine and choline in human urine using self-packed column and column-switching ion chromatography with nonsuppressed conductivity detection.

PubMed

Wei, Dan; Zhu, Yan; Guo, Ming

2018-02-01

A sequential online extraction, clean-up and separation system for the determination of betaine, l-carnitine and choline in human urine using column-switching ion chromatography with nonsuppressed conductivity detection was developed in this work. A self-packed pretreatment column (50 × 4.6 mm, i.d.) was used for the extraction and clean-up of betaine, l-carnitine and choline. The separation was achieved using self-packed cationic exchange column (150 × 4.6 mm, i.d.), followed by nonsuppressed conductivity detection. Under optimized experimental conditions, the developed method presented good analytical performance, with excellent linearity in the range of 0.60-100 μg mL -1 for betaine, 0.75-100 μg mL -1 for l-carnitine and 0.50-100 μg mL -1 for choline, with all correlation coefficients (R 2 ) >0.99 in urine. The limits of detection were 0.15 μg mL -1 for betaine, 0.20 μg mL -1 for l-carnitine and 0.09 μg mL -1 for choline. The intra- and inter-day accuracy and precision for all quality controls were within ±10.32 and ±9.05%, respectively. Satisfactory recovery was observed between 92.8 and 102.0%. The validated method was successfully applied to the detection of urinary samples from 10 healthy people. The values detected in human urine using the proposed method showed good agreement with the measurement reported previously. Copyright © 2017 John Wiley & Sons, Ltd.

Validation of a pressurized solvent extraction and GC-NCI-MS method for the low level determination of 40 polybrominated diphenyl ethers in mothers' milk.

PubMed

Lacorte, Silvia; Guillamon, Míriam

2008-08-01

This study reports an efficient method for the determination of 40 PBDEs from mono- to hepta-brominated in human milk. Pressurized liquid extraction (PLE) was optimized to recover PBDEs in a quantitative way using 1g of freeze dried milk. Due to the great amount of coextracted compounds, the clean-up step was optimized using alumina SPE disposable cartridges of 2 and 5 g. Whereas 2g alumina SPE failed in providing good extraction yields, all PBDEs were satisfactorily recovered using 5 g alumina SPE cartridges. Detection was performed with gas chromatography coupled to mass spectrometry with negative chemical ionization and method detection limits ranged from 0.01 to 0.05 microg kg(-1) wet weight (ww) with a good intra and inter-day variation (coefficient of variation lower than 13.4%). This method was validated by participating in an interlaboratory exercise from Quasimeme (United Kingdom), where a standard solution containing seven congeners and a certified unspiked mothers' milk were analyzed. In the standard mixture, levels between 96.915 and 570.172 microg l(-1) were quantified, whereas in certified mothers' milk, BDEs 47, 99, 100 and 154 were detected at levels from 0.010 and 0.061 microg kg(-1) ww, with an error <30%. The applicability of the method was tested experimentally in five mothers' milk samples, where only BDE 47 was detected at a maximum concentration of 10.45 microg kg(-1) lipid weight (lw). PLE succeeded in extracting all PBDEs from the sample with good reproducibility although the clean-up step had to be severely performed to eliminate sample interferences such as milk lipids and proteins.

Quantitative determination of several synthetic corticosteroids by gas chromatography-mass spectrometry after purification by immunoaffinity chromatography.

PubMed

Delahaut, P; Jacquemin, P; Colemonts, Y; Dubois, M; De Graeve, J; Deluyker, H

1997-08-29

A study was conducted to test a multiresidue analytical procedure for detecting and quantifying several corticosteroids on which the European Union imposes maximum residue limits (MRLs). Primary extracts from different matrices (liver, milk, urine, faeces) were first purified on C18 cartridges. A new immunoaffinity clean-up step was included. The immunoaffinity gel was used to purify several corticosteroids simultaneously with enrichment of the corresponding fractions. The extracts were treated with an aqueous solution of pyridinium chlorochromate to fully oxidise all corticosteroids and to facilitate their extraction with dichloromethane. After evaporation, the final extract was reconstituted with toluene before injection into the GC-MS apparatus. The analysis was performed in the CI-negative ionisation mode using ammonia as the reactant gas. The estimated detection and quantification limits were, respectively, 0.25 and 0.5 ppb or lower. Overall, the method is reproducible to within 20%. Recovery is between 50 and 80% according to the corticosteroid.

Dissipation and residue of myclobutanil in lychee.

PubMed

Liu, Yanping; Sun, Haibin; Liu, Fengmao; Wang, Siwei

2012-06-01

The dissipation and residue of myclobutanil in lychee under field conditions were studied. To determine myclobutanil residue in samples, an analytical method with a florisil column clean-up and detected by gas chromatography-electron capture detector (GC-ECD) was developed. Recoveries were found in the range of 83.24 %-89.00 % with relative standard deviations of 2.67 %-9.88 %. This method was successfully applied to analyze the dissipation and residue of myclobutanil in lychee in Guangdong and Guangxi Province, China. The half lives in lychee were from 2.2 to 3.4 days. The residues of myclobutanil in lychee flesh were all below the limit of quantification (LOQ) value (0.01 mg/kg), and most of the residues were concentrated in the peel. The terminal residues of myclobutanil were all bellow the maximum residue limit (MRL) value set by European Union (EU) (0.02 mg/kg). Hence it was safe for the use of this pesticide and the results also could give a reference for MRL setting of myclobutanil in lychee in China.

Gas chromatography with flame photometric detection of 31 organophosphorus pesticide residues in Alpinia oxyphylla dried fruits.

PubMed

Zhao, Xiangsheng; Kong, Weijun; Wei, Jianhe; Yang, Meihua

2014-11-01

A simple, rapid and effective gas chromatography-flame photometric detection method was established for simultaneous multi-component determination of 31 organophosphorus pesticides (OPPs) residues in Alpinia oxyphylla, which is widely consumed as a traditional medicine and food in China. Sample preparation was completed in a single step without any clean-up procedure. All pesticides expressed good linear relationships between 0.004 and 1.0 μg/mL with correlation coefficients higher than 0.9973. The method gave satisfactory recoveries for most pesticides. The limits of detection varied from 1 to 10 ng/mL, and the limits of quantification (LOQs) were between 4 and 30 ng/mL. The proposed method was successfully applied to 55 commercial samples purchased from five different areas. Five pesticide residues were detected in four (7.27%) samples. The positive samples were confirmed by gas chromatography with tandem mass spectrometry (GC-MS/MS). Copyright © 2014 Elsevier Ltd. All rights reserved.

Simultaneous determination of atropine and scopolamine in buckwheat and related products using modified QuEChERS and liquid chromatography tandem mass spectrometry.

PubMed

Chen, Hongping; Marín-Sáez, Jesús; Romero-González, Roberto; Garrido Frenich, Antonia

2017-03-01

A method was developed for the determination of atropine and scopolamine in buckwheat and related products. A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction procedure was evaluated. Dispersive solid phase extraction (d-SPE) was studied as clean-up step, using graphitized black carbon (GBC) and primary secondary amine (PSA). The extract was diluted with water (50:50, v/v) prior to chromatographic analysis. The method was validated and recoveries (except chia samples spiked at 10μg/kg) ranged from 75% to 92%. Intra and inter-day precision was lower than or equal to 17%. The limit of quantification of atropine and scopolamine was 0.4 and 2μg/kg, respectively. Eight types of samples (buckwheat, wheat, soy, buckwheat flour, buckwheat noodle, amaranth grain, chia seeds and peeled millet) were analyzed. Target compounds were not found above the detection limits of the method, but three transformation products of scopolamine (norscopine, hydroscopolamine and dihydroxyscopolamine) were putative identified in the tested samples using high resolution mass spectrometry (Exactive-Orbitrap). Copyright © 2016 Elsevier Ltd. All rights reserved.

Development and Validation of GC-ECD Method for the Determination of Metamitron in Soil

PubMed Central

Tandon, Shishir; Kumar, Satyendra; Sand, N. K.

2015-01-01

This paper aims at developing and validating a convenient, rapid, and sensitive method for estimation of metamitron from soil samples.Determination andquantification was carried out by Gas Chromatography on microcapillary column with an Electron Capture Detector source. The compound was extracted from soil using methanol and cleanup by C-18 SPE. After optimization, the method was validated by evaluating the analytical curves, linearity, limits of detection, and quantification, precision (repeatability and intermediate precision), and accuracy (recovery). Recovery values ranged from 89 to 93.5% within 0.05- 2.0 µg L−1 with average RSD 1.80%. The precision (repeatability) ranged from 1.7034 to 1.9144% and intermediate precision from 1.5685 to 2.1323%. Retention time was 6.3 minutes, and minimum detectable and quantifiable limits were 0.02 ng mL−1 and 0.05 ng g−1, respectively. Good linearity (R 2 = 0.998) of the calibration curves was obtained over the range from 0.05 to 2.0 µg L−1. Results indicated that the developed method is rapid and easy to perform, making it applicable for analysis in large pesticide monitoring programmes. PMID:25733978

Rapid determination of ractopamine residues in edible animal products by enzyme-linked immunosorbent assay: development and investigation of matrix effects.

PubMed

Zhang, Yan; Wang, Fengxia; Fang, Li; Wang, Shuo; Fang, Guozhen

2009-01-01

To determine ractopamine residues in animal food products (chicken muscle, pettitoes, pig muscle, and pig liver), we established a rapid direct competitive enzyme-linked immunosorbent assay (ELISA) using a polyclonal antibody generated from ractopamine-linker-BSA. The antibody showed high sensitivity and specificity in phosphate buffer, with an IC(50) of 0.6 ng/mL, and the limit of detection was 0.04 ng/mL. The matrix effect of the samples was easily eliminated by one-step extraction with PBS, without any organic solution or clean-up procedure such as SPE or liquid-liquid extraction, making it a much more simple and rapid method than previously reported ones. The detection limit in blank samples was 0.2 mug/kg. To validate this new RAC (ractopamine hydrochloride) ELISA, a RAC-free pig liver sample spiked at three different concentrations was prepared and analyzed by HPLC and ELISA. The results showed a good correlation between the data of ELISA and HPLC (R(2) > 0.95), which proves that the established ELISA is accurate enough to quantify the residue of RAC in the animal derived foods.

Polyamide as an efficient sorbent for simultaneous interface-free determination of three Sudan dyes in saffron and urine using high-performance liquid chromatography-ultra violet detection.

PubMed

Saeidi, Iman; Barfi, Behruz; Payrovi, Moazameh; Feizy, Javid; Sheibani, Hojat A; Miri, Mina; Ghollasi Moud, Farahnaz

2015-01-01

With polyamide (PA) as an efficient sorbent for solid phase extraction (SPE) of Sudan dyes II, III and Red 7B from saffron and urine, their determination by HPLC was performed. The optimum conditions for SPE were achieved using 7 mL methanol/water (1:9, v/v, pH 7) as the washing solvent and 3 mL tetrahydrofuran for elution. Good clean-up and high (above 90%) recoveries were observed for all the analytes. The optimized mobile phase composition for HPLC analysis of these compounds was methanol-water (70:30, v/v). The SPE parameters, such as the maximum loading capacity and breakthrough volume, were also determined for each analyte. The limits of detection (LODs), limits of quantification (LOQs), linear ranges and recoveries for the analytes were 4.6-6.6 microg/L, 13.0-19.8 microg/L, 13.0-5000 microg/L (r2>0.99) and 92.5%-113.4%, respectively. The precisions (RSDs) of the overall analytical procedure, estimated by five replicate measurements for Sudan II, III and Red 7B in saffron and urine samples were 2.3%, 1.8% and 3.6%, respectively. The developed method is simple and successful in the application to the determination of Sudan dyes in saffron and urine samples with HPLC coupled with UV detection.

Changing the focus of Brownfields cleanups

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

Cichon, E.

The Brownfields Tax Incentive proposed by President Clinton illustrates the remarkable evolution in the government`s view of contaminated property remediation. The current program, spearheaded by the president`s Brownfields Initiative, reflects a significant shift of emphasis. Remedial programs now pinpoint the end use of the affected property as the ultimate objective, with the required cleanup of impacted media regarded as only one of several elements. In place of enforcement, government now is employing incentives--from federal policies limiting landowner liability to proposed tax incentives--to eliminate traditional obstacles to the remediation and reuse of contaminated land. Some three dozen Brownfields Initiative pilot projectsmore » have been launched across the country. These first-generation brownfields remediation efforts demonstrate that to realize the program`s regulatory and economic advantages, practical and cost-effective remedial efforts are required.« less

Corrective Action Sites around the Nation

EPA Pesticide Factsheets

Provide info to the public/community orgs, local officials & consultants on nearby corrective action cleanups, the status of the cleanup and future plans. Links to the Natl Corrective Action, Cleanups in My Community & Cleaning Up Our Land, Water & Air

Green Remediation Best Management Practices: Overview of EPA's Methodology to Address the Environmental Footprint of Site Cleanup

EPA Pesticide Factsheets

Contaminated site cleanups involving complex activities may benefit from a detailed environmental footprint analysis to inform decision-making about application of suitable best management practices for greener cleanups.

Military Base Realignments and Closures: DOD Has Improved Environmental Cleanup Reporting but Should Obtain and Share More Information

DTIC Science & Technology

2017-01-01

the property, put final cleanup remedies in place before the property is transferred. However, under some circumstances the services may conduct an...early transfer before cleanup has been completed. When remedies are in place for addressing the contamination of a former installation or the...cleanup at BRAC installations will significantly increase due to the high cost of remediating emerging contaminants, primarily perfluorooctane

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

Kamboj, Sunita; Durham, Lisa A.

A post-remediation radiological dose assessment was conducted for the Formerly Utilized Sites Remedial Action Program (FUSRAP) Linde Site by using the measured residual concentrations of the radionuclides of concern following the completion of the soils remedial action. The site’s FUSRAP-related contaminants of concern (COCs) are radionuclides associated with uranium processing activities conducted by the Manhattan Engineer District (MED) in support of the Nation’s early atomic energy and weapons program and include radium-226 (Ra-226), thorium-230 (Th-230), and total uranium (Utotal). Remedial actions to address Linde Site soils and structures were conducted in accordance with the Record of Decision for the Lindemore » Site, Tonawanda, New York (ROD) (USACE 2000a). In the ROD, the U.S. Army Corps of Engineers (USACE) determined that the cleanup standards found in Title 40, Part 192 of the Code of Federal Regulations (40 CFR Part 192), the standards for cleanup of uranium mill sites designated under the Uranium Mill Tailings Radiation Control Act (UMTRCA), and the Nuclear Regulatory Commission (NRC) standards for decommissioning of licensed uranium and thorium mills, found in 10 CFR Part 40, Appendix A, Criterion 6(6), are Applicable or Relevant and Appropriate Requirements (ARARs) for cleanup of MED-related contamination at the Linde Site. The major elements of this remedy will involve excavation of the soils with COCs above soil cleanup levels and placement of clean materials to meet the other criteria of 40 CFR Part 192.« less

The National LUST Cleanup Backlog: A Study of Opportunities

EPA Pesticide Factsheets

To understand the makeup of UST releases remaining and why the pace of cleanups is slowing, EPA undertook a two-phase, data-driven analysis of the cleanups remaining as of 2006 (Phase 1) and 2009 (Phase 2).

Science plus management equals successful remediation: A case study

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

Buehlman, M.D.; Rogers, D.T.; Payne, F.C.

A case study involving a Brownfields site in southeastern Michigan clearly illustrates the elements of successful remediation. The site`s soil was contaminated with polychlorinated biphenyls (PCBs) and its groundwater with a variety of chlorinated solvents. The original estimate for remediation has exceeded $30 million. Several phases of investigation were conducted to evaluate the nature and sources of contaminants, the site`s hydrogeology, potential risks to human health and the environment, and feasible remedial technologies. Multiple cleanup criteria were established for different affected areas based on the results of the investigations, changes that were taking place with the state cleanup regulations andmore » standards and subsequent negotiations with state and federal regulators. Innovative remedial technologies were selected. The result was a remediation that met or exceeded all soil and groundwater cleanup objectives, was performed on schedule, and was highly cost-effective. The final cost was limited to $3 million--one-tenth of the original estimate. The success of this project involved meticulous scientific study and comprehensive understanding of applicable regulatory requirements and available remediation technologies. It also required effective project management to coordinate the multidisciplinary efforts involved and to maintain the constant vertical and horizontal communications necessary to ensure sound decisions at every step in the process.« less

Investigation of post hydraulic fracturing well cleanup physics in the Cana Woodford Shale

NASA Astrophysics Data System (ADS)

Lu, Rong

Hydraulic fracturing was first carried out in the 1940s and has gained popularity in current development of unconventional resources. Flowing back the fracturing fluids is critical to a frac job, and determining well cleanup characteristics using the flowback data can help improve frac design. It has become increasingly important as a result of the unique flowback profiles observed in some shale gas plays due to the unconventional formation characteristics. Computer simulation is an efficient and effective way to tackle the problem. History matching can help reveal some mechanisms existent in the cleanup process. The Fracturing, Acidizing, Stimulation Technology (FAST) Consortium at Colorado School of Mines previously developed a numerical model for investigating the hydraulic fracturing process, cleanup, and relevant physics. It is a three-dimensional, gas-water, coupled fracture propagation-fluid flow simulator, which has the capability to handle commonly present damage mechanisms. The overall goal of this research effort is to validate the model on real data and to investigate the dominant physics in well cleanup for the Cana Field, which produces from the Woodford Shale in Oklahoma. To achieve this goal, first the early time delayed gas production was explained and modeled, and a simulation framework was established that included all three relevant damage mechanisms for a slickwater fractured well. Next, a series of sensitivity analysis of well cleanup to major reservoir, fracture, and operational variables was conducted; five of the Cana wells' initial flowback data were history matched, specifically the first thirty days' gas and water producing rates. Reservoir matrix permeability, net pressure, Young's modulus, and formation pressure gradient were found to have an impact on the gas producing curve's shape, in different ways. Some moderately good matches were achieved, with the outcome of some unknown reservoir information being proposed using the corresponding inputs from the history matching study. It was also concluded that extended shut-in durations after fracturing all the stages do not delay production in the overall situation. The success of history matching will further knowledge of well cleanup characteristics in the Cana Field, enable the future usage of this tool in other hydraulically fractured gas wells, and help operators optimize the flowback operations. Future improvements can be achieved by further developing the current simulator so that it has the capability of optimizing its grids setting every time the user changes the inputs, which will result in better stability when the relative permeability setting is modified.

Single-run determination of polybrominated diphenyl ethers (PBDEs) di- to deca-brominated in fish meal, fish oil and fish feed by isotope dilution: application of automated sample purification and gas chromatography/ion trap tandem mass spectrometry (GC/ITMS).

PubMed

Blanco, Sonia Lucía; Vieites, Juan M

2010-07-05

The present paper describes the application of automated cleanup and fractionation procedures of the Power Prep system (Fluid Management Systems) for the determination of polybrominated diphenyl ethers (PBDEs) in feeding stuffs and fish meal and oil. Gas chromatography (GC) separation followed by ion trap tandem mass spectrometry detection in EI mode (ITMS) allowed the analysis of di- to deca-BDEs in the samples matrices used in fish aquaculture. The method developed enabled the determination of 26 native PBDE congeners and 11 (13)C(12)-labelled congeners, including deca-BDE 209, in a single-run analysis, using isotope dilution. The automated cleanup, consisting of a succession of multilayer silica and basic alumina columns previously applied by Wyrzykowska et al. (2009) [28] in combustion flue gas, was successfully applied in our complex matrices. The method allowed an increase in productivity, i.e. lower time was required to process samples, and simultaneous purification of several samples was achieved at a time, reducing analyst dedication and human error input. Average recoveries of 43-96% were obtained. GC/ITMS can overcome the complexity originating from the sample matrix, eliminating matrix effects by tandem MS, to enable the detection of congeners penta- to nona-BDEs where interferent masses were present. The provisional detection limits, estimated in the samples, were 5-30 pg for di-, tri-, tetra-, and penta-BDEs, 20-65 pg for hexa-, hepta-, octa- and nona-BDEs, and 105 pg for deca-BDE. Reduction of deca-BDE 209 blank values is of concern to ongoing research. Good accuracy was obtained by application of the whole procedure, representing an efficient, low-cost and fast alternative for routine analyses. Copyright 2010 Elsevier B.V. All rights reserved.

Determination of α- and β-boldenone sulfate, glucuronide and free forms, and androstadienedione in bovine urine using immunoaffinity columns clean-up and liquid chromatography tandem mass spectrometry analysis.

PubMed

Chiesa, Luca; Pavlovic, Radmila; Dusi, Guglielmo; Pasquale, Elisa; Casati, Alessio; Panseri, Sara; Arioli, Francesco

2015-01-01

The debate about the origins of boldenone in bovine urine is ongoing for two decades in Europe. Despite the fact that its use as a growth promoter has been banned in the European Union (EU) since 1981, its detection in bovine urine, in the form of α-boldenone conjugate, is considered fully compliant up to 2 ng mL(-1). The conjugated form of β-boldenone must be absent. In recent years, the literature about boldenone has focused on the identification of biomarkers that can indicate an illicit treatment. β-boldenone sulfate is a candidate molecule, even if the only studies currently available have taken place in small populations. In this study, a method for the determination of sulfate and glucuronate conjugates of β-boldenone was developed and validated according to the European Commission Decision 2002/657/EC and applied to α-boldenone sulfate and glucuronide, α- and β-boldenone free forms and androstadienedione (ADD), too. The clean-up with immunoaffinity columns enabled the direct determination of the conjugates and free forms and allowed specific and sensitive analyses of urine samples randomly selected to verify this method. The decision limits (CCα) ranged between 0.07 and 0.08 ng mL(-1), the detection capabilities (CCβ) between 0.08 and 0.1 ng mL(-1). Recovery was higher than 92% for all the analytes. Intra-day repeatability was between 5.8% and 17.2%, and inter-day repeatability was between 6.0% and 21.8% for the studied free and conjugated forms. This method has been developed as a powerful tool with the aim to study the origin of boldenone in a trial on a significant number of animals. Copyright © 2014 Elsevier B.V. All rights reserved.

Central Plateau Cleanup at DOE's Hanford Site - 12504

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

Dowell, Jonathan

The discussion of Hanford's Central Plateau includes significant work in and around the center of the Hanford Site - located about 7 miles from the Columbia River. The Central Plateau is the area to which operations will be shrunk in 2015 when River Corridor cleanup is complete. This work includes retrieval and disposal of buried waste from miles of trenches; the cleanup and closure of massive processing canyons; the clean-out and demolition to 'slab on grade' of the high-hazard Plutonium Finishing Plant; installation of key groundwater treatment facilities to contain and shrink plumes of contaminated groundwater; demolition of all othermore » unneeded facilities; and the completion of decisions about remaining Central Plateau waste sites. A stated goal of EM has been to shrink the footprint of active cleanup to less than 10 square miles by 2020. By the end of FY2011, Hanford will have reduced the active footprint of cleanup by 64 percent exceeding the goal of 49 percent. By 2015, Hanford will reduce the active footprint of cleanup by more than 90 percent. The remaining footprint reduction will occur between 2015 and 2020. The Central Plateau is a 75-square-mile region near the center of the Hanford Site including the area designated in the Hanford Comprehensive Land Use Plan Environmental Impact Statement (DOE 1999) and Record of Decision (64 FR 61615) as the Industrial-Exclusive Area, a rectangular area of about 20 square miles in the center of the Central Plateau. The Industrial-Exclusive Area contains the 200 East and 200 West Areas that have been used primarily for Hanford's nuclear fuel processing and waste management and disposal activities. The Central Plateau also encompasses the 200 Area CERCLA National Priorities List site. The Central Plateau has a large physical inventory of chemical processing and support facilities, tank systems, liquid and solid waste disposal and storage facilities, utility systems, administrative facilities, and groundwater monitoring wells. As a companion to the Hanford Site Cleanup Completion Framework document, DOE issued its draft Central Plateau Cleanup Completion Strategy in September 2009 to provide an outline of DOE's vision for completion of cleanup activities across the Central Plateau. As major elements of the Hanford cleanup along the Columbia River Corridor near completion, DOE believed it appropriate to articulate the agency vision for the remainder of the cleanup mission. The Central Plateau Cleanup Completion Strategy and the Hanford Site Cleanup Completion Framework were provided to the regulatory community, the Tribal Nations, political leaders, the public, and Hanford stakeholders to promote dialogue on Hanford's future. The Central Plateau Cleanup Completion Strategy describes DOE's vision for completion of Central Plateau cleanup and outlines the decisions needed to achieve the vision. The Central Plateau strategy involves steps to: (1) contain and remediate contaminated groundwater, (2) implement a geographic cleanup approach that guides remedy selection from a plateau-wide perspective, (3) evaluate and deploy viable treatment methods for deep vadose contamination to provide long-term protection of the groundwater, and (4) conduct essential waste management operations in coordination with cleanup actions. The strategy will also help optimize Central Plateau readiness to use funding when it is available upon completion of River Corridor cleanup projects. One aspect of the Central Plateau strategy is to put in place the process to identify the final footprint for permanent waste management and containment of residual contamination within the 20-square-mile Industrial-Exclusive Area. The final footprint identified for permanent waste management and containment of residual contamination should be as small as practical and remain under federal ownership and control for as long as a potential hazard exists. Outside the final footprint, the remainder of the Central Plateau will be available for other uses consistent with the Hanford Comprehensive Land-Use Plan (DOE 1999), while maintained under federal ownership and control. (author)« less

Laser intensity scaling through stimulated scattering in optical fibers

NASA Astrophysics Data System (ADS)

Russell, Timothy H.

The influence of stimulated scattering on laser intensity in fiber optic waveguides is examined. Stimulated Brillouin scattering (SBS) in long, multimode optical waveguides is found to generate a Stokes beam that propagates in the fiber LP01 mode. This characteristic of the Stokes beam was first applied to beam cleanup, where an aberrated pump generated a Gaussian-like Stokes beam. Additionally, the same process is found to combine multiple laser beams into a single spatially coherent source. The mean square difference between the two beams was used to measure the degree of spatial overlap, demonstrating spatial coherence between the Stokes beams even when the pump beams are not spatially correlated. This result is obtained regardless of whether the pump beams are at the same or different frequencies; producing two temporally coherent or incoherent Stokes beams respectively. Limitations in beam cleanup and combining are also examined to identify ways to overcome them. Output couplers are designed that could be used to spatially filter the Stokes beam from the pump, thus increasing the number of beams that could be combined. The combined power restriction induced by second order Stokes threshold is examined experimentally and theoretically and is not found to be a significant limitation. Finally, stimulated Raman scattering (SRS) beam cleanup is examined to overcome the stringent spectral requirements on the pump beams required by SBS. The last portion of the dissertation theoretically examines suppression of stimulated Raman scattering in fibers to eliminate the restriction this imposes on the power of a fiber laser or amplifier. The suppression was modeled using both a holmium dopant and adding a long period grating to the fiber. Both methods were shown to have a significant effect on the SRS threshold.

Non-cancer morbidity among Estonian Chernobyl cleanup workers: a register-based cohort study.

PubMed

Rahu, Kaja; Bromet, Evelyn J; Hakulinen, Timo; Auvinen, Anssi; Uusküla, Anneli; Rahu, Mati

2014-05-14

To examine non-cancer morbidity in the Estonian Chernobyl cleanup workers cohort compared with the population sample with special attention to radiation-related diseases and mental health disorders. Register-based cohort study. Estonia. An exposed cohort of 3680 men (cleanup workers) and an unexposed cohort of 7631 men (population sample) were followed from 2004 to 2012 through the Population Registry and Health Insurance Fund database. Morbidity in the exposed cohort compared with the unexposed controls was estimated in terms of rate ratio (RR) with 95% CIs using Poisson regression models. Elevated morbidity in the exposed cohort was found for diseases of the nervous system, digestive system, musculoskeletal system, ischaemic heart disease and for external causes. The most salient excess risk was observed for thyroid diseases (RR=1.69; 95% CI 1.38 to 2.07), intentional self-harm (RR=1.47; 95% CI 1.04 to 2.09) and selected alcohol-related diagnoses (RR=1.25; 95% CI 1.12 to 1.39). No increase in morbidity for stress reactions, depression, headaches or sleep disorders was detected. No obvious excess morbidity consistent with biological effects of radiation was seen in the exposed cohort, with the possible exception of benign thyroid diseases. Increased alcohol-induced morbidity may reflect alcohol abuse, and could underlie some of the higher morbidity rates. Mental disorders in the exposed cohort were probably under-reported. The future challenge will be to study mental and physical comorbidities in the Chernobyl cleanup workers cohort. Published by the BMJ Publishing Group Limited. For permission to use (where not already granted under a licence) please go to http://group.bmj.com/group/rights-licensing/permissions.

Multi-class analysis of new psychoactive substances and metabolites in hair by pressurized liquid extraction coupled to HPLC-HRMS.

PubMed

Montesano, Camilla; Vannutelli, Gabriele; Massa, Maristella; Simeoni, Maria Chiara; Gregori, Adolfo; Ripani, Luigi; Compagnone, Dario; Curini, Roberta; Sergi, Manuel

2017-05-01

In this paper, an analytical method has been developed and validated for the analysis of new psychoactive substances (NPS) and metabolites in hair samples. The method was based on pressurized liquid extraction (PLE) followed by solid-phase extraction (SPE) clean-up and high performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) analysis. To evaluate extraction efficiency and the applicability of the method, hair samples were fortified by soaking in order to obtain a good surrogate for drug users' hair; the amount of incorporated drugs related to their lipophilicity, similarly to in vivo drug incorporation. To the best of our knowledge, this is the first method that allowed for the analysis of both cathinones (5) and synthetic cannabinoids (7) in hair with a single extraction procedure and chromatographic run. A phenethylamine (2C-T-4), 4- fluorophenylpiperazine and methoxetamine were also included showing that PLE coupled to SPE clean-up was suitable for a multi-class analysis of NPS in hair. In addition, the use of PLE significantly reduced hair analysis time: decontamination, incubation, clean-up, and liquid chromatography-mass spectrometry (LC-MS) analysis were carried out in approximately 45 min. The method was fully validated according to Scientific Working Group for Forensic Toxicology (SWGTOX) and Society of Hair Testing (SoHT) guidelines. Limit of quantification (LOQ) values ranged from 8 to 50 pg mg -1 for cathinones, phenetylamines and piperazines, and from 9 to 40 pg mg -1 for synthetic cannabinoids (10 pg mg -1 for methoxetamine). Matrix effects were below 15% for all the analytes, demonstrating the effectiveness of the clean-up step. Inaccuracy was lower than 9% in terms of bias. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Tephra fall clean-up in urban environments

NASA Astrophysics Data System (ADS)

Hayes, Josh L.; Wilson, Thomas M.; Magill, Christina

2015-10-01

Tephra falls impact urban communities by disrupting transport systems, contaminating and damaging buildings and infrastructures, and are potentially hazardous to human health. Therefore, prompt and effective tephra clean-up measures are an essential component of an urban community's response to tephra fall. This paper reviews case studies of tephra clean-up operations in urban environments around the world, spanning 50 years. It identifies methods used in tephra clean-up and assesses a range of empirical relationships between level of tephra accumulation and clean-up metrics such as collected tephra volume, costs, and duration of operations. Results indicate the volume of tephra collected from urban areas is proportional to tephra accumulation. Urban areas with small tephra accumulations (1,000 m3/km2 or an average of 1 mm thickness) may collect < 1% of the total deposit, whereas urban areas which experience large accumulations (> 50,000 m3/km2 or an average of 50 mm thickness) remove up to 80%. This relationship can inform impact and risk assessments by providing an estimate of the likely response required for a given tephra fall. No strong relationship was found between tephra fall accumulation and clean-up cost or duration for urban environments which received one-off tephra falls, suggesting that these aspects of tephra fall clean-up operations are context specific. Importantly, this study highlights the advantage of effective planning for tephra clean-up and disposal in potentially exposed areas.

ENERGY CONSERVATION AND PRODUCTION AT WASTE CLEANUP SITES (ISSUE PAPER)

EPA Science Inventory

Saving energy used by hazardous waste cleanup remediation systems should interest those people working on waste cleanup sites. Presidential Executive Order 13123, "Greening the Government Through Efficient Energy Management", states that each agency shall strive to expand the us...

Oil persistence on beaches in Prince William Sound - a review of SCAT surveys conducted from 1989 to 2002.

PubMed

Taylor, Elliott; Reimer, Doug

2008-03-01

In 2002, 13 years after the Exxon Valdez oil spill (EVOS), 39 selected sites in Prince William Sound (PWS) were re-surveyed following established shoreline cleanup assessment team (SCAT) field observation procedures to document surface and sub-surface oiling conditions in shoreline sediments and to compare results with those from previous Shoreline Cleanup Assessment Team (SCAT) surveys and other surveys in PWS. The selected sites are locations where EVOS oil persisted in 1992, at the time the Federal and State On-Scene Coordinators determined that the cleanup was complete and that further cleanup activities would provide no net environmental benefit. These sites had been included in a 2001 NOAA survey of shoreline oiling conditions and account for 88% of the sub-surface oil residues (SSO) oil documented by that study. The 2002 field survey found isolated occurrences of residual EVOS surface oil residues (SO) in the form of weathered asphalt pavement at 15 of the 39 sites. This residual SO typically consisted of asphalt in mixed sand/gravel substrate, located within a wave shadow effect created by boulders or bedrock in the upper intertidal to supratidal zone. Residual SO, expressed as a continuous oil cover, was less than 200 m(2) within the approximately 111,120 m(2) surveyed. A total of 1182 pits were dug at locations where SSO residues were present in 1992. Six of the 39 sites and 815 (68%) of the pits contained no residual SSO. Eighty-three percent of pits with SSO residues were found primarily in middle to upper intertidal locations. SSO residues commonly occurred in a discontinuous approximately 3 cm thick band 5-10 cm below the boulder/cobble or pebble/gravel veneer. The SO and SSO occurrences in the 2002 survey closely match the locations where they were found in 1992 and earlier surveys; however, in 2002 residual SSO patches are more discontinuous and thinner than they were in the earlier surveys. These sites are biased toward SSO persistence; those that have SSO residues represent less than 0.5% of the originally oiled shorelines in PWS. Despite evidence of continued oil weathering, both at the surface and in the sub-surface, it is clear that the natural cleaning processes at these particular locations are slow. The slow weathering rates are a consequence of the oil residue being incorporated in finer sediments (fine sand, silt, mix) and isolated from active weathering processes as boulders and outcrops, shallow bedrock asperities, or boulder-armoring create wave shadows and limit effective physical action on shorelines.

Brownfields Grants Information

EPA Pesticide Factsheets

This asset includes all types of information regarding Brownfields grant programs that subsidize/support Brownfield cleanup. This includes EPA's Brownfields Program grant funding for brownfields assessment, cleanup, revolving loans, and environmental job training. Assessment grants provide funding for a grant recipient to inventory, characterize, assess, and conduct planning and community involvement related to brownfield sites. Revolving Loan Fund Grants enable States, political subdivisions, and Indian tribes to make low interest loans to carryout cleanup activities at brownfields properties. Cleanup grants provide funding for a grant recipient to carry out cleanup activities at brownfield sites. Environmental Workforce Development and Job Training Grants are designed to provide funding to eligible entities, including nonprofit organizations, to recruit, train, and place predominantly low-income and minority, unemployed and under-employed residents of solid and hazardous waste-impacted communities with the skills needed to secure full-time, sustainable employment in the environmental field and in the assessment and cleanup work taking place in their communities. Training, Research, and Technical Assistance Grants provide funding to eligible organizations to provide training, research, and technical assistance to facilitate brownfields cleanup. Regulatory authority for the collection and use of this information is found in the Small Business Liability Relief

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

Flynn, Karen; McCormick, Matt

Hanford's DOE offices are responsible for one of the largest nuclear cleanup efforts in the world, cleaning up the legacy of nearly five decades of nuclear weapons production. Nowhere in the DOE Complex is cleanup more challenging than at the Hanford Site in southeastern Washington. Hanford cleanup entails remediation of hundreds of large complex hazardous waste sites; disposition of nine production reactors and the preservation of one as a National Historic Landmark; demolition of hundreds of contaminated facilities including five enormous process canyons; remediation of billions of gallons of contaminated groundwater; disposition of millions of tons of low-level, mixed low-level,more » and transuranic waste; disposition of significant quantities of special nuclear material; storage and ultimate disposition of irradiated nuclear fuel; remediation of contamination deep in the soil that could impact groundwater; decontamination and decommissioning of hundreds of buildings and structures; and treatment of 56 million gallons of radioactive waste in 177 large underground tanks through the construction of a first-of-its-kind Waste Treatment Plant. Cleanup of the Hanford Site is a complex and challenging undertaking. The DOE Richland Operations Office has a vision and a strategy for completing Hanford's cleanup including the transition to post-cleanup activities. Information on the strategy is outlined in the Hanford Site Completion Framework. The framework describes three major components of cleanup - River Corridor, Central Plateau, and Tank Waste. It provides the context for individual cleanup actions by describing the key challenges and approaches for the decisions needed to complete cleanup. The U.S. Department of Energy (DOE), as regulated by the U.S. Environmental Protection Agency (EPA) and Washington State Department of Ecology (Ecology), is implementing a strategy to achieve final cleanup decisions for the River Corridor portion of the Hanford Site. The DOE Richland Operations Office (RL) and DOE Office of River Protection (ORP) have prepared this document to describe the strategy and to begin developing the approach for making cleanup decisions for the remainder of the Hanford Site. DOE's intent is that the Completion Framework document will facilitate dialogue among the Tri-Parties and with Hanford's diverse interest groups, including Tribal Nations, State of Oregon, Hanford Advisory Board, Natural Resource Trustees, and the public. Future cleanup decisions will be enhanced by an improved understanding of the challenges facing cleanup and a common understanding of the goals and approaches for cleanup completion. The overarching goals for cleanup are sevenfold. - Goal 1: Protect the Columbia River. - Goal 2: Restore groundwater to its beneficial use to protect human health, the environment, and the Columbia River. - Goal 3: Clean up River Corridor waste sites and facilities to: Protect groundwater and the Columbia River. Shrink the active cleanup footprint to the Central Plateau, and support anticipated future uses of the land. - Goal 4: Clean up Central Plateau waste sites, tank farms, and facilities to: Protect groundwater. Minimize the footprint of areas requiring long-term waste management activities. Support anticipated future uses of the land. - Goal 5: Safely manage and transfer legacy materials scheduled for off-site disposition including special nuclear material (including plutonium), spent nuclear fuel, transuranic waste, and immobilized high-level waste. - Goal 6: Consolidate waste treatment, storage, and disposal operations on the Central Plateau. - Goal 7: Develop and implement institutional controls and long-term stewardship activities that protect human health, the environment, and Hanford's unique cultural, historical and ecological resources after cleanup activities are completed. These goals embody more than 20 years of dialogue among the Tri-Party Agencies, Tribal Nations, State of Oregon, stakeholders, and the public. They carry forward key values captured in forums such as the Hanford Future Site Uses Working Group, Tank Waste Task Force, Hanford Summits, and Hanford Advisory Board Exposure Scenario Workshops, as well as more than 200 advice letters issued by the Hanford Advisory Board (http://www.hanford.gov/page.cfm/hab). These goals help guide all aspects of Hanford Site cleanup. Cleanup activities at various areas of the site support the achievement of one or more of these goals. These goals help set priorities to apply resources and sequence cleanup efforts for the greatest benefit. These goals reflect DOE's recognition that the Columbia River is a critical resource for the people and ecology of the Pacific Northwest. The 50-mile stretch of the river known as the Hanford Reach is home to the last free-flowing section of the river in the U.S. As one of the largest rivers in North America, its waters support a multitude of uses that are vital to the economic and environmental well being of the region and it is particularly important in sustaining the culture of Native Americans. Cleanup actions must protect this river. (authors)« less

Optimization of sample preparation by central composite design for multi-class determination of veterinary drugs in bovine muscle, kidney and liver by ultra-high-performance liquid chromatographic-tandem mass spectrometry.

PubMed

Rizzetti, Tiele M; de Souza, Maiara P; Prestes, Osmar D; Adaime, Martha B; Zanella, Renato

2018-04-25

In this study a simple and fast multi-class method for the determination of veterinary drugs in bovine liver, kidney and muscle was developed. The method employed acetonitrile for extraction followed by clean-up with EMR-Lipid® sorbent and trichloracetic acid. Tests indicated that the use of TCA was most effective when added in the final step of the clean-up procedure instead of during extraction. Different sorbents were tested and optimized using central composite design and the analytes determined by ultra-high-performance liquid chromatographic-tandem mass spectrometry (UHPLC-MS/MS). The method was validated according the European Commission Decision 2002/657 presenting satisfactory results for 69 veterinary drugs in bovine liver and 68 compounds in bovine muscle and kidney. The method was applied in real samples and in proficiency tests and proved to be adequate for routine analysis. Residues of abamectin, doramectin, eprinomectin and ivermectin were found in samples of bovine muscle and only ivermectin in bovine liver. Copyright © 2017 Elsevier Ltd. All rights reserved.

Hazardous Waste: Cleanup and Prevention.

ERIC Educational Resources Information Center

Vandas, Steve; Cronin, Nancy L.

1996-01-01

Discusses hazardous waste, waste disposal, unsafe exposure, movement of hazardous waste, and the Superfund clean-up process that consists of site discovery, site assessment, clean-up method selection, site clean up, and site maintenance. Argues that proper disposal of hazardous waste is everybody's responsibility. (JRH)

HANDBOOK ON THE BENEFITS, COSTS, AND IMPACTS OF LAND CLEANUP AND REUSE

EPA Science Inventory

Summarizes the theoretical and empirical literature addressing benefit-cost and impact assessment of the land cleanup and reuse scenario. When possible, recommendations are provided for conducting economic analysis of land cleanup and reuse sites and programs. The knowledge base ...

Analysis of state Superfund programs: 50 state study. 1998 update

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

NONE

States have remediated over 40,000 contaminated sites not on the federal Superfund list. ELI`s latest analysis of state Superfund programs examines the cleanup programs of all 50 states, Puerto Rico, and the District of Columbia. The study provides the most current data on state statutes, program organization, staffing, funding, expenditures, cleanup standards, and cleanup activities, voluntary cleanup programs and brownfields programs. State and federal policymakers and attorneys working on non-NPL sites should find this study useful.

Determination of acrylamide and acrylic acid by isocratic liquid chromatography with pulsed electrochemical detection.

PubMed

Casella, Innocenzo G; Pierri, Marianna; Contursi, Michela

2006-02-24

The electrochemical behaviour of the polycrystalline platinum electrode towards the oxidation/reduction of short-chain unsaturated aliphatic molecules such as acrylamide and acrylic acid was investigated in acidic solutions. Analytes were separated by reverse phase liquid chromatographic and quantified using a pulsed amperometric detection. A new two-step waveform, is introduced for detection of acrylamide and acrylic acid. Detection limits (LOD) of 20 nM (1. 4 microg/kg) and 45 nM (3.2 microg/kg) were determined in water solutions containing acrylamide and acrylic acid, respectively. Compared to the classical three-step waveform, the proposed two-step waveform shows favourable analytical performance in terms of LOD, linear range, precision and improved long-term reproducibility. The proposed analytical method combined with clean-up procedure accomplished by Carrez clearing reagent and subsequent extraction with a strong cation exchanger cartridges (SPE), was successfully used for the quantification of low concentrations of acrylamide in foodstuffs such as coffee and potato fries.

Rapid preconcentration method for the determination of azadirachtin-A and -B, nimbin and salannin in neem oil samples by using graphitised carbon solid phase extraction.

PubMed

Ramesh, A; Balasubramanian, M

1999-01-01

A simple and rapid method involving solid phase extraction and liquid chromatography for the determination of azadirachtin-A and -B, nimbin and salannin at nanogram levels in neem oil samples is presented. The neem oil samples are defatted and the compounds of interest extracted by mixing the sample with hexane and passing the hexane solution through a graphitised carbon black column. After washing the column with 2 ml of hexane, azadirachtin-A and -B, nimbin and salannin are eluted with 5 ml of acetonitrile and quantified using HPLC with UV detection. The recoveries of azadirachtin-A and -B, nimbin and salannin in fortified oil samples were 97.4-104.7%. The upper limit of quantification is up to 100 micrograms ml-1 without any additional clean-up and with little interference from lipids during the analysis by HPLC. The method was successfully applied to various neem oil samples collected from different locations in India.

Analysis of Trace Quaternary Ammonium Compounds (QACs) in Vegetables Using Ultrasonic-Assisted Extraction and Gas Chromatography-Mass Spectrometry.

PubMed

Xiang, Lei; Wang, Xiong-Ke; Li, Yan-Wen; Huang, Xian-Pei; Wu, Xiao-Lian; Zhao, Hai-Ming; Li, Hui; Cai, Quan-Ying; Mo, Ce-Hui

2015-08-05

A reliable, sensitive, and cost-effective method was developed for determining three quaternary ammonium compounds (QACs) including dodecyltrimethylammonium chloride, cetyltrimethylammonium chloride, and didodecyldimethylammonium chloride in various vegetables using ultrasonic-assisted extraction and gas chromatography-mass spectrometry. The variety and acidity of extraction solvents, extraction times, and cleanup efficiency of sorbents were estimated to obtain an optimized procedure for extraction of the QACs in nine vegetable matrices. Excellent linearities (R(2) > 0.992) were obtained for the analytes in the nine matrices. The limits of detection and quantitation were 0.7-6.0 and 2.3-20.0 μg/kg (dry weight, dw) in various matrices, respectively. The recoveries in the nine matrices ranged from 70.5% to 108.0% with relative standard deviations below 18.0%. The developed method was applied to determine the QACs in 27 vegetable samples collected from Guangzhou in southern China, showing very high detection frequency with a concentration of 23-180 μg/kg (dw).

Determination of tilmicosin residues in chicken, cattle, swine, and sheep tissues by liquid chromatography.

PubMed

Stobba-Wiley, C M; Chang, J P; Elsbury, D T; Moran, J W; Turner, J M; Readnour, R S; Stobba-Wiley, C M; Chang, J P; Elsbury, D T; Moran, J W; Turner, J M; Readnour, R S

2000-01-01

A method was developed and validated for determination and quantitation of tilmicosin residues in swine, cattle, and sheep edible tissues, as well as chicken fat, skin, and muscle over a concentration range of 0.025 microg/g-20 microg/g. For chicken kidney and liver, the method was validated over a range of 0.060 microg/g-20 microg/g. The tissue sample was extracted with methanol and a C18 cartridge was used for solid-phase extraction cleanup. A reversed-phase gradient liquid chromatographic method with detection at 280 nm was used to separate the tilmicosin from matrix components in 30 min run time. The limit of quantitation (LOQ) of the method was 0.025 microg/g for all tested tissues except chicken kidney and liver, for which the LOQ was 0.06 microg/g. Average recoveries for tissue samples ranged from 73 to 98%. Relative standard deviation values ranged from 0.6 to 14.7%.

Selective pressurized liquid extraction of pesticides, polychlorinated biphenyls and polybrominated diphenyl ethers in a whale earplug (earwax): a novel method for analyzing organic contaminants in lipid-rich matrices.

PubMed

Robinson, Eleanor M; Trumble, Stephen J; Subedi, Bikram; Sanders, Rebel; Usenko, Sascha

2013-12-06

Lipid-rich matrices are often sinks for lipophilic contaminants, such as pesticides, polychlorinated biphenyls (PCBs), and polybrominated diphenyl ethers (PBDEs). Typically methods for contaminant extraction and cleanup for lipid-rich matrices require multiple cleanup steps; however, a selective pressurized liquid extraction (SPLE) technique requiring no additional cleanup has been developed for the simultaneous extraction and cleanup of whale earwax (cerumen; a lipid-rich matrix). Whale earwax accumulates in select whale species over their lifetime to form wax earplugs. Typically used as an aging technique in cetaceans, layers or laminae that comprise the earplug are thought to be associated with annual or semiannual migration and feeding patterns. Whale earplugs (earwax) represent a unique matrix capable of recording and archiving whales' lifetime contaminant profiles. This study reports the first analytical method developed for identifying and quantifying lipophilic persistent organic pollutants (POPs) in a whale earplug including organochlorine pesticides, polychlorinated biphenyls (PCBs), and polybrominated diphenyl ethers (PBDEs). The analytical method was developed using SPLE to extract contaminants from ∼0.25 to 0.5g aliquots of each lamina of sectioned earplug. The SPLE was optimized for cleanup adsorbents (basic alumina, silica gel, and Florisil(®)), adsorbent to sample ratio, and adsorbent order. In the optimized SPLE method, the earwax homogenate was placed within the extraction cell on top of basic alumina (5g), silica gel (15g), and Florisil(®) (10g) and the target analytes were extracted from the homogenate using 1:1 (v/v) dichloromethane:hexane. POPs were analyzed using gas chromatography-mass spectrometry with electron capture negative ionization and electron impact ionization. The average percent recoveries for the POPs were 91% (±6% relative standard deviation), while limits of detection and quantification ranged from 0.00057 to 0.96ngg(-1) and 0.0017 to 2.9ngg(-1), respectively. Pesticides, PCBs, and PBDEs, were measured in a single blue whale (Balaenoptera musculus) cerumen lamina at concentrations ranging from 0.11 to 150ng g(-1). Copyright © 2013 Elsevier B.V. All rights reserved.

Evaluation of surface roughness of enamel after various bonding and clean-up procedures on enamel bonded with three different bonding agents: An in-vitro study

PubMed Central

Goel, Amit; Singh, Atul; Gupta, Tarun

2017-01-01

Background The purpose of this study was to analyze and compare the enamel surface roughness before bonding and after debonding, to find correlation between the adhesive remnant index and its effect on enamel surface roughness and to evaluate which clean-up method is most efficient to provide a smoother enamel surface. Material and Methods 135 premolars were divided into 3 groups containing 45 premolars in each group. Group I was bonded by using moisture insensitive primer, Group II by using conventional orthodontic adhesive and Group III by using self-etching primer. Each group was divided into 3 sub-groups on the basis of type of clean-up method applied i,e scaling followed by polishing, tungsten carbide bur and Sof-Lex disc. Enamel surface roughness was measured and compared before bonding and after clean-up. Results Evaluation of pre bonding and post clean-up enamel surface roughness (Ra value) with the t test showed that Post clean-up Ra values were greater than Pre bonding Ra values in all the groups except in teeth bonded with self-etching primer cleaned with Sof-Lex disc. Reliability of ARI score taken at different time interval tested with Kruskal Wallis test suggested that all the readings were reliable. Conclusions No clean-up procedure was able to restore the enamel to its original smoothness. Self-etching primer and Sof-Lex disc clean-up method combination restored the enamel surface roughness (Ra value) closest to its pre-treatment value. Key words:Enamel surface roughness, clean-up method, adhesive remnant index. PMID:28512535

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. Copyright © 2012 Elsevier Ltd. All rights reserved.

DEMONSTRATION BULLETIN: CIRCULATING BED COMBUSTOR - OGDEN ENVIRONMENTAL SERVICES, INC.

EPA Science Inventory

An evaluation of the Ogden Environmental Services (OES) circulating bed combustor (CBC) technology was carried out under the superfund Innovative Technology Evaluation (SITE) Program to determine its applicabilitY as an on-site treatment method for waste site cleanups, and more s...

Multiresidue analysis of endocrine-disrupting compounds and perfluorinated sulfates and carboxylic acids in sediments by ultra-high-performance liquid chromatography-tandem mass spectrometry.

PubMed

Cavaliere, Chiara; Capriotti, Anna Laura; Ferraris, Francesca; Foglia, Patrizia; Samperi, Roberto; Ventura, Salvatore; Laganà, Aldo

2016-03-18

A multiresidue analytical method for the determination of 11 perfluorinated compounds and 22 endocrine-disrupting compounds (ECDs) including 13 natural and synthetic estrogens (free and conjugated forms), 2 alkylphenols, 1 plasticiser, 2 UV-filters, 1 antimicrobial, and 2 organophosphorus compounds in sediments has been developed. Ultrasound-assisted extraction followed by solid phase extraction (SPE) with graphitized carbon black (GCB) cartridge as clean-up step were used. The extraction process yield was optimized in terms of solvent composition. Then, a 3(2) experimental design was used to optimize solvent volume and sonication time by response surface methodology, which simplifies the optimization procedure. The final extract was analyzed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry. The optimized sample preparation method is simple and robust, and allows recovery of ECDs belonging to different classes in a complex matrix such as sediment. The use of GCB for SPE allowed to obtain with a single clean-up procedure excellent recoveries ranging between 75 and 110% (relative standard deviation <16%). The developed methodology has been successfully applied to the analysis of ECDs in sediments from different rivers and lakes of the Lazio Region (Italy). These analyses have shown the ubiquitous presence of chloro-substituted organophosphorus flame retardants and bisphenol A, while other analyzed compounds were occasionally found at concentration between the limit of detection and quantification. Copyright © 2016 Elsevier B.V. All rights reserved.

[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.

Evaluation of the performance of statistical tests used in making cleanup decisions at Superfund sites. Part 1: Choosing an appropriate statistical test

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

Berman, D.W.; Allen, B.C.; Van Landingham, C.B.

1998-12-31

The decision rules commonly employed to determine the need for cleanup are evaluated both to identify conditions under which they lead to erroneous conclusions and to quantify the rate that such errors occur. Their performance is also compared with that of other applicable decision rules. The authors based the evaluation of decision rules on simulations. Results are presented as power curves. These curves demonstrate that the degree of statistical control achieved is independent of the form of the null hypothesis. The loss of statistical control that occurs when a decision rule is applied to a data set that does notmore » satisfy the rule`s validity criteria is also clearly demonstrated. Some of the rules evaluated do not offer the formal statistical control that is an inherent design feature of other rules. Nevertheless, results indicate that such informal decision rules may provide superior overall control of error rates, when their application is restricted to data exhibiting particular characteristics. The results reported here are limited to decision rules applied to uncensored and lognormally distributed data. To optimize decision rules, it is necessary to evaluate their behavior when applied to data exhibiting a range of characteristics that bracket those common to field data. The performance of decision rules applied to data sets exhibiting a broader range of characteristics is reported in the second paper of this study.« less

Novel method for the rapid and specific extraction of multiple β2 -agonist residues in food by tailor-made Monolith-MIPs extraction disks and detection by gas chromatography with mass spectrometry.

PubMed

Liu, Haibo; Gan, Ning; Chen, Yinji; Ding, Qingqing; Huang, Jie; Lin, Saichai; Cao, Yuting; Li, Tianhua

2016-09-01

A quick and specific pretreatment method based on a series of extraction clean-up disks, consisting of molecularly imprinted polymer monoliths and C18 adsorbent, was developed for the specific enrichment of salbutamol and clenbuterol residues in food. The molecularly imprinted monolithic polymer disk was synthesized using salbutamol as a template through a one-step synthesis process. It can simultaneously and specifically recognize salbutamol and clenbuterol. The monolithic polymer disk and series of C18 disks were assembled with a syringe to form a set of tailor-made devices for the extraction of target molecules. In a single run, salbutamol and clenbuterol can be specifically extracted, cleaned, and eluted by methanol/acetic acid/H2 O. The target molecules, after a silylation derivatization reaction were detected by gas chromatography-mass spectrometry. The parameters including solvent desorption, sample pH, and the cycles of reloading were investigated and discussed. Under the optimized extraction and clean-up conditions, the limits of detection and quantitation were determined as 0.018-0.022 and 0.042-0.049 ng/g for salbutamol and clenbuterol, respectively. The assay described was convenient, rapid, and specific; thereby potentially efficient in the high-throughput analysis of β2 -agonists residues in real food samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High Throughput Determination of Ricinine Abrine and Alpha ...

EPA Pesticide Factsheets

Analytical Method This document provides the standard operating procedure for determination of ricinine (RIC), abrine (ABR), and α-amanitin (AMAN) in drinking water by isotope dilution liquid chromatography tandem mass spectrometry (LC/MS/MS). This method is designed to support site-specific cleanup goals of environmental remediation activities following a homeland security incident involving one or a combination of these analytes.

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

PubMed

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

2002-05-01

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

Review of State Soil Cleanup Levels for Dioxin (December 2009)

EPA Science Inventory

This final report summarizes a survey of state soil cleanup levels for dioxin and characterizes the science underlying these values. The objective of this project was to summarize existing state cleanup levels for dioxin in soil, together with their scientific bases where availa...

40 CFR 312.25 - Searches for recorded environmental cleanup liens.

Code of Federal Regulations, 2010 CFR

2010-07-01

... cleanup liens. 312.25 Section 312.25 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) SUPERFUND, EMERGENCY PLANNING, AND COMMUNITY RIGHT-TO-KNOW PROGRAMS INNOCENT LANDOWNERS, STANDARDS FOR... cleanup liens. (a) All appropriate inquiries must include a search for the existence of environmental...

Successful implementation of property cleanup under the Ohio and the Texas voluntary programs

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

Roffman, A.

1999-07-01

Cleanups of two properties, one located in Ohio and the other in Texas were successfully implemented. The facilities were printing plants that manufactured printed material and forms for commercial and industrial use. Primary products and chemicals involved in the manufacturing of the forms included ink, petroleum products and cleaning solvents. The Ohio property underwent a successful cleanup under the Ohio EPA Voluntary Action Program (VAP). It met the Ohio EPA residential land use cleanup standards for soil and shallow groundwater. A No Further Action letter has been submitted to the state and it resulted in the issuance of a Covenantmore » Not to Sue. The Texas facility underwent a successful cleanup under the Texas Natural Resource Conservation Commission (TNRCC) Voluntary Cleanup Program (VCP). It resulted in the issuance of a Certificate of Completion (COC) for residential land use for soil, and a conditional COC for industrial land use for the shallow groundwater.« less

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

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

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 ismore » 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.« less

Determination of the clean-up efficiency of the solid-phase extraction of rosemary extracts: Application of full-factorial design in hyphenation with Gaussian peak fit function.

PubMed

Meischl, Florian; Kirchler, Christian Günter; Jäger, Michael Andreas; Huck, Christian Wolfgang; Rainer, Matthias

2018-02-01

We present a novel method for the quantitative determination of the clean-up efficiency to provide a calculated parameter for peak purity through iterative fitting in conjunction with design of experiments. Rosemary extracts were used and analyzed before and after solid-phase extraction using a self-fabricated mixed-mode sorbent based on poly(N-vinylimidazole/ethylene glycol dimethacrylate). Optimization was performed by variation of washing steps using a full three-level factorial design and response surface methodology. Separation efficiency of rosmarinic acid from interfering compounds was calculated using an iterative fit of Gaussian-like signals and quantifications were performed by the separate integration of the two interfering peak areas. Results and recoveries were analyzed using Design-Expert® software and revealed significant differences between the washing steps. Optimized parameters were considered and used for all further experiments. Furthermore, the solid-phase extraction procedure was tested and compared with commercial available sorbents. In contrast to generic protocols of the manufacturers, the optimized procedure showed excellent recoveries and clean-up rates for the polymer with ion exchange properties. Finally, rosemary extracts from different manufacturing areas and application types were studied to verify the developed method for its applicability. The cleaned-up extracts were analyzed by liquid chromatography with tandem mass spectrometry for detailed compound evaluation to exclude any interference from coeluting molecules. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Factors affecting cleanup of exhaust gases from a pressurized, fluidized-bed coal combustor

NASA Technical Reports Server (NTRS)

Rollbuhler, R. J.; Kobak, J. A.

1980-01-01

The cleanup of effluent gases from the fluidized-bed combustion of coal is examined. Testing conditions include the type and feed rate of the coal and the sulfur sorbent, the coal-sorbent ratio, the coal-combustion air ratio, the depth of the reactor fluidizing bed, and the technique used to physically remove fly ash from the reactor effluent gases. Tests reveal that the particulate loading matter in the effluent gases is a function not only of the reactor-bed surface gas velocity, but also of the type of coal being burnt and the time the bed is operating. At least 95 percent of the fly ash particules in the effluent gas are removed by using a gas-solids separator under controlled operating conditions. Gaseous pollutants in the effluent (nitrogen and sulfur oxides) are held within the proposed Federal limits by controlling the reactor operating conditions and the type and quantity of sorbent material.

48 CFR 49.105-4 - Cleanup of construction site.

Code of Federal Regulations, 2010 CFR

2010-10-01

... 48 Federal Acquisition Regulations System 1 2010-10-01 2010-10-01 false Cleanup of construction site. 49.105-4 Section 49.105-4 Federal Acquisition Regulations System FEDERAL ACQUISITION REGULATION CONTRACT MANAGEMENT TERMINATION OF CONTRACTS General Principles 49.105-4 Cleanup of construction site. In...

Relative bioavailability of arsenic contaminated soils in a mouse model

EPA Science Inventory

Exposure to As contaminated soils compels extensive soil cleanups so that human health risks are minimized. In order to improve exposure estimates and potentially reduce remediation costs, determination of the bioavailability of As in soils is needed. The objective of this study ...

Brownfields Assessing Contractor Capabilities for Streamlined Site Investigation: Additional Information Regarding All Appropriate Inquiries and Hiring an Environmental Professional

EPA Pesticide Factsheets

This document assists Brownfields grantees and other decision makers as they assess the capabilities of contractors and consultants to determine their qualifications to provide streamlined and innovative strategies for the assessment and and cleanup.

Analysis of imazaquin in soybeans by solid-phase extraction and high-performance liquid chromatography.

PubMed

Guo, C; Hu, J-Y; Chen, X-Y; Li, J-Z

2008-02-01

An analytical method for the determination imazaquin residues in soybeans was developed. The developed liquid/liquid partition and strong anion exchange solid-phase extraction procedures provide the effective cleanup, removing the greatest number of sample matrix interferences. By optimizing mobile-phase pH water/acetonitrile conditions with phosphoric acid, using a C-18 reverse-phase chromatographic column and employing ultraviolet detection, excellent peak resolution was achieved. The combined cleanup and chromatographic method steps reported herein were sensitive and reliable for determining the imazaquin residues in soybean samples. This method is characterized by recovery >88.4%, precision <6.7% CV, and sensitivity of 0.005 ppm, in agreement with directives for method validation in residue analysis. Imazaquin residues in soybeans were further confirmed by high performance liquid chromatography-mass spectrometry (LC-MS). The proposed method was successfully applied to the analysis of imazaquin residues in soybean samples grown in an experimental field after treatments of imazaquin formulation.

30 CFR 75.400-2 - Cleanup program.

Code of Federal Regulations, 2012 CFR

2012-07-01

... 30 Mineral Resources 1 2012-07-01 2012-07-01 false Cleanup program. 75.400-2 Section 75.400-2 Mineral Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR COAL MINE SAFETY AND HEALTH MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Combustible Materials and Rock Dusting § 75.400-2 Cleanup...

30 CFR 75.400-2 - Cleanup program.

Code of Federal Regulations, 2011 CFR

2011-07-01

... 30 Mineral Resources 1 2011-07-01 2011-07-01 false Cleanup program. 75.400-2 Section 75.400-2 Mineral Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR COAL MINE SAFETY AND HEALTH MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Combustible Materials and Rock Dusting § 75.400-2 Cleanup...

30 CFR 75.400-2 - Cleanup program.

Code of Federal Regulations, 2013 CFR

2013-07-01

... 30 Mineral Resources 1 2013-07-01 2013-07-01 false Cleanup program. 75.400-2 Section 75.400-2 Mineral Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR COAL MINE SAFETY AND HEALTH MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Combustible Materials and Rock Dusting § 75.400-2 Cleanup...

30 CFR 75.400-2 - Cleanup program.

Code of Federal Regulations, 2014 CFR

2014-07-01

... 30 Mineral Resources 1 2014-07-01 2014-07-01 false Cleanup program. 75.400-2 Section 75.400-2 Mineral Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR COAL MINE SAFETY AND HEALTH MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Combustible Materials and Rock Dusting § 75.400-2 Cleanup...

30 CFR 75.400-2 - Cleanup program.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Cleanup program. 75.400-2 Section 75.400-2 Mineral Resources MINE SAFETY AND HEALTH ADMINISTRATION, DEPARTMENT OF LABOR COAL MINE SAFETY AND HEALTH MANDATORY SAFETY STANDARDS-UNDERGROUND COAL MINES Combustible Materials and Rock Dusting § 75.400-2 Cleanup...

A comprehensive study of Superfund program benefits in the Denver and Tampa Bay metropolitan areas

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

Held, K.; Casper, B.; Siddhanti, S.K.

1995-12-31

The purpose of the study is to evaluate the benefits of the Superfund program in selected geographic areas. The study demonstrates how the cleanup of Superfund sites has improved the overall quality of life of those in the affected communities. The study presents findings on the benefits of Superfund cleanup activity in the Denver, Colorado and Tampa Bay, Florida metropolitan areas. Denver and Tampa Bay were chosen from several areas that the EPA evaluated and screened during the initial phase of the study. These locations were chosen because of a substantial presence of Superfund activities, making it possible to assessmore » the efficacy of the program. Several features make this study unique in terms of its overall goal. The study examines a broad range of benefit categories related to human health, environmental, and socioeconomic effects of Superfund cleanup activities. The study is also designed to assess benefits due to completed, current, and future planned activity at Superfund sites. This assessment covers Federal remedial activities at National Priorities List (NPL) sites, as well as relevant Federal removal actions in the study areas. These benefits are investigated from an area-wide perspective, as opposed to site-by-site, to determine Superfund`s overall effect on the communities in each area. The study consists of two major phases: Phase 1: Screening and ranking 16 prospective geographic areas and selecting Denver and Tampa Bay as the most appropriate areas for in-depth analysis; and Phase 2: Developing methodologies for assessing benefits, collecting relevant data, and analyzing the benefits from Superfund cleanup activity.« less

Immunoaffinity column cleanup with liquid chromatography using post-column bromination for determination of aflatoxins in peanut butter, pistachio paste, fig paste, and paprika powder: collaborative study.

PubMed

Stroka, J; Anklam, E; Jörissen, U; Gilbert, J

2000-01-01

A collaborative study was conducted to evaluate the effectiveness of an immunoaffinity column cleanup liquid chromatography (LC) method for the determination of aflatoxin B1 and total aflatoxins at European regulatory limits. The test portion is extracted with methanol-water (8 + 2) for dried figs and paprika, and with methanol-water (8 + 2) plus hexane (or cyclohexane) for peanut butter and pistachios. The sample extract is filtered, diluted with phosphate buffer saline, and applied to an immunoaffinity column. The column is washed with water and the aflatoxins are eluted with methanol. Aflatoxins are quantitated by reversed-phase LC with post-column derivatization (PCD) involving bromination. PCD is achieved with either an electrochemical cell (Kobra cell) and addition of bromide to the mobile phase or pyridinium hydrobromide perbromide. Determination is by fluorescence. Peanut butter, pistachio paste, dried fig paste, and paprika powder samples, both naturally contaminated with aflatoxins and containing added aflatoxins, were sent to 16 collaborators in 16 European countries. Test portions of samples were spiked at levels of 2.4 and 9.6 ng/g for total aflatoxins which included 1.0 and 4.0 ng/g aflatoxin B1, respectively. Recoveries for total aflatoxins ranged from 71 to 92% with corresponding recoveries for aflatoxin B1 of 82 to 109%. Based on results for spiked samples (blind duplicates at 2 levels) as well as naturally contaminated samples (blind duplicates at 4 levels, including blank), the relative standard deviation for repeatability ranged from 4.6 to 23.3% for total aflatoxins and from 3.1 to 20.0% for aflatoxin B1. The relative standard deviation for reproducibility ranged from 14.1 to 34.2% for total aflatoxins, and from 9.1 to 32.2% for aflatoxin B1. The method showed acceptable within-laboratory and between-laboratory precision for all 4 matrixes, as evidenced by HORRAT values <1, at the low levels of determination for both total aflatoxins and aflatoxin B1.

High-performance liquid chromatographic determination of methotrexate, 7-hydroxymethotrexate, 5-methyltetrahydrofolic acid and folinic acid in serum and cerebrospinal fluid.

PubMed

Belz, S; Frickel, C; Wolfrom, C; Nau, H; Henze, G

1994-11-04

A method for the simultaneous determination of the antifolates methotrexate and 7-hydroxymethotrexate as well as the folates 5-methyltetrahydrofolic acid and folinic acid (5-formyltetrahydrofolic acid) in serum and cerebrospinal fluid (CSF) is described. High-performance liquid chromatography with gradient elution and dual detection (ultraviolet absorption and fluorescence) was used to separate and quantitate the analytes. Serum samples containing high levels of the substances of interest and CSF samples were injected directly onto the HPLC column. For determination of low concentrations, serum samples were subjected to a solid-phase extraction method for clean-up and concentration purposes. The determination limits were 10 ng/ml for both antifolates, 100 ng/ml for folinic acid, and 0.1 ng/ml for the physiologically occurring methylated folate which is about 1/100 the serum concentration in healthy children. The suitability of the method for pharmacokinetic monitoring of high-dose methotrexate therapy combined with leucovorin rescue administered to children with acute lymphoblastic leukemia was demonstrated. Minimum values of the serum folate during treatment ranged from 0.2 to 3.1 ng/ml. Even those very low concentrations could be reliably measured.

Quantitative analysis of three chiral pesticide enantiomers by high-performance column liquid chromatography.

PubMed

Wang, Peng; Liu, Donghui; Gu, Xu; Jiang, Shuren; Zhou, Zhiqiang

2008-01-01

Methods for the enantiomeric quantitative determination of 3 chiral pesticides, paclobutrazol, myclobutanil, and uniconazole, and their residues in soil and water are reported. An effective chiral high-performance liquid chromatographic (HPLC)-UV method using an amylose-tris(3,5-dimethylphenylcarbamate; AD) column was developed for resolving the enantiomers and quantitative determination. The enantiomers were identified by a circular dichroism detector. Validation involved complete resolution of each of the 2 enantiomers, plus determination of linearity, precision, and limit of detection (LOD). The pesticide enantiomers were isolated by solvent extraction from soil and C18 solid-phase extraction from water. The 2 enantiomers of the 3 pesticides could be completely separated on the AD column using n-hexane isopropanol mobile phase. The linearity and precision results indicated that the method was reliable for the quantitative analysis of the enantiomers. LODs were 0.025, 0.05, and 0.05 mg/kg for each enantiomer of paclobutrazol, myclobutanil, and uniconazole, respectively. Recovery and precision data showed that the pretreatment procedures were satisfactory for enantiomer extraction and cleanup. This method can be used for optical purity determination of technical material and analysis of environmental residues.

Building Toxic Metal Characterization and Decontamination Report: Area 6, Building 914

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

NSTec Industrial Hygiene

2011-08-15

The purpose of this report is to outline the toxic metal characterization and decontamination efforts in Area 6, Building 914. This includes the initial building inspection, the hotspot sampling, results/findings, building cleanup, and the verification sampling. Building 914 is a steel light frame building that was constructed in 1992. It is about 16,454 square feet, and five employees are assigned to this building. According to the building's floor plan blueprints, it could be inferred that this building was once a Wiremen/Lineman shop. In 2002-2004, the National Nuclear Security Administration Nevada Site Office embarked on a broad characterization of beryllium (Be)more » surface concentrations throughout the North Las Vegas Facility, the Nevada National Security Site (NNSS), and ancillary facilities like the Special Technologies Laboratory, Remote Sensing Laboratory, etc. Building 914 was part of this characterization. The results of the 2002 study illustrated that the metal housekeeping limits were within acceptable limits and from a Be standpoint, the building was determined to be fit for occupancy. On March 2, 2011, based on a request from Building 914 users, National Security Technologies, LLC (NSTec) Industrial Hygiene (IH) collected bulk samples from the southwest corner of Building 914 at heights above 6 feet where black dust had been noticed on this particular wall. IH conducted surface swipe sampling of the area and analyzed the samples for toxic metals, namely, beryllium (Be), cadmium (Cd), chromium (Cr), lead (Pb), and manganese (Mn). The sample results indicated values two to four times above the housekeeping threshold for Be, Cd, Cr, Pb, and Mn. Subsequently, the facility was closed and posted; the necessary personnel were notified; and controls were instituted for ingress and egress of the building. On March 17, 2011, IH performed an extensive sampling event involving the entire warehouse in accordance with NSTec Organization Procedure OP-P250.004, Sampling Procedures. Analysis of the results from this exercise illustrated that toxic metal contamination was ubiquitous throughout the warehouse section of this building but did not extend into the office, restroom, and break room areas. On March 22, 2011, a planning meeting was held with Environment, Safety, Health & Quality management; Operations & Infrastructure (O&I) mangement; Facility Management; Occupational Medicine; O&I Operations; and IH. After a brief discussion concerning the salient facts of the surface sample results, it was agreed that the facility and its contents required cleaning. The facility would then be re-sampled to verify cleanliness and suitability for re-occupancy. On April 18, 2011, warehouse cleanup activites began. On July 5, 2011, upon receipt of the results from the last cleaned section, the cleanup operations were concluded. The building was statistically determined to be clean; thus, it could be reoccupied and the warehouse operations could resume immediately.« less

A Numerical Study of Factors Affecting Fracture-Fluid Cleanup and Produced Gas/Water in Marcellus Shale: Part II

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

Seales, Maxian B.; Dilmore, Robert; Ertekin, Turgay

Horizontal wells combined with successful multistage-hydraulic-fracture treatments are currently the most-established method for effectively stimulating and enabling economic development of gas-bearing organic-rich shale formations. Fracture cleanup in the stimulated reservoir volume (SRV) is critical to stimulation effectiveness and long-term well performance. But, fluid cleanup is often hampered by formation damage, and post-fracture well performance frequently falls to less than expectations. A systematic study of the factors that hinder fracture-fluid cleanup in shale formations can help optimize fracture treatments and better quantify long-term volumes of produced water and gas. Fracture-fluid cleanup is a complex process influenced by mutliphase flow through porousmore » media (relative permeability hysteresis, capillary pressure), reservoir-rock and -fluid properties, fracture-fluid properties, proppant placement, fracture-treatment parameters, and subsequent flowback and field operations. Changing SRV and fracture conductivity as production progresses further adds to the complexity of this problem. Numerical simulation is the best and most-practical approach to investigate such a complicated blend of mechanisms, parameters, their interactions, and subsequent effect on fracture-fluid cleanup and well deliverability. Here, a 3D, two-phase, dual-porosity model was used to investigate the effect of mutliphase flow, proppant crushing, proppant diagenesis, shut-in time, reservoir-rock compaction, gas slippage, and gas desorption on fracture-fluid cleanup and well performance in Marcellus Shale. Our findings have shed light on the factors that substantially constrain efficient fracture-fluid cleanup in gas shales, and we have provided guidelines for improved fracture-treatment designs and water management.« less

A Numerical Study of Factors Affecting Fracture-Fluid Cleanup and Produced Gas/Water in Marcellus Shale: Part II

DOE PAGES

Seales, Maxian B.; Dilmore, Robert; Ertekin, Turgay; ...

2017-04-01

Horizontal wells combined with successful multistage-hydraulic-fracture treatments are currently the most-established method for effectively stimulating and enabling economic development of gas-bearing organic-rich shale formations. Fracture cleanup in the stimulated reservoir volume (SRV) is critical to stimulation effectiveness and long-term well performance. But, fluid cleanup is often hampered by formation damage, and post-fracture well performance frequently falls to less than expectations. A systematic study of the factors that hinder fracture-fluid cleanup in shale formations can help optimize fracture treatments and better quantify long-term volumes of produced water and gas. Fracture-fluid cleanup is a complex process influenced by mutliphase flow through porousmore » media (relative permeability hysteresis, capillary pressure), reservoir-rock and -fluid properties, fracture-fluid properties, proppant placement, fracture-treatment parameters, and subsequent flowback and field operations. Changing SRV and fracture conductivity as production progresses further adds to the complexity of this problem. Numerical simulation is the best and most-practical approach to investigate such a complicated blend of mechanisms, parameters, their interactions, and subsequent effect on fracture-fluid cleanup and well deliverability. Here, a 3D, two-phase, dual-porosity model was used to investigate the effect of mutliphase flow, proppant crushing, proppant diagenesis, shut-in time, reservoir-rock compaction, gas slippage, and gas desorption on fracture-fluid cleanup and well performance in Marcellus Shale. Our findings have shed light on the factors that substantially constrain efficient fracture-fluid cleanup in gas shales, and we have provided guidelines for improved fracture-treatment designs and water management.« less

Evaluation of Final Radiological Conditions at Areas of the Niagara Falls Storage Site Remediated under the Formerly Utilized Sites Remedial Action Program - 12184

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

Clayton, Christopher; Kothari, Vijendra; Starr, Ken

2012-07-01

The U.S. Department of Energy (DOE) methods and protocols allow evaluation of remediation and final site conditions to determine if remediated sites remain protective. Two case studies are presented that involve the Niagara Falls Storage Site (NFSS) and associated vicinity properties (VPs), which are being remediated under the Formerly Utilized Sites Remedial Action Program (FUSRAP). These properties are a part of the former Lake Ontario Ordnance Works (LOOW). In response to stakeholders concerns about whether certain remediated NFSS VPs were putting them at risk, DOE met with stakeholders and agreed to evaluate protectiveness. Documentation in the DOE records collection adequatelymore » described assessed and final radiological conditions at the completed VPs. All FUSRAP wastes at the completed sites were cleaned up to meet DOE guidelines for unrestricted use. DOE compiled the results of the investigation in a report that was released for public comment. In conducting the review of site conditions, DOE found that stakeholders were also concerned about waste from the Separations Process Research Unit (SPRU) at the Knolls Atomic Power Laboratory (KAPL) that was handled at LOOW. DOE agreed to determine if SPRU waste remained at that needed to be remediated. DOE reviewed records of waste characterization, historical handling locations and methods, and assessment and remediation data. DOE concluded that the SPRU waste was remediated on the LOOW to levels that pose no unacceptable risk and allow unrestricted use and unlimited exposure. This work confirms the following points as tenets of an effective long-term surveillance and maintenance (LTS and M) program: - Stakeholder interaction must be open and transparent, and DOE must respond promptly to stakeholder concerns. - DOE, as the long-term custodian, must collect and preserve site records in order to demonstrate that remediated sites pose no unacceptable risk. - DOE must continue to maintain constructive relationships with the U.S. Army Corps of Engineers and state and federal regulators. After review of historical site documentation, DOE reports, and USACE radiological data, DOE concluded the following: - DOE had access to adequate documentation to evaluate site conditions at the former LOOW. This is important to confirm now, while institutional knowledge of early FUSRAP work remains available. - DOE remediated the completed VPs to conditions that are protective for unrestricted residential use. Sample and walkover gamma scan results indicate that no wastes remain that exceed cleanup criteria. - Process knowledge and field observations establish that Cs-137 is the predominant radionuclide in the KAPL waste stream. Cs-137, a strong gamma emitter, was used as an indicator for remediation of KAPL waste. Other radionuclides were present in much lower relative concentrations and were likely also removed during remediation of the VPs. - KAPL contaminants were removed during remedial activities at the former LOOW as either co-located or co-mingled with other radionuclides. - For the active VPs (VP-E, VP-E', and VP-G), results of DOE's cleanup of the accessible portions of these properties indicate that KAPL waste does not remain at concentrations greater than the DOE cleanup limit: - Inaccessible areas were not associated with historic KAPL waste handling. Therefore, it is unlikely that KAPL waste remains on the active VPs. - Because gamma activity was used by DOE during remediation/verification activities for excavation control, additional USACE cleanup of FUSRAP wastes on these properties will likely result in the remediation of any co-located residual KAPL wastes to acceptable levels or identification of KAPL waste that is not co-located. - Although USACE has not established a cleanup level for Cs-137 on the active NFSS VPs, DOE assessment and remediation data indicate that assessed Cs-137 was remediated and significant Cs-137 is unlikely to remain. Because of the low likelihood of encountering significant KAPL waste on the active NFSS VPs, additional remediation is not anticipated at these properties. - USACE assessment soil sampling results on the NFSS proper indicate that KAPL waste does not exceed the DOE cleanup level for Cs-137. USACE has not established a cleanup level for Cs-137 on NFSS proper. The USACE cleanup of FUSRAP wastes on the NFSS proper will likely result in the remediation of any co-located residual KAPL wastes or identification of KAPL waste that is not co-located. DOE is drafting a report of the investigation of KAPL waste at LOOW. The report will be released to the public for comment when the draft is complete. DOE responses to stakeholder inquiries resulted in a common understanding of site conditions and site risk. DOE expects additional interaction with stakeholders at the former LOOW as USACE completes remediation of the active VPs and the NFSS proper, and these relationships will hopefully have built trust between DOE and the stakeholders that DOE will perform its duties in an open and transparent manner that includes stakeholders as stewards for remediated FUSRAP sites. (authors)« less

78 FR 50447 - Agency Information Collection Activities; Submission for OMB Review; Comment Request; Cleanup...

Federal Register 2010, 2011, 2012, 2013, 2014

2013-08-19

... for OMB Review; Comment Request; Cleanup Program for Accumulations of Coal and Float Coal Dusts, Loose Coal, and Other Combustibles ACTION: Notice. SUMMARY: The Department of Labor (DOL) is submitting the... (ICR) proposal; titled, ``Cleanup Program for Accumulations of Coal and Float Coal Dusts, Loose Coal...

Brownfields to School Sites: How Can the State Facilitate Cleanup To Build Essential Schools?

ERIC Educational Resources Information Center

California State Legislature, Sacramento. Select Committee on Environmental Justice.

This document presents background information and testimony concerning the cleanup of potentially contaminated vacant or underutilized property for use as future school sites in low-income and minority communities. Various proposals are offered that would allow the state, where necessary, to facilitate the cleanup of these "brownfields"…

Texas Coastal Cleanup Report, 1986.

ERIC Educational Resources Information Center

O'Hara, Kathryn; And Others

During the 1986 Coastweek, a national event dedicated to improvement of the marine environment, a large beach cleanup was organized on the Texas coast. The goals of the cleanup were to create public awareness of the problems caused by marine debris, and to collect data on the types and quantities of debris found on the Texas coastline. The…

75 FR 76280 - Regulated Navigation Area; Thea Foss and Wheeler-Osgood Waterways EPA Superfund Cleanup Site...

Federal Register 2010, 2011, 2012, 2013, 2014

2010-12-08

.../ Tideflats superfund cleanup remediation efforts. This RNA will prohibit activities that would disturb the.../Tideflats superfund cleanup remediation process in those waters. These caps consist of approximately three... remediation efforts of the U.S. Environmental Protection Agency (EPA) and others in the Thea Foss and Wheeler...

40 CFR 761.125 - Requirements for PCB spill cleanup.

Code of Federal Regulations, 2012 CFR

2012-07-01

...) Additional pre- or post-cleanup sampling. (B) The estimated cost of the cleanup by man-hours, dollars, or... section are designed to be consistent with existing reporting requirements to the extent possible so as to...) by standard commercial wipe tests. (ii) All soil within the spill area (i.e., visible traces of soil...

40 CFR 761.125 - Requirements for PCB spill cleanup.

Code of Federal Regulations, 2014 CFR

2014-07-01

...) Additional pre- or post-cleanup sampling. (B) The estimated cost of the cleanup by man-hours, dollars, or... section are designed to be consistent with existing reporting requirements to the extent possible so as to...) by standard commercial wipe tests. (ii) All soil within the spill area (i.e., visible traces of soil...

40 CFR 761.125 - Requirements for PCB spill cleanup.

Code of Federal Regulations, 2011 CFR

2011-07-01

...) Additional pre- or post-cleanup sampling. (B) The estimated cost of the cleanup by man-hours, dollars, or... section are designed to be consistent with existing reporting requirements to the extent possible so as to...) by standard commercial wipe tests. (ii) All soil within the spill area (i.e., visible traces of soil...

40 CFR 761.125 - Requirements for PCB spill cleanup.

Code of Federal Regulations, 2013 CFR

2013-07-01

...) Additional pre- or post-cleanup sampling. (B) The estimated cost of the cleanup by man-hours, dollars, or... section are designed to be consistent with existing reporting requirements to the extent possible so as to...) by standard commercial wipe tests. (ii) All soil within the spill area (i.e., visible traces of soil...

40 CFR 761.125 - Requirements for PCB spill cleanup.

Code of Federal Regulations, 2010 CFR

2010-07-01

...) Additional pre- or post-cleanup sampling. (B) The estimated cost of the cleanup by man-hours, dollars, or... section are designed to be consistent with existing reporting requirements to the extent possible so as to...) by standard commercial wipe tests. (ii) All soil within the spill area (i.e., visible traces of soil...

Waste Oil Burn-Off in Coast Guard Powerplants : Waste Oil Filtering Systems and Diesel Engine Performance

DOT National Transportation Integrated Search

1976-06-01

This report documents two tasks of a continuing study to determine the feasibility of burning waste lubricating oils in Coast Guard powerplants. The first task evaluated the effectiveness of two treatment devices for the clean-up of waste lubricating...

Brownfields Assessing Contractor Capabilities for Streamlined Site Investigations -- Additional Information Regarding All Appropriate Inquiries and Hiring an Environmental Professional (November 2006)

EPA Pesticide Factsheets

Guidance for Brownfields grantees and other decision makers to assess the capabilities of contractors and consultants to determine their qualifications to provide streamlined and innovative strategies for the assessment and cleanup of brownfields.

Development and application of an in-cell cleanup pressurized liquid extraction with ultra-high-performance liquid chromatography-tandem mass spectrometry to detect prohibited antiviral agents sensitively in livestock and poultry feces.

PubMed

Wu, Huizhen; Wang, Jianmei; Yang, Hua; Li, Guoqin; Zeng, Yinhuan; Xia, Wei; Li, Zuguang; Qian, Mingrong

2017-03-10

An in-cell cleanup pressurized liquid extraction was developed to analyze prohibited antiviral agents in livestock and poultry feces. Extraction and cleanup were integrated into one step. The extraction was performed using methanol-acetonitrile (1:1, v/v) with 0.5% glacial acetic acid at 90°C, and 0.75g of PSA was used as the adsorbent during the extraction procedure. Under optimal conditions, the average recoveries for 11 antiviral drugs were 71.5-112.5% at three spiked levels (20, 40, and 100μgkg -1 ). The detection limits and detection quantitations of the analysis method for the eleven antiviral drugs were 0.6-1.4 and 1.4-4.7μgkg -1 , respectively. Finally, the method was applied to analyze amantadine, oseltamivir and its metabolites oseltamivir acid in duck feces based on an experiment of an oral dose of two antiviral drugs in duck. The amantadine, oseltamivir and oseltamivir acid can be detected in feces within approximately four weeks after amantadine and oseltamivir were orally administered. The results indicate that the residue analysis in feces is a noninvasive method to monitor inhibited antiviral agents efficiently in livestock and poultry breeding. Copyright © 2017. Published by Elsevier B.V.

Production of activated char from Illinois coal for flue gas cleanup

USGS Publications Warehouse

Lizzio, A.A.; DeBarr, J.A.; Kruse, C.W.

1997-01-01

Activated chars were produced from Illinois coal and tested in several flue gas cleanup applications. High-activity chars that showed excellent potential for both SO2 and NOx removal were prepared from an Illinois No. 2 bituminous coal. The SO2 (120 ??C) and NOx (25 ??C) removal performance of one char compared favorably with that of a commercial activated carbon (Calgon Centaur). The NOx removal performance of the same char at 120 ??C exceeded that of the Centaur carbon by more than 1 order of magnitude. Novel char preparation methods were developed including oxidation/thermal desorption and hydrogen treatments, which increased and preserved, respectively, the active sites for SO2 and NOx adsorption. The results of combined SO2/NOx removal tests, however, suggest that SO2 and NOx compete for similar adsorption sites and SO2 seems to be more strongly adsorbed than NO. A low-activity, low-cost char was also developed for cleanup of incinerator flue gas. A three-step method involving coal preoxidation, pyrolysis, and CO2 activation was used to produce the char from Illinois coal. Five hundred pounds of the char was tested on a slipstream of flue gas from a commercial incinerator in Germany. The char was effective in removing >97% of the dioxins and furans present in the flue gas; mercury levels were below detectable limits.

Screening of a Combinatorial Library of Organic Polymers for the Solid-Phase Extraction of Patulin from Apple Juice

PubMed Central

Giovannoli, Cristina; Spano, Giulia; Di Nardo, Fabio; Anfossi, Laura; Baggiani, Claudio

2017-01-01

Patulin is a water-soluble mycotoxin produced by several species of fungi. Governmental bodies have placed it under scrutiny for its potential negative health effects, and maximum residue limits are fixed in specific food matrices to protect consumers’ health. Confirmatory analysis of patulin in complex food matrices can be a difficult task, and sample clean-up treatments are frequently necessary before instrumental analyses. With the aim of simplifying the clean-up step, we prepared a 256-member combinatorial polymeric library based on 16 functional monomers, four cross-linkers and four different porogenic solvents. The library was screened for the binding towards patulin in different media (acetonitrile and citrate buffer at pH 3.2), with the goal of identifying polymer formulations with good binding properties towards the target compound. As a proof of concept, a methacrylic acid-co-pentaerithrytole tetraacrylate polymer prepared in chloroform was successfully used as a solid-phase extraction material for the clean-up and extraction of patulin from apple juice. Clean chromatographic patterns and acceptable recoveries were obtained for juice spiked with patulin at concentration levels of 25 (64 ± 12%), 50 (83 ± 5.6%) and 100 μg L−1 (76 ± 4.5%). The within-day and between-day reproducibility evaluated at a concentration level of 25 μg L−1 were 5.6 and 7.6%, respectively. PMID:28531103

Health Effects of Exposure to Water-Damaged New Orleans Homes Six Months After Hurricanes Katrina and Rita

PubMed Central

Cummings, Kristin J.; Cox-Ganser, Jean; Riggs, Margaret A.; Edwards, Nicole; Hobbs, Gerald R.; Kreiss, Kathleen

2008-01-01

Objectives. We investigated the relation between respiratory symptoms and exposure to water-damaged homes and the effect of respirator use in posthurricane New Orleans, Louisiana. Methods. We randomly selected 600 residential sites and then interviewed 1 adult per site. We created an exposure variable, calculated upper respiratory symptom (URS) and lower respiratory symptom (LRS) scores, and defined exacerbation categories by the effect on symptoms of being inside water-damaged homes. We used multiple linear regression to model symptom scores (for all participants) and polytomous logistic regression to model exacerbation of symptoms when inside (for those participating in clean-up). Results. Of 553 participants (response rate=92%), 372 (68%) had participated in clean-up; 233 (63%) of these used a respirator. Respiratory symptom scores increased linearly with exposure (P<.05 for trend). Disposable-respirator use was associated with lower odds of exacerbation of moderate or severe symptoms inside water-damaged homes for URS (odds ratio (OR)=.51; 95% confidence interval (CI)=0.24, 1.09) and LRS (OR=0.33; 95% CI=0.13, 0.83). Conclusions. Respiratory symptoms were positively associated with exposure to water-damaged homes, including exposure limited to being inside without participating in clean-up. Respirator use had a protective effect and should be considered when inside water-damaged homes regardless of activities undertaken. PMID:18381997

Quantification of Complex Polycyclic Aromatic Hydrocarbon Mixtures in Standard Reference Materials Using GC×GC/ToF-MS

PubMed Central

Manzano, Carlos; Hoh, Eunha; Massey Simonich, Staci L.

2014-01-01

This research is the first to quantify complex PAH mixtures in NIST SRMs using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC/ToF-MS), with and without extract cleanup, and reports previously unidentified PAH isomers in the NIST SRMs. We tested a novel, high orthogonality GC column combination (LC-50×NSP-35), as well as with a commonly used column combination (Rtx-5ms×Rxi-17) for the quantification of a complex mixture of 85 different PAHs, including parent (PAHs), alkyl- (MPAHs), nitro- (NPAHs), oxy- (OPAHs), thio- (SPAHs), bromo- (BrPAHs), and chloro-PAHs (ClPAHs) in extracts from two standard reference materials: NIST SRM1650b (diesel particulate matter), with cleanup and NIST SRM1975 (diesel particulate extract), with and without extract cleanup. The LC-50×NSP-35 column combination resulted in an average absolute percent difference of 33.8%, 62.2% and 30.8% compared to the NIST certified PAH concentrations for NIST SRM1650b, NIST SRM1975 with cleanup and NIST SRM1975 without cleanup, while the Rtx-5ms×Rxi-17 resulted in an absolute percent difference of 38.6%, 67.2% and 79.6% for NIST SRM1650b, NIST SRM1975 with cleanup and NIST SRM1975 without cleanup, respectively. This GC×GC/ToF-MS method increases the number of PAHs detected and quantified in complex environmental extracts using a single chromatographic run. Without clean-up, 7 additional compounds were detected and quantified in NIST SRM1975 using the LC-50×NSP-35 column combination. These results suggest that the use of the LC-50×NSP-35 column combination in GC×GC/ToF-MS not only results in better chromatographic resolution and greater orthogonality for the separation of complex PAH mixtures, but can also be used for the accurate quantification of complex PAH mixtures in environmental extracts without cleanup. PMID:23932031

SUPERFUND CLEANUPS AND INFANT HEALTH.

PubMed

Currie, Janet; Greenstone, Michael; Moretti, Enrico

2011-05-01

We are the first to examine the effect of Superfund cleanups on infant health rather than focusing on proximity to a site. We study singleton births to mothers residing within 5km of a Superfund site between 1989-2003 in five large states. Our "difference in differences" approach compares birth outcomes before and after a site clean-up for mothers who live within 2,000 meters of the site and those who live between 2,000- 5,000 meters of a site. We find that proximity to a Superfund site before cleanup is associated with a 20 to 25% increase in the risk of congenital anomalies.

Cleanup procedure for water, soil, animal and plant extracts for the use of electron-capture detector in the gas chromatographic analysis of organophosphorus insecticide residues.

PubMed

Kadoum, A M

1968-07-01

A simple, aqueous acetonitrile partition cleanup method for analyses of some common organophosphorus insecticide residues is described. The procedure described is for cleanup and quantitative recovery of parathion, methyl parathion, diazinon, malathion and thimet from different extracts. Those insecticides in the purified extracts of ground water, grain, soil, plant and animal tissues can be detected quantitatively by gas chromatography with an electron capture-detector at 0.01 ppm. Cleanup is satisfactory for paper and thin-layer chromatography for further identification of individual insecticides in the extracts.

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

PubMed

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

2014-01-01

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

Single-laboratory validation of a saponification method for the determination of four polycyclic aromatic hydrocarbons in edible oils by HPLC-fluorescence detection.

PubMed

Akdoğan, Abdullah; Buttinger, Gerhard; Wenzl, Thomas

2016-01-01

An analytical method is reported for the determination of four polycyclic aromatic hydrocarbons (benzo[a]pyrene (BaP), benz[a]anthracene (BaA), benzo[b]fluoranthene (BbF) and chrysene (CHR)) in edible oils (sesame, maize, sunflower and olive oil) by high-performance liquid chromatography. Sample preparation is based on three steps including saponification, liquid-liquid partitioning and, finally, clean-up by solid phase extraction on 2 g of silica. Guidance on single-laboratory validation of the proposed analysis method was taken from the second edition of the Eurachem guide on method validation. The lower level of the working range of the method was determined by the limits of quantification of the individual analytes, and the upper level was equal to 5.0 µg kg(-1). The limits of detection and quantification of the four PAHs ranged from 0.06 to 0.12 µg kg(-1) and from 0.13 to 0.24 µg kg(-1). Recoveries of more than 84.8% were achieved for all four PAHs at two concentration levels (2.5 and 5.0 µg kg(-1)), and expanded relative measurement uncertainties were below 20%. The performance of the validated method was in all aspects compliant with provisions set in European Union legislation for the performance of analytical methods employed in the official control of food. The applicability of the method to routine samples was evaluated based on a limited number of commercial edible oil samples.

Pollution control: utility ships adapt for spill cleanups

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

Not Available

1986-02-01

A practical and cost effective approach to oil spill cleanup is being undertaken by Dutch companies. The approach involves constructing and equipping multi-use ships for pollution control. Usually, these ships are maintained in another type of service and come into use for spill cleanup only when needed. The use of these ships in pollution control is discussed.

75 FR 30753 - Regulated Navigation Area; Thea Foss and Wheeler-Osgood Waterways EPA Superfund Cleanup Site...

Federal Register 2010, 2011, 2012, 2013, 2014

2010-06-02

... superfund cleanup remediation efforts. To more effectively protect those efforts, the Coast Guard is... cleanup remediation process in those waters. These caps consist of approximately three feet of sand and... remediation efforts that underlie the whole concept of the proposed RNA, and we would consult with the City of...

39 CFR 958.23 - Settlement.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 39 Postal Service 1 2010-07-01 2010-07-01 false Settlement. 958.23 Section 958.23 Postal Service..., CLEAN-UP COSTS AND DAMAGES FOR VIOLATION OF HAZARDOUS MATERIAL REGULATIONS § 958.23 Settlement. Either party may make offers of settlement or proposals of adjustment at any time. The Determining Official has...

Savannah River Site Robotics

ScienceCinema

None

2018-04-16

Meet Sandmantis and Frankie, two advanced robotic devices that are key to cleanup at Savannah River Site. Sandmantis cleans hard, residual waste off huge underground storage tanks. Frankie is equipped with unique satellite capabilities and sensing abilties that can determine what chemicals still reside in the tanks in a cost effective manner.

IMPROVED CLEANUP AND DETERMINATION METHOD OF DIALKYL PHOSPHATES IN THE URINE OF CHILDREN EXPOSED TO ORGANOPHOSPHORUS INSECTICIDES. (R825171)

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...

Savannah River Site Robotics

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

None

Meet Sandmantis and Frankie, two advanced robotic devices that are key to cleanup at Savannah River Site. Sandmantis cleans hard, residual waste off huge underground storage tanks. Frankie is equipped with unique satellite capabilities and sensing abilties that can determine what chemicals still reside in the tanks in a cost effective manner.

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

EPA Science Inventory

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

Integrated Forensics Approach To Fingerprint PCB Sources In Sediments Using Immunoassays And GC/MS Congener Analyses

EPA Science Inventory

Determining the original source of contamination to a heterogeneous matrix such as sediments is a requirement for both clean-up and compliance programs within the military. Understanding the source of contaminants to sediment in industrial settings is a prerequisite to implement...

Predicting performance of almonds shells for cleanup of almond soil fumigants from potable water.

USDA-ARS?s Scientific Manuscript database

Almond shell strength and bulk density were determined to differ significantly among almond varieties, and further research demonstrated that granular activated carbons (GAC) produced from shells of different varieties had similar abilities to adsorb DBCP from contaminated water. As an extension of...

Sensitivity limits and EC50 values of the Vibrio fischeri test for organic micropollutants in natural and spiked extracts from sediments

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

Salizzato, M.; Bertato, V.; Pavoni, B.

1998-04-01

Chemical analyses and bioassays were used in conjunction to assess the quality of sediments of the Venice lagoon. Organic micropollutants (polycyclic aromatic hydrocarbons [PAHs] polychlorinated biphenyls [PCBs], and chlorinated pesticides) were extracted from sediment samples and analyzed by gas chromatography after fractionation into classes of compounds. The Vibrio fischeri test was used to assess the acute toxicity of sediment extracts. The test was applied to organic extracts before cleanup and to extracts purified from sulfur and fractionated into single classes of compounds. Extracts before purification were much more toxic than single fractions. In particular, sulfur was toxic to V. fischeri.more » For PAHs and PCBs the 50% effective concentration (EC50) and EC20 values were determined using natural and spiked extracts. Sensitivity limits of the method for these compounds were also estimated as was in EC50 value of elemental sulfur dissolved in ethanol. A mathematical model was used to fit the concentration-response data to a sigmoid curve.« less

Validation of QuEChERS method for the determination of some pesticide residues in two apple varieties.

PubMed

Tiryaki, Osman

2016-10-02

This study was undertaken to validate the "quick, easy, cheap, effective, rugged and safe" (QuEChERS) method using Golden Delicious and Starking Delicious apple matrices spiked at 0.1 maximum residue limit (MRL), 1.0 MRL and 10 MRL levels of the four pesticides (chlorpyrifos, dimethoate, indoxacarb and imidacloprid). For the extraction and cleanup, original QuEChERS method was followed, then the samples were subjected to liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) for chromatographic analyses. According to t test, matrix effect was not significant for chlorpyrifos in both sample matrices, but it was significant for dimethoate, indoxacarb and imidacloprid in both sample matrices. Thus, matrix-matched calibration (MC) was used to compensate matrix effect and quantifications were carried out by using MC. The overall recovery of the method was 90.15% with a relative standard deviation of 13.27% (n = 330). Estimated method detection limit of analytes blew the MRLs. Some other parameters of the method validation, such as recovery, precision, accuracy and linearity were found to be within the required ranges.

A Numerical Study of Factors Affecting Fracture-Fluid Cleanup and Produced Gas/Water in Marcellus Shale: Part II

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

Seales, Maxian B.; Dilmore, Robert; Ertekin, Turgay

Horizontal wells combined with successful multi-stage hydraulic fracture treatments are currently the most established method for effectively stimulating and enabling economic development of gas bearing organic-rich shale formations. Fracture cleanup in the Stimulated Reservoir Volume (SRV) is critical to stimulation effectiveness and long-term well performance. However, fluid cleanup is often hampered by formation damage, and post-fracture well performance frequently falls below expectations. A systematic study of the factors that hinder fracture fluid cleanup in shale formations can help optimize fracture treatments and better quantify long term volumes of produced water and gas. Fracture fluid cleanup is a complex process influencedmore » by multi-phase flow through porous media (relative permeability hysteresis, capillary pressure etc.), reservoir rock and fluid properties, fracture fluid properties, proppant placement, fracture treatment parameters, and subsequent flowback and field operations. Changing SRV and fracture conductivity as production progresses further adds to the complexity of this problem. Numerical simulation is the best, and most practical approach to investigate such a complicated blend of mechanisms, parameters, their interactions, and subsequent impact on fracture fluid cleanup and well deliverability. In this paper, a 3-dimensional, 2-phase, dual-porosity model was used to investigate the impact of multiphase flow, proppant crushing, proppant diagenesis, shut-in time, reservoir rock compaction, gas slippage, and gas desorption on fracture fluid cleanup, and well performance in Marcellus shale. The research findings have shed light on the factors that substantially constrains efficient fracture fluid cleanup in gas shales, and provided guidelines for improved fracture treatment designs and water management.« less

Mental disorders among Chernobyl cleanup workers from Estonia: A clinical assessment.

PubMed

Laidra, Kaia; Rahu, Kaja; Kalaus, Katri-Evelin; Tekkel, Mare; Leinsalu, Mall

2017-08-01

To assess, at a clinical level, the mental health of former Chernobyl cleanup workers from Estonia by comparing them with same-age controls. The Mini International Neuropsychiatric Interview (MINI) was administered during 2011-2012 to 99 cleanup workers and 100 population-based controls previously screened for mental health symptoms. Logistic regression analysis showed that cleanup workers had higher odds of current depressive disorder (odds ratio [OR] = 3.07, 95% confidence interval [CI: 1.34, 7.01]), alcohol dependence (OR = 3.47, 95% CI [1.29, 9.34]), and suicide ideation (OR = 3.44, 95% CI [1.28, 9.21]) than did controls. Except for suicide ideation, associations with Chernobyl exposure became statistically nonsignificant when adjusted for education and ethnicity. A quarter of a century after the Chernobyl accident, Estonian cleanup workers were still at increased risk of mental disorders, which was partly attributable to sociodemographic factors. (PsycINFO Database Record (c) 2017 APA, all rights reserved).

From Cleanup to Stewardship. A companion report to Accelerating Cleanup: Paths to Closure and background information to support the scoping process required for the 1998 PEIS Settlement Study

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

None, None

1999-10-01

Long-term stewardship is expected to be needed at more than 100 DOE sites after DOE's Environmental Management program completes disposal, stabilization, and restoration operations to address waste and contamination resulting from nuclear research and nuclear weapons production conducted over the past 50 years. From Cleanup to stewardship provides background information on the Department of Energy (DOE) long-term stewardship obligations and activities. This document begins to examine the transition from cleanup to long-term stewardship, and it fulfills the Secretary's commitment to the President in the 1999 Performance Agreement to provide a companion report to the Department's Accelerating Cleanup: Paths to Closuremore » report. It also provides background information to support the scoping process required for a study on long-term stewardship required by a 1998 Settlement Agreement.« less

Acrylamide analysis in food by liquid chromatographic and gas chromatographic methods.

PubMed

Elbashir, Abdalla A; Omar, Mei M Ali; Ibrahim, Wan Aini Wan; Schmitz, Oliver J; Aboul-Enein, Hassan Y

2014-01-01

Acrylamide (AA) is a compound classified as carcinogenic to humans by the International Agency for Research on Cancer. It was first discovered to be present in certain heated processed food by the Swedish National Food Administration (SNFA) and University of Stockholm in early 2002. The major pathway for AA formation in food is the Maillard reaction between reducing sugar and the amino acid asparagine at high temperature. Since the discovery of AA's presence in food, many analytical methods have been developed for determination of AA contents in different food matrices. Also, several studies have been conducted to develop extraction procedures for AA from difficult food matrices. AA is a small, highly polar molecule, which makes its extraction and analysis challenging. Many articles and reviews have been published dealing with AA in food. The aim of the review is to discuss AA formation in food, the factors affecting AA formation and removal, AA exposure assessment, AA extraction and cleanup from food samples, and analytical methods used in AA determination, such as high-performance liquid chromatography (HPLC) and gas chromatography (GC). Special attention is given to sample extraction and cleanup procedures and analytical techniques used for AA determination.

Determination of organochlorine pesticide and polychlorinated biphenyl residues in fatty fish by tandem solid-phase extraction cleanup.

PubMed

Schenck, F J; Calderon, L; Podhorniak, L V

1996-01-01

A rapid, multiresidue solid-phase extraction (SPE) technique for determination of organochlorine pesticide and polychlorinated biphenyl (PCB) residues in nonfatty fish was modified for use with fatty fish. In the modified procedures, samples are extracted with acetonitrile, and the extract is cleaned up with both C18 and Florisil SPE columns. Residues are determined by gas chromatography with electron capture detection. The original method was modified for use with fatty fish by reducing the amount of tissue extracted and by using an improved Florisil SPE cleanup. Recovery data are presented for 24 fortified organochlorine pesticide residues (0.12 ppm) and 3 fortified PCB residues (0.80 ppm) from flounder, bluefish, and shad samples, which contained 0.8, 5.4, and 22.6% fat, respectively. For the 3 types of fish, recoveries of 23 of 24 fortified organochlorine pesticide residues ranged from 55 to 129%, and recoveries of 3 fortified PCB residues ranged from 55 to 104%. There were no significant differences in recovery based on fish species and/or fat content for the majority of residues studied. This SPE method and the official AOAC method yielded comparable results for fish containing incurred organochlorine residues.

Combined extraction-cleanup column chromatographic procedure for determination of dicofol in avian eggs

USGS Publications Warehouse

Krynitsky, A.J.; Stafford, C.J.; Wiemeyer, Stanley N.

1988-01-01

Dicofol in avian eggs was completely oxidized to dichlorobenzophenone (DCBP) when a hexane Soxhlet extraction procedure was used. This degradation did not occur with other avian tissues (muscle and liver). For this reason, a combined extraction-cleanup column chromatographic procedure, without added heat, was developed for the determination of dicofol in avian eggs. Homogenized subsamples of eggs were mixed with sodium sulfate, and the mixture was added as the top layer on a column prepacked with Florisil. The dicofol and other compounds of interest were then eluted with ethyl ether-hexane. The extracts, relatively free from lipids, were quantitated on a gas chromatograph equipped with a 63Ni electron-capture detector and a methyl silicone capillary column. Recoveries from chicken eggs, fortified with dicofol and other DDT-related compounds, averaged 96%. Analysis of eggs of eastern screech-owls, fed a meat diet containing 10 ppm technical Kelthane, showed that both dicofol and DCBP were present. Results were confirmed by gas chromatography/mass spectrometry. This method is rapid and reliable, involves a minimum of sample handling, and is well suited for high volume determination of dicofol in eggs and other avian tissues.

Lysergic acid amide as chemical marker for the total ergot alkaloids in rye flour - Determination by high-performance thin-layer chromatography-fluorescence detection.

PubMed

Oellig, Claudia

2017-07-21

Ergot alkaloids are generally determined by high-performance liquid chromatography (HPLC) coupled to fluorescence detection (FLD) or mass selective detection, analyzing the individual compounds. However, fast and easy screening methods for the determination of the total ergot alkaloid content are more suitable, since for monitoring only the sum of the alkaloids is relevant. The herein presented screening uses lysergic acid amide (LSA) as chemical marker, formed from ergopeptine alkaloids, and ergometrine for the determination of the total ergot alkaloids in rye with high-performance thin-layer chromatography-fluorescence detection (HPTLC-FLD). An ammonium acetate buffered extraction step was followed by liquid-liquid partition for clean-up before the ergopeptine alkaloids were selectively transformed to LSA and analyzed by HPTLC-FLD on silica gel with isopropyl acetate/methanol/water/25% ammonium hydroxide solution (80:10:3.8:1.1, v/v/v/v) as the mobile phase. The enhanced native fluorescence of LSA and unaffected ergometrine was used for quantitation without any interfering matrix. Limits of detection and quantitation were 8 and 26μg LSA/kg rye, which enables the determination of the total ergot alkaloids far below the applied quality criterion limit for rye. Close to 100% recoveries for different rye flours at relevant spiking levels were obtained. Thus, reliable results were guaranteed, and the fast and efficient screening for the total ergot alkaloids in rye offers a rapid alternative to the HPLC analysis of the individual compounds. Copyright © 2017 Elsevier B.V. All rights reserved.

Microwave-assisted extraction at atmospheric pressure coupled to different clean-up methods for the determination of organophosphorus pesticides in olive and avocado oil.

PubMed

Fuentes, Edwar; Báez, María E; Díaz, Juan

2009-12-18

An effective extraction method was devised for the determination of organophosphorus pesticides (OPPs) in olive and avocado oil samples, using atmospheric pressure microwave-assisted liquid-liquid extraction (APMAE) and solid-phase extraction or low-temperature precipitation as clean-up step. A simple glass system equipped with an air-cooled condenser was designed as an extraction vessel. The pesticides were partitioned between acetonitrile and oil solution in hexane. Analytical determinations were carried out by gas chromatography-flame photometric detection and gas chromatography-tandem mass spectrometry, using a triple quadrupole mass analyzer, for confirmation purposes. Several factors influencing the extraction efficiency were investigated and optimized through fractional factorial design and Doehlert design. Under optimal conditions the recovery of pesticides from oil at 0.025 microg g(-1) ranged from 71% to 103%, except for fenthion in avocado oil, with RSDs < or = 13% (n=5). The LOQ for the entire method ranged from 0.004 to 0.015 microg g(-1). Finally, the proposed method was successfully applied to the extraction and determination of the selected pesticides in 20 commercially packed extra virgin olive oils and four commercially packed avocado oils produced in Chile. Detectable residues of different OPPs were observed in 85% of samples.

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

USDA-ARS?s Scientific Manuscript database

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...

Environmental Liabilities: DoD Training Range Cleanup Cost Estimates Are Likely Understated

DTIC Science & Technology

2001-04-01

1Federal accounting standards define environmental cleanup costs as...report will not be complete or accurate. Federal financial accounting standards have required that DOD report a liability for the estimated cost of...within the range is better than any other amount. SFFAS No. 6, Accounting for Property, Plant, and Equipment, further defines cleanup costs as costs for

Cleanup Verification Package for the 118-F-5 PNL Sawdust Pit

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

L. D. Habel

2008-05-20

This cleanup verification package documents completion of remedial action, sampling activities, and compliance with cleanup criteria for the 118-F-5 Burial Ground, the PNL (Pacific Northwest Laboratory) Sawdust Pit. The 118-F-5 Burial Ground was an unlined trench that received radioactive sawdust from the floors of animal pens in the 100-F Experimental Animal Farm.

SUPERFUND CLEANUPS AND INFANT HEALTH

PubMed Central

Currie, Janet; Greenstone, Michael; Moretti, Enrico

2013-01-01

We are the first to examine the effect of Superfund cleanups on infant health rather than focusing on proximity to a site. We study singleton births to mothers residing within 5km of a Superfund site between 1989–2003 in five large states. Our “difference in differences” approach compares birth outcomes before and after a site clean-up for mothers who live within 2,000 meters of the site and those who live between 2,000– 5,000 meters of a site. We find that proximity to a Superfund site before cleanup is associated with a 20 to 25% increase in the risk of congenital anomalies. PMID:25152535

Managing previously disposed waste to today's standards

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

Not Available

1990-01-01

A Radioactive Waste Management Complex (RWMC) was established at the Idaho National Engineering Laboratory (INEL) in 1952 for controlled disposal of radioactive waste generated at the INEL. Between 1954 and 1970 waste characterized by long lived, alpha emitting radionuclides from the Rocky Flats Plant was also buried at this site. Migration of radionuclides and other hazardous substances from the buried Migration of radionuclides and other hazardous substances from the buried waste has recently been detected. A Buried Waste Program (BWP) was established to manage cleanup of the buried waste. This program has four objectives: (1) determine contaminant sources, (2) determinemore » extent of contamination, (3) mitigate migration, and (4) recommend an alternative for long term management of the waste. Activities designed to meet these objectives have been under way since the inception of the program. The regulatory environment governing these activities is evolving. Pursuant to permitting activities under the Resource Conservation and Recovery Act (RCRA), the Department of Energy (DOE) and the Environmental Protection Agency (EPA) entered into a Consent Order Compliance Agreement (COCA) for cleanup of past practice disposal units at the INEL. Subsequent to identification of the RWMC as a release site, cleanup activities proceeded under dual regulatory coverage of RCRA and the Atomic Energy Act. DOE, EPA, and the State of Idaho are negotiating a RCRA/Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA) Interagency Agreement (IAG) for management of waste disposal sites at the INEL as a result of the November 1989 listing of the INEL on the National Priority List (NPL). Decision making for selection of cleanup technology will be conducted under the CERCLA process supplemented as required to meet the requirements of the National Environmental Policy Act (NEPA). 7 figs.« less

Structural changes in lymphocytes membrane of Chernobyl clean-up workers from Latvia.

PubMed

Kalnina, Inta; Zvagule, Tija; Gabruseva, Natalija; Kirilova, Jelena; Kurjane, Natalja; Bruvere, Ruta; Kesters, Andris; Kizane, Gunta; Kirilovs, Georgijs; Meirovics, Imants

2007-11-01

ABM (3-aminobenzanthrrone derivative) developed at the Riga Technical University, Riga, Latvia) has been previously shown as a potential probe for determination of the immune state of patients with different pathologies . The fist study (using probe ABM) of peripheral blood mononuclear cells (PBMC) membranes of 97 Chernobyl clean-up workers from Latvia was conducted in 1997. Now we repeatedly examine the same (n = 54) individuals in dynamics. ABM spectral parameters in PBMC suspension, fluorescence anisotropy and blood plasma albumin characteristics were recorded. In 1997 screening showed 5 different patterns of fluorescence spectra, from which in 2007 we obtained only two. These patterns of spectra had never been previously seen in healthy individuals or patients with tuberculosis, multiple sclerosis, rheumatoid arthritis, etc., examined by us. Patterns of ABM fluorescence spectra are associated with membrane anisotropy and conformational changes of blood plasma albumin. We observed that in dynamics 1997-2007 the lipid compartment of the membrane became more fluid while the lipid-protein interface became more rigid. The use of probe ANS and albumin auto-fluorescence allowed show conformational alterations in Chernobyl clean-up workers blood plasma. It is necessary to note that all investigated parameters significantly differ in observed groups of patients. These findings reinforce our understanding that that the cell membrane is a significant biological target of radiation. The role of the membrane in the expression and course of cell damage after radiation exposure must be considered. So ten years dynamic of PBMC membrane characteristics by ABM (spectral shift and anisotropy indexes) in Chernobyl clean-up workers reveal progressive trend toward certain resemblance with those of chronic B-cell lymphoid leukemia.

Liquid chromatography determination of 10-hydroxycamptothecin in human serum by a column-switching system containing a pre-column with restricted access media and its application to a clinical pharmacokinetic study.

PubMed

Ma, Jun; Jia, Zheng-Ping; Zhang, Qiang; Fan, Jun-Jie; Jiang, Ning-Xi; Wang, Rong; Xie, Hua; Wang, Juan

2003-10-25

A simple, rapid, sensitive column-switching HPLC method is described for the analysis of the 10-hydroxycamptothecin (HCPT) in human serum. A pre-column containing restricted access media (RAM) is used for the sample clean-up and trace enrichment and is combined with a C18 column for the final separation. The analytical time is 8 min. The HCPT is monitored with fluorescence detector, excitation and emission wavelengths being 385 and 539 nm, respectively. There is a linear response range of 1-1000 ng/ml with correlation coefficient of 0.998 while the limit of quantification is 0.1 ng/ml. The intra-day and inter-day variations are less than 5%. This analytic procedure has been applied to a pharmacokinetic study of HCPT in clinical patients and the pharmacokinetic parameters of one-compartment model are calculated.

Current approaches for the assessment of in situ biodegradation.

PubMed

Bombach, Petra; Richnow, Hans H; Kästner, Matthias; Fischer, Anko

2010-04-01

Considering the high costs and technical difficulties associated with conventional remediation strategies, in situ biodegradation has become a promising approach for cleaning up contaminated aquifers. To verify if in situ biodegradation of organic contaminants is taking place at a contaminated site and to determine if these processes are efficient enough to replace conventional cleanup technologies, a comprehensive characterization of site-specific biodegradation processes is essential. In recent years, several strategies including geochemical analyses, microbial and molecular methods, tracer tests, metabolite analysis, compound-specific isotope analysis, and in situ microcosms have been developed to investigate the relevance of biodegradation processes for cleaning up contaminated aquifers. In this review, we outline current approaches for the assessment of in situ biodegradation and discuss their potential and limitations. We also discuss the benefits of research strategies combining complementary methods to gain a more comprehensive understanding of the complex hydrogeological and microbial interactions governing contaminant biodegradation in the field.

A rapid high-performance liquid-chromatographic method for simultaneously determining the concentrations of TFM and Bayer 73 in water during lampricide treatments

USGS Publications Warehouse

Dawson, V.K.

1982-01-01

The high-performance liquid-chromatography (HPLC) procedure requires only minutes per sample, is specific, and is relatively sensitive (limit of detection 18 disposable cartridge. The cartridge adsorbs and retains both the lampricides and the internal standard. The quantitative elution of the three chemicals from the cartridge with a small volume of methanol effectively concentrates the sample and provides sample cleanup. The methanol extract is then analyzed directly by HPLC on an MCH 10 reverse phase column by using a methanol:0.01 mol/L acetate buffer (87:13, v:v) as the mobile phase at 2 mL/min and detected by ultraviolet spectrophotometry at 330 (or 254) nm. A microprocessor data system further facilitates the procedure by quantifying off-scale peaks and yielding results directly in units of concentration (mg/L).

Screening of grapes and wine for azoxystrobin, kresoxim-methyl and trifloxystrobin fungicides by HPLC with diode array detection.

PubMed

De Melo Abreu, Susana; Correia, Manuela; Herbert, Paulo; Santos, Lúcia; Alves, Arminda

2005-06-01

The Quinone outside Inhibitors (QoI) are one of the most important and recent fungicide groups used in viticulture and also allowed by Integrated Pest Management. Azoxystrobin, kresoxim-methyl and trifloxystrobin are the main active ingredients for treating downy and powdery mildews that can be present in grapes and wines. In this paper, a method is reported for the analysis of these three QoI-fungicides in grapes and wine. After liquid-liquid extraction and a clean-up on commercial silica cartridges, analysis was by isocratic HPLC with diode array detection (DAD) with a run time of 13 min. Confirmation was by solid-phase micro-extraction (SPME), followed by GC/MS determination. The main validation parameters for the three compounds in grapes and wine were a limit of detection up to 0.073 mg kg(-1), a precision not exceeding 10.0% and an average recovery of 93% +/- 38.

Early decision framework for integrating sustainable risk management for complex remediation sites: Drivers, barriers, and performance metrics.

PubMed

Harclerode, Melissa A; Macbeth, Tamzen W; Miller, Michael E; Gurr, Christopher J; Myers, Teri S

2016-12-15

As the environmental remediation industry matures, remaining sites often have significant underlying technical challenges and financial constraints. More often than not, significant remediation efforts at these "complex" sites have not achieved stringent, promulgated cleanup goals. Decisions then have to be made about whether and how to commit additional resources towards achieving those goals, which are often not achievable nor required to protect receptors. Guidance on cleanup approaches focused on evaluating and managing site-specific conditions and risks, rather than uniformly meeting contaminant cleanup criteria in all media, is available to aid in this decision. Although these risk-based cleanup approaches, such as alternative endpoints and adaptive management strategies, have been developed, they are under-utilized due to environmental, socio-economic, and risk perception barriers. Also, these approaches are usually implemented late in the project life cycle after unsuccessful remedial attempts to achieve stringent cleanup criteria. In this article, we address these barriers by developing an early decision framework to identify if site characteristics support sustainable risk management, and develop performance metrics and tools to evaluate and implement successful risk-based cleanup approaches. In addition, we address uncertainty and risk perception challenges by aligning risk-based cleanup approaches with the concepts of risk management and sustainable remediation. This approach was developed in the context of lessons learned from implementing remediation at complex sites, but as a framework can, and should, be applied to all sites undergoing remediation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Automated Mini-Column Solid-Phase Extraction Cleanup for High-Throughput Analysis of Chemical Contaminants in Foods by Low-Pressure Gas Chromatography-Tandem Mass Spectrometry.

PubMed

Lehotay, Steven J; Han, Lijun; Sapozhnikova, Yelena

2016-01-01

This study demonstrated the application of an automated high-throughput mini-cartridge solid-phase extraction (mini-SPE) cleanup for the rapid low-pressure gas chromatography-tandem mass spectrometry (LPGC-MS/MS) analysis of pesticides and environmental contaminants in QuEChERS extracts of foods. Cleanup efficiencies and breakthrough volumes using different mini-SPE sorbents were compared using avocado, salmon, pork loin, and kale as representative matrices. Optimum extract load volume was 300 µL for the 45 mg mini-cartridges containing 20/12/12/1 (w/w/w/w) anh. MgSO 4 /PSA (primary secondary amine)/C 18 /CarbonX sorbents used in the final method. In method validation to demonstrate high-throughput capabilities and performance results, 230 spiked extracts of 10 different foods (apple, kiwi, carrot, kale, orange, black olive, wheat grain, dried basil, pork, and salmon) underwent automated mini-SPE cleanup and analysis over the course of 5 days. In all, 325 analyses for 54 pesticides and 43 environmental contaminants (3 analyzed together) were conducted using the 10 min LPGC-MS/MS method without changing the liner or retuning the instrument. Merely, 1 mg equivalent sample injected achieved <5 ng g -1 limits of quantification. With the use of internal standards, method validation results showed that 91 of the 94 analytes including pairs achieved satisfactory results (70-120 % recovery and RSD ≤ 25 %) in the 10 tested food matrices ( n  = 160). Matrix effects were typically less than ±20 %, mainly due to the use of analyte protectants, and minimal human review of software data processing was needed due to summation function integration of analyte peaks. This study demonstrated that the automated mini-SPE + LPGC-MS/MS method yielded accurate results in rugged, high-throughput operations with minimal labor and data review.

Alternative Endpoints and Approaches Selected for the Remediation of Contaminated Groundwater at Complex Sites

NASA Astrophysics Data System (ADS)

Deeb, R. A.; Hawley, E.

2011-12-01

This presentation will focus on findings, statistics, and case studies from a recently-completed report for the Department of Defense's Environmental Security Technology Certification Program (ESTCP) (Project ER-0832) on alternative endpoints and alternative remedial strategies for groundwater remediation under a variety of Federal and state cleanup programs, including technical impracticability (TI) and other Applicable or Relevant and Appropriate Requirement (ARAR) waivers, state and local designations such as groundwater management zones, Alternate Concentration Limits (ACLs), use of monitored natural attenuation (MNA) over long timeframes, and more. The primary objective of the project was to provide environmental managers and regulators with tools, metrics, and information needed to evaluate alternative endpoints for groundwater remediation at complex sites. A statistical analysis of Comprehensive Environmental Response, Compensation and Liability Act (CERCLA) sites receiving TI waivers will be presented as well as case studies of other types of alternative endpoints and alternative remedial strategies to illustrate the variety of approaches used at complex sites and the technical analyses used to predict and document cost, timeframe, and potential remedial effectiveness. Case studies provide examples of the flexible, site-specific, application of alternative endpoints and alternative remedial strategies that have been used in the past to manage and remediate groundwater contamination at complex sites. For example, at least 13 states consider some designation for groundwater containment in their corrective action policies, such as groundwater management zones, containment zones, and groundwater classification exemption areas. These designations typically indicate that groundwater contamination is present above permissible levels. Soil and groundwater within these zones are managed to protect human health and the environment. Lesson learned for the analyses conducted and the case studies evaluated allow for a more careful consideration of alternative, beneficial, and cost-effective cleanup objectives and metrics that can be achieved over the short-term (while eventually meeting long-term cleanup objectives or demonstrating the applicability of alternative endpoints), thus improving the site cleanup process at complex sites where appropriate.

Analysis of sulfonamides, tilmicosin and avermectins residues in typical animal matrices with multi-plug filtration cleanup by liquid chromatography-tandem mass spectrometry detection.

PubMed

Qin, Yuhong; Jatamunua, Freedom; Zhang, Jingru; Li, Yanjie; Han, Yongtao; Zou, Nan; Shan, Jihao; Jiang, Yanbin; Pan, Canping

2017-05-15

The frequent use of various veterinary drugs could lead to residue bioaccumulation in animal tissues, which could cause dietary risks to human health. In order to quickly analyze the residues, a liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for detecting Sulfonamides, Tilmicosin and Avermectins (AVMs) residues in animal samples. For sample preparation, modified QuEChERS (quick, easy, cheap, effective, rugged and safe) and ultrasound-assisted extraction (UAE) methods were used. For sample cleanup, n-Hexane delipidation and multi-plug filtration cleanup (m-PFC) method based on primary-secondary amine (PSA) and octadecyl-silica (C18) were used, followed by LC-MS/MS analysis. It was validated on 7 animal matrices (bovine, caprine, swine meat and their kidneys, milk) at two fortified concentration levels of 5 and 100μg/kg. The recoveries ranged from 82 to 107% for all analytes with relative standard deviations (RSDs) less than 15%. Matrix-matched calibrations were performed with coefficients of determination above 0.998 for all analytes within concentration levels of 5-500μg/kg. The developed method was successfully used to analysis veterinary drugs of real animal samples from local markets. Copyright © 2017 Elsevier B.V. All rights reserved.

Study of Hand-Held Fire Extinguishers Aboard Civil Aviation Aircraft.

DTIC Science & Technology

1982-06-01

or combustion products of the polymers used in aircraft construction have been found to include carbon monoxide (CO), carbon dioxide (CO ), hydrogen...toxicity rating, and ease of cleanup. The extinguishing agents used in this country for hand portable fire extinguishers are Carbon Dioxide, water, Halon...point where combustion stops." " Carbon dioxide fire extinguishing systems are useful within the limits of this standard in extinguishing fires in

Determination of novel brominated flame retardants and polybrominated diphenyl ethers in serum using gas chromatography-mass spectrometry with two simplified sample preparation procedures.

PubMed

Gao, Le; Li, Jian; Wu, Yandan; Yu, Miaohao; Chen, Tian; Shi, Zhixiong; Zhou, Xianqing; Sun, Zhiwei

2016-11-01

Two simple and efficient pretreatment procedures have been developed for the simultaneous extraction and cleanup of six novel brominated flame retardants (NBFRs) and eight common polybrominated diphenyl ethers (PBDEs) in human serum. The first sample pretreatment procedure was a quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based approach. An acetone/hexane mixture was employed to isolate the lipid and analytes from the serum with a combination of MgSO 4 and NaCl, followed by a dispersive solid-phase extraction (d-SPE) step using C18 particles as a sorbent. The second sample pretreatment procedure was based on solid-phase extraction. The sample extraction and cleanup were conducted directly on an Oasis HLB SPE column using 5 % aqueous isopropanol, concentrated sulfuric acid, and 10 % aqueous methanol, followed by elution with dichloromethane. The NBFRs and PBDEs were then detected using gas chromatography-negative chemical ionization mass spectrometry (GC-NCI MS). The methods were assessed for repeatability, accuracy, selectivity, limits of detection (LODs), and linearity. The results of spike recovery experiments in fetal bovine serum showed that average recoveries ranged from 77.9 % to 128.8 % with relative standard deviations (RSDs) from 0.73 % to 12.37 % for most of the analytes. The LODs for the analytes in fetal bovine serum ranged from 0.3 to 50.8 pg/mL except for decabromodiphenyl ethane. The proposed method was successfully applied to the determination of the 14 brominated flame retardants in human serum. The two pretreatment procedures described here are simple, accurate, and precise, and are suitable for the routine analysis of human serum. Graphical Abstract Workflow of a QuEChERS-based approach (top) and an SPE-based approach (bottom) for the detection of PBDEs and NBFRs in serum.

The use of coenzyme Q0 as a template in the development of a molecularly imprinted polymer for the selective recognition of coenzyme Q10.

PubMed

Contin, Mario; Flor, Sabrina; Martinefski, Manuela; Lucangioli, Silvia; Tripodi, Valeria

2014-01-07

In this work, a novel molecularly imprinted polymer (MIP) for use as a solid phase extraction sorbent was developed for the determination of coenzyme Q10 (CoQ10) in liver extract. CoQ10 is an essential cofactor in mitochondrial oxidative phosphorylation and a powerful antioxidant agent found in low concentrations in biological samples. This fact and its high hydrophobicity make the analysis of CoQ10 technically challenging. Accordingly, a MIP was synthesised using coenzyme Q0 as the template, methacrylic acid as the functional monomer, acetonitrile as the porogen, ethylene glycol dimethacrylate as the crosslinker and benzoyl peroxide as the initiator. Various parameters affecting the polymer preparation and extraction efficiency were evaluated. Morphological characterisation of the MIP and its proper comparison with C18 as a sorbent in solid phase extraction were performed. The optimal conditions for the molecularly imprinted solid phase extraction (MISPE) consisted of 400 μL of sample mixed with 30 mg of MIP and 600 μL of water to reach the optimum solution loading. The loading was followed by a washing step consisting of 1 mL of a 1-propanol solution (1-propanol:water, 30:70,v/v) and elution with 1 mL of 1-propanol. After clean-up, the CoQ10 in the samples was analysed by high performance liquid chromatography. The extraction recoveries were higher than 73.7% with good precision (3.6-8.3%). The limits of detection and quantification were 2.4 and 7.5 μg g(-1), respectively, and a linear range between 7.5 and 150 μg g(-1) of tissue was achieved. The new MISPE procedure provided a successful clean-up for the determination of CoQ10 in a complex matrix. Copyright © 2013 Elsevier B.V. All rights reserved.

[Determination of paraquat and diquat in drinking water and environmental water by high performance liquid chromatography coupled with on-line clean-up and solid phase extraction].

PubMed

Chen, Jing; Liu, Zhaojin; An, Baochao; Lu, Yan; Xu, Qun

2012-10-01

An on-line solid phase extraction (SPE) system was used to eliminate the interferences sufficiently and fulfill the simple and sensitive determination of diquat and paraquat in tap and pond water. This on-line SPE system used two SPE cartridges. One was an Acclaim Mixed-Mode WAX-1 cartridge for the elimination of anionic interferences; the other one was an Acclaim Mixed-Mode WCX-1 cartridge for the enrichment of diquat and paraquat and the elimination of co-enriched cationic interferences. The baseline separation of diquat and paraquat was achieved on an Acclaim Trinity P1 column. A dual-gradient high performance liquid chromatographic (HPLC) system provided an efficient platform to fulfill the on-line SPE and separation, and the system operated under automatic control of chromatography data system software. The complete analysis only required 16 min, and the detection limits of the method were 0.12 microg/L for diquat and 0.10 microg/L for paraquat. The method is simple, rapid and sensitive, and can be applied to the determination of diquat and paraquat in drinking water and environmental water.

Multi-class methodology to determine pesticides and mycotoxins in green tea and royal jelly supplements by liquid chromatography coupled to Orbitrap high resolution mass spectrometry.

PubMed

Martínez-Domínguez, Gerardo; Romero-González, Roberto; Garrido Frenich, Antonia

2016-04-15

A multi-class methodology was developed to determine pesticides and mycotoxins in food supplements. The extraction was performed using acetonitrile acidified with formic acid (1%, v/v). Different clean-up sorbents were tested, and the best results were obtained using C18 and zirconium oxide for green tea and royal jelly, respectively. The compounds were determined using ultra high performance liquid chromatography (UHPLC) coupled to Exactive-Orbitrap high resolution mass spectrometry (HRMS). The recovery rates obtained were between 70% and 120% for most of the compounds studied with a relative standard deviation <25%, at three different concentration levels. The calculated limits of quantification (LOQ) were <10 μg/kg. The method was applied to green tea (10) and royal jelly (8) samples. Nine (eight of green tea and one of royal jelly) samples were found to be positive for pesticides at concentrations ranging from 10.6 (cinosulfuron) to 47.9 μg/kg (paclobutrazol). The aflatoxin B1 (5.4 μg/kg) was also found in one of the green tea samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

Optimization of matrix solid-phase dispersion for the rapid determination of salicylate and benzophenone-type UV absorbing substances in marketed fish.

PubMed

Tsai, Dung-Ying; Chen, Chien-Liang; Ding, Wang-Hsien

2014-07-01

A simple and effective method for the rapid determination of five salicylate and benzophenone-type UV absorbing substances in marketed fish is described. The method involves the use of matrix solid-phase dispersion (MSPD) prior to their determination by on-line silylation gas chromatography tandem mass spectrometry (GC-MS/MS). The parameters that affect the extraction efficiency were optimized using a Box-Behnken design method. The optimal extraction conditions involved dispersing 0.5g of freeze-dried powdered fish with 1.0g of Florisil using a mortar and pestle. This blend was then transferred to a solid-phase extraction (SPE) cartridge containing 1.0g of octadecyl bonded silica (C18), as the clean-up co-sorbent. The target analytes were then eluted with 7mL of acetonitrile. The extract was derivatized on-line in the GC injection-port by reaction with a trimethylsilylating (TMS) reagent. The TMS-derivatives were then identified and quantitated by GC-MS/MS. The limits of quantitation (LOQs) were less than 0.1ng/g. Copyright © 2014 Elsevier Ltd. All rights reserved.

[Determination of alkylphenol and alkylphenolpolyethoxylates in brine by solid phase extraction and high performance liquid chromatography-mass spectrometry].

PubMed

Wang, Jincheng; Xiong, Li; Zhang, Haijun; Chen, Jiping

2011-12-01

A simple method based on solid phase extraction (SPE) coupled with high performance liquid chromatography-mass spectrometry (HPLC-MS) was developed for the determination of octylphenol (OP), nonylphenol (NP), octylphenol ethoxylates (OPEOs) and nonylphenol ethoxylates (NPEOs) in brine. The extraction and cleanup of brine samples were performed on C18 solid-phase extraction cartridges. The complete separation among OP, NP, OPEOs and NPEOs was achieved on a Hypersil GOLD analytical column with methanol-water as the mobile phase. The determination was achieved using HPLC-MS with electrospray ionization (ESI) in selected ion monitoring mode. The results showed that the average recoveries of target compounds were 59.6% - 104.4% and the corresponding relative standard deviations (RSDs, n = 3) were 1.0% - 13.5%. The instrumental limits of detection for the compounds were 0.08 - 3 microg/L. This method was applied to the analysis of the samples of seawater near Dalian coast. The results showed that both NP and NPEOs were detected in all samples and their concentrations in seaport and oil port were much higher than those in other sampling sites.

Coast Guard's Response to Spilled Oil

ERIC Educational Resources Information Center

Ard, R. W., Jr.

1976-01-01

The Coast Guard utilizes a number of monitoring detectors, sensors, and techniques to find, recover and identify oil spills. Discussed in this article are in-situ and airborne sensors, systems developed to provide clean-up capability such as air deployable anti-pollution transfer system (ADAPTS), and techniques which will determine the source of a…

77 FR 9847 - Safety Zone; Kinnickinnic River Containment and Cleanup; Milwaukee, WI

Federal Register 2010, 2011, 2012, 2013, 2014

2012-02-21

... entering the Kinnickinnic River from an underground fuel leak in the vicinity of the airport in Milwaukee... That Significantly Affect Energy Supply, Distribution, or Use. We have determined that it is not a... Executive Order 12866 and is not likely to have a significant adverse effect on the supply, distribution, or...

PROTOCOL FOR DETERMINING BIOAVAILABILITY AND BIOKINETICS OF ORGANIC POLLUTANTS IN DISPERSED, COMPACTED AND INTACT SOIL SYSTEMS TO ENHANCE IN SITU BIOREMEDIATION

EPA Science Inventory

The development of effective in situ and on-site bioremediation technologies can facilitate the cleanup of chemically-contaminated soil sites. Knowledge of biodegradation kinetics and bioavailability of organic pollutants can facilitate decisions on the efficacy of in situ and o...

Reactor water cleanup system

DOEpatents

Gluntz, Douglas M.; Taft, William E.

1994-01-01

A reactor water cleanup system includes a reactor pressure vessel containing a reactor core submerged in reactor water. First and second parallel cleanup trains are provided for extracting portions of the reactor water from the pressure vessel, cleaning the extracted water, and returning the cleaned water to the pressure vessel. Each of the cleanup trains includes a heat exchanger for cooling the reactor water, and a cleaner for cleaning the cooled reactor water. A return line is disposed between the cleaner and the pressure vessel for channeling the cleaned water thereto in a first mode of operation. A portion of the cooled water is bypassed around the cleaner during a second mode of operation and returned through the pressure vessel for shutdown cooling.

Clean-up and disposal process of polluted sediments from urban rivers.

PubMed

He, P J; Shao, L M; Gu, G W; Bian, C L; Xu, C

2001-10-01

In this paper, the discussion is concentrated on the properties of the polluted sediments and the combination of clean-up and disposal process for the upper layer heavily polluted sediments with good flowability. Based on the systematic analyses of various clean-up processes, a suitable engineering process has been evaluated and recommended. The process has been applied to the river reclamation in Yangpu District of Shanghai City, China. An improved centrifuge is used for dewatering the dredged sludge, which plays an important role in the combination of clean-up and disposal process. The assessment of the engineering process shows its environmental and technical economy feasibility, which is much better than that of traditional dredging-disposal processes.

Assessments of the efficacy of a long-term application of a phytoremediation system using hybrid poplar trees at former oil tank farm sites.

PubMed

El-Gendy, Ahmed S; Svingos, Sotero; Brice, Donald; Garretson, Joel H; Schnoor, Jerald

2009-05-01

A poplar tree-phytoremediation system was installed at former refinery and tank farm sites in Cabin Creek, West Virginia, to cleanup petroleum-contaminated-soils and groundwater. Groundwater and soils in both sites were sampled and analyzed on a regular basis to monitor changes in contaminant concentration since 1999. The concentration of benzene, toluene, ethylbenzene, xylene, and gasoline range organics (GRO) decreased an average of 81%, 90%, 67%, 78%, and 82%, respectively, in the lower soil horizons and 34%, 84%, 12%, 19%, and 59%, respectively, in groundwater. In addition, concentrations of oxygen, methane, and carbon dioxide in soil gas demonstrated that tree roots dewatered soils and allowed penetration of oxygen deep into the soil profile, creating necessary conditions for rhizosphere bioremediation. Although required clean-up time can limit phytoremediation, it has proven to be a cost-effective strategy for site improvement if imminent pathways for human exposure and risk are not an issue.

Simple determination of aflatoxins in rice by ultra-high performance liquid chromatography coupled to chemical post-column derivatization and fluorescence detection.

PubMed

Huertas-Pérez, José Fernando; Arroyo-Manzanares, Natalia; Hitzler, Dominik; Castro-Guerrero, Francisco Germán; Gámiz-Gracia, Laura; García-Campaña, Ana M

2018-04-15

A fast and simple analytical method was developed and characterized for the determination of aflatoxins (B 1 , B 2 , G 1 and G 2 ) in rice. The procedure is based on a simple solid-liquid extraction without further clean-up, and analysis by ultra-high performance liquid chromatography coupled with fluorescence detection. Fluorescence emission of aflatoxins B 1 and G 1 was enhanced by post-column chemical derivatization using pyridinium bromide perbromide. The analytical method was satisfactorily characterized in white and brown rice. Under optimum conditions, external calibration in solvent could be used for quantification purposes and limits of quantification were below the maximum contents established by the European Union regulation for these contaminants/commodity group combination (0.07-0.14 µg/kg for white rice and 0.20-0.28 µg/kg for brown rice). Recovery studies carried out at three different concentration levels (0.5, 2 and 5 µg/kg) showed values in the range of 84.5-105.3%, and RSDs ≤ 5%. Copyright © 2017 Elsevier Ltd. All rights reserved.

Evaluation of a modified QuEChERS extraction of multiple classes of pesticides from a rice paddy soil by LC-APCI-MS/MS.

PubMed

Caldas, Sergiane S; Bolzan, Cátia M; Cerqueira, Maristela B; Tomasini, Débora; Furlong, Eliana B; Fagundes, Carlos; Primel, Ednei G

2011-11-23

A new method for the determination of clomazone, fipronil, tebuconazole, propiconazole, and azoxystrobin in samples of rice paddy soil is presented. The extraction of the pesticides from soil samples was performed by using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. Some extraction conditions such as salt addition, sample acidification, use of buffer, and cleanup step were evaluated. The optimized method dealt with a single extraction of the compounds under study with acidified acetonitrile, followed by the addition of MgSO(4) and NaCl prior to the final determination by liquid chromatography-atmospheric chemical pressure ionization-tandem mass spectrometry. Validation studies were carried out in soil samples. Recoveries of the spiked samples ranged between 70.3 and 120% with relative standard deviation lower than 18.2%. The limits of quantification were between 10 and 50 μg kg(-1). The method was applied to the analysis of real samples of soils where rice is cultivated.

The analysis of carbohydrates in milk powder by a new "heart-cutting" two-dimensional liquid chromatography method.

PubMed

Ma, Jing; Hou, Xiaofang; Zhang, Bing; Wang, Yunan; He, Langchong

2014-03-01

In this study, a new"heart-cutting" two-dimensional liquid chromatography method for the simultaneous determination of carbohydrate contents in milk powder was presented. In this two dimensional liquid chromatography system, a Venusil XBP-C4 analysis column was used in the first dimension ((1)D) as a pre-separation column, a ZORBAX carbohydrates analysis column was used in the second dimension ((2)D) as a final-analysis column. The whole process was completed in less than 35min without a particular sample preparation procedure. The capability of the new two dimensional HPLC method was demonstrated in the determination of carbohydrates in various brands of milk powder samples. A conventional one dimensional chromatography method was also proposed. The two proposed methods were both validated in terms of linearity, limits of detection, accuracy and precision. The comparison between the results obtained with the two methods showed that the new and completely automated two dimensional liquid chromatography method is more suitable for milk powder sample because of its online cleanup effect involved. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

Determination of alkylphenol and alkylphenolethoxylates in biota by liquid chromatography with detection by tandem mass spectrometry and fluorescence spectroscopy

USGS Publications Warehouse

Schmitz-Afonso, I.; Loyo-Rosales, J.E.; de la Paz Aviles, M.; Rattner, B.A.; Rice, C.P.

2003-01-01

A quantitative method for the simultaneous determination of octylphenol, nonylphenol and the corresponding ethoxylates (1 to 5) in biota is presented. Extraction methods were developed for egg and fish matrices based on accelerated solvent extraction followed by a solid-phase extraction cleanup, using octadecylsilica or aminopropyl cartridges. Identification and quantitation were accomplished by liquid chromatography-electrospray tandem mass spectrometry (LC-MS-MS) and compared to the traditional liquid chromatography with fluorescence spectroscopy detection. LC-MS-MS provides high sensitivity and specificity required for these complex matrices and an accurate quantitation with the use of 13C-labeled internal standards. Quantitation limits by LC-MS-MS ranged from 4 to 12 ng/g in eggs, and from 6 to 22 ng/g in fish samples. These methods were successfully applied to osprey eggs from the Chesapeake Bay and fish from the Great Lakes area. Total levels found in osprey egg samples were up to 18 ng/g wet mass and as high as 8.2 ug/g wet mass in the fish samples.

Identification of Proteins and Peptide Biomarkers for Detecting Banned Processed Animal Proteins (PAPs) in Meat and Bone Meal by Mass Spectrometry.

PubMed

Marbaix, Hélène; Budinger, Dimitri; Dieu, Marc; Fumière, Olivier; Gillard, Nathalie; Delahaut, Philippe; Mauro, Sergio; Raes, Martine

2016-03-23

The outbreak of bovine spongiform encephalopathy (BSE) in the United Kingdom in 1986, with processed animal proteins (PAPs) as the main vector of the disease, has led to their prohibition in feed. The progressive release of the feed ban required the development of new analytical methods to determine the exact origin of PAPs from meat and bone meal. We set up a promising MS-based method to determine the species and the source (legal or not) present in PAPs: a TCA-acetone protein extraction followed by a cleanup step, an in-solution tryptic digestion of 5 h (with a 1:20 protein/trypsin ratio), and mass spectrometry analyses, first without any a priori, with a Q-TOF, followed by a targeted triple-quadrupole analysis. Using this procedure, we were able to overcome some of the major limitations of the official methods to analyze PAPs, detecting and identifying prohibited animal products in feedstuffs by the monitoring of peptides specific for cows, pigs, and sheep in PAPs.

Determination of Fusarium toxins in functional vegetable milks applying salting-out-assisted liquid-liquid extraction combined with ultra-high-performance liquid chromatography tandem mass spectrometry.

PubMed

Hamed, Ahmed M; Arroyo-Manzanares, Natalia; García-Campaña, Ana M; Gámiz-Gracia, Laura

2017-11-01

Vegetable milks are considered as functional foods due to their physiological benefits. Although the consumption of these products has significantly increased, they have received little attention in legislation with regard to contaminants. However, they may contain mycotoxins resulting from the use of contaminated raw materials. In this work, ultra-high-performance liquid chromatography tandem mass spectrometry has been proposed for the determination of the most relevant Fusarium toxins (fumonisin B 1 and B 2 , HT-2 and T-2 toxins, zearalenone, deoxynivalenol and fusarenon-X) in different functional beverages based on cereals, legumes and seeds. Sample treatment consisted of a simple salting-out-assisted liquid-liquid extraction with no further clean-up. The method provided limits of quantification between 3.2 and 57.7 µg L -1 , recoveries above 80% and precision with RSD lower than 12%. The method was also applied for studying the occurrence of these mycotoxins in market samples of vegetable functional beverages and deoxynivalenol was found in three oat-based commercial drinks.

Development and validation of a capillary electrophoresis method for the determination of codeine, diphenhydramine, ephedrine and noscapine in pharmaceuticals.

PubMed

Gomez, María R; Sombra, Lorena; Olsina, Roberto A; Martínez, Luis D; Silva, María F

2005-01-01

The present work describes a simple, accurate and rapid method for the separation and simultaneous determination of codeine, diphenhydramine, ephedrine and noscapine present in cough-cold syrup formulations by capillary zone electrophoresis. Factors affecting the separation were the buffer pH and concentration, applied voltage, and presence of additives. Separations were carried out in less than 10 min with a 20 mM sodium tetraborate buffer, pH 8.50. The carrier electrolyte gave baseline separation with good resolution, great reproducibility and accuracy. Calibration plots were linear over at least three orders of magnitude of analyte concentrations, the lower limits of detection being within the range 0.42-1.33 microg ml(-1). Detection was performed by UV absorbance at wavelengths of 205 and 250 nm. Quantification of the components in actual syrup formulations was calculated against the responses of freshly prepared external standard solutions. The method was validated and met all analysis requirements of quality assurance and quality control. The procedure was fast and reliable and commercial pharmaceuticals could be analyzed without prior sample clean-up procedure.

Simultaneous Determination of Fluoroquinolones and Sulfonamides Originating from Sewage Sludge Compost

PubMed Central

Herodes, K.

2017-01-01

A simultaneous method for quantitative determination of traces of fluoroquinolones (FQs) and sulfonamides (SAs) in edible plants fertilized with sewage sludge was developed. The compounds were extracted from the plants by rapid and simple liquid extraction followed by extracts clean-up using solid phase extraction. The eluent additive 1,1,1,3,3,3-hexafluoro-2-propanol was used for liquid chromatographic detection to achieve separation of structurally similar antimicrobials like ciprofloxacin and norfloxacin. Identification and quantification of the compounds were performed using high-performance liquid chromatography with electrospray ionization mass spectrometry in selected reaction monitoring mode. Method was validated and extraction recoveries of FQs and SAs ranged from 66% to 93%. The limit of quantifications was from 5 ng/g in the case of ofloxacin to 40 ng/g for norfloxacin. The method precision ranged from 1.43% to 2.61%. The developed novel method was used to evaluate the plats antimicrobial uptake (potato (Solanum tuberosum L.), carrot (Daucus carota L.), lettuce (Lactuca sativa L.), and wheat (Triticum vulgare L.)) from soil and migration of the analytes inside the plants. PMID:28695191

Purification of Derivatized Oligosaccharides by Solid Phase Extraction for Glycomic Analysis

PubMed Central

Zhang, Qiwei; Li, Henghui; Feng, Xiaojun; Liu, Bi-Feng; Liu, Xin

2014-01-01

Profiling of glycans released from proteins is very complex and important. To enhance the detection sensitivity, chemical derivatization is required for the analysis of carbohydrates. Due to the interference of excess reagents, a simple and reliable purification method is usually necessary for the derivatized oligosaccharides. Various SPE based methods have been applied for the clean-up process. To demonstrate the differences among these methods, seven types of self-packed SPE cartridges were systematically compared in this study. The optimized conditions were determined for each type of cartridge and it was found that microcrystalline cellulose was the most appropriate SPE material for the purification of derivatized oligosaccharide. Normal phase HPLC analysis of the derivatized maltoheptaose was realized with a detection limit of 0.12 pmol (S N−1 = 3) and a recovery over 70%. With the optimized SPE method, relative quantification analysis of N-glycans from model glycoproteins were carried out accurately and over 40 N-glycans from human serum samples were determined regardless of the isomers. Due to the high stability and sensitivity, microcrystalline cellulose cartridge showed potential applications in glycomics analysis. PMID:24705408

Method validation for the determination of ochratoxin A in green and soluble coffee by immunoaffinity column cleanup and liquid chromatography.

PubMed

Diaz, G J; Ariza, D; Perilla, N S

2004-06-01

A method was validated for the determination of ochratoxin A (OTA) in soluble and green coffee. Performance parameters evaluated included selectivity, accuracy, intermediate precision, linearity, limit of detection, limit of quantitation, and ruggedness. The method was found to be selective for OTA in both matrices tested. Recovery rates from soluble coffee samples ranged from 73.5 to 91.2%, and from green coffee samples from 68.7 to 84.5%. The intermediate precision (RSDr) was between 9.1 and 9.4% for soluble coffee and between 14.3 and 15.5% for green coffee analysis. The linearity of the standard calibration curve (r(2)) was <0.999 for OTA levels of 1.0-20.0 μg/kg in coffee samples. The limit of detection was determined to be 0.01 ng of OTA on column, while the limit of quantitation was found to be 0.03 ng on column. The limit of quantitation is equivalent to 0.6 μg/kg in soluble coffee samples and 0.3 μg/kg in green coffee samples. The results of the ruggedness trial showed two factors are critical for soluble coffee analysis: the extraction method, and the flow rate of the mobile phase. For green coffee analysis two critical factors detected were the extraction method and the storage temperature of the immunoaffinity column.Five samples of soluble coffee and 42 of green coffee were analysed using the validated method. All soluble coffee samples contained OTA at levels that ranged from 8.4 to 13.9 μg/kg. Six of the 42 green coffee samples analysed (14.3%) contained OTA at levels ranging from 0.9 to 19.4 μg/kg. The validated method can be used to monitor OTA levels in Colombian coffee for export or for local consumption.

Cleanups In My Community (CIMC) - Recovery Act Funded Cleanups, National Layer

EPA Pesticide Factsheets

This data layer provides access to Recovery Act Funded Cleanup sites as part of the CIMC web service. The American Recovery and Reinvestment Act was signed into law by President Obama on February 17th, 2009 and all reporting on ARRA for these 3 programs was complete as of 2013. Out of the five EPA programs that distributed recovery act funding, three of them were cleanup programs: Brownfields, Superfund and Leaking Underground Storage Tanks. CIMC provides information on site cleanups that received ARRA Recovery Act funding for Superfund and Brownfields, but not Leaking Underground Storage Tanks. Data for Brownfields came from the ACRES database. Data for Superfund came from the Comprehensive Environmental Response, Compensation, and Liability Information System (CERCLIS) database. Data in CIMC no longer need to be updated for the ARRA program. For information on all EPA Recovery Act funded work, please see: http://archive.epa.gov/recovery/web/html/ and http://epamap17.epa.gov/arra/.

Mature B-cell neoplasms in Chernobyl clean-up workers of 1986-1987: summary of cytomorphological and immunocytochemical study in 25 years after Chernobyl accident.

PubMed

Gluzman, D F; Sklyarenko, L M; Nadgornaya, V A; Zavelevich, M P

2011-03-01

The data on the verified cases of mature B-cell neoplasms (chronic lymphocytic leukemia - CLL, B-prolymphocytic leukemia, non-Hodgkin's lymphoma in leukemization phase and multiple myeloma - MM; 146 cases in total) in the consecutive group of Ukrainian clean-up workers within 10-25 years after Chernobyl accident are summarized. B-cell neoplasms represent the most prevalent group among all diagnosed neoplasms of hematopoietic and lymphoid tissues in clean-up worker patients under study (49.4%). MM percentage in the patients of Chernobyl clean-up worker group turned out to be significantly higher than in the patients of the general populations studied at the same period. While the percentage of B-CLL is similar in clean-up worker patients and patients of general population, the trend towards younger age of patients with mature B-cell neoplasms in clean-up worker group is evident. The current concepts on the possible association between mature B-cell neoplasms (mainly B-CLL) and radiation exposure are briefly outlined. Only the precise diagnosis of hematopoietic malignancies combining with large-scale analytical epidemiological studies with careful dose assessment and long-term follow-up may represent the basis for resolving the question whether mature B-cell neoplasms may be radiogenic.

Extent and Degree of Shoreline Oiling: Deepwater Horizon Oil Spill, Gulf of Mexico, USA

PubMed Central

Michel, Jacqueline; Owens, Edward H.; Zengel, Scott; Graham, Andrew; Nixon, Zachary; Allard, Teresa; Holton, William; Reimer, P. Doug; Lamarche, Alain; White, Mark; Rutherford, Nicolle; Childs, Carl; Mauseth, Gary; Challenger, Greg; Taylor, Elliott

2013-01-01

The oil from the 2010 Deepwater Horizon spill in the Gulf of Mexico was documented by shoreline assessment teams as stranding on 1,773 km of shoreline. Beaches comprised 50.8%, marshes 44.9%, and other shoreline types 4.3% of the oiled shoreline. Shoreline cleanup activities were authorized on 660 km, or 73.3% of oiled beaches and up to 71 km, or 8.9% of oiled marshes and associated habitats. One year after the spill began, oil remained on 847 km; two years later, oil remained on 687 km, though at much lesser degrees of oiling. For example, shorelines characterized as heavily oiled went from a maximum of 360 km, to 22.4 km one year later, and to 6.4 km two years later. Shoreline cleanup has been conducted to meet habitat-specific cleanup endpoints and will continue until all oiled shoreline segments meet endpoints. The entire shoreline cleanup program has been managed under the Shoreline Cleanup Assessment Technique (SCAT) Program, which is a systematic, objective, and inclusive process to collect data on shoreline oiling conditions and support decision making on appropriate cleanup methods and endpoints. It was a particularly valuable and effective process during such a complex spill. PMID:23776444

Science plus management equals successful remediation -- A case study

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

Buehlman, M.D.; Rogers, D.T.; Payne, F.C.

In the past, owners of contaminated sites attempted to remediate as quickly as possible, usually by excavating contaminated soil or pumping and treating contaminated groundwater. Often, they started remediation before identifying all potential types and sources of contaminants, and before conducting a thorough hydrogeologic study. Such premature action usually resulted in the selected remedy not working, the contamination spreading, or unnecessary remedial activities. Today, successful site remediation is recognized as a complex and time-consuming undertaking--requiring a combination of careful scientific study, effective negotiation with the regulatory agencies and skillful management of multidisciplinary efforts. A case study involving a Brownfields sitemore » in southeastern Michigan clearly illustrates the elements of successful remediation. The site`s soil was contaminated with polychlorinated biphenyls (PCBs) and its groundwater with a variety of chlorinated solvents. The original estimate for remediation had exceeded $30 million. Several phases of investigation were conducted to evaluate the nature and sources of contaminants, the site`s hydrogeology, potential risks to human health and the environment, and feasible remedial technologies. Multiple cleanup criteria were established for different affected areas based on the results of the investigations, changes that were taking place with the state cleanup regulations and standards and subsequent negotiations with state and federal regulators. Innovative remedial technologies were selected. The result was a remediation that met or exceeded all soil and groundwater cleanup objectives, was performed on schedule, and was highly cost-effective. The final cost was limited to $3 million--one-tenth of the original estimate.« less

Solutions Network Formulation Report. Landsat Data Continuity Mission Simulated Data Products for Bureau of Land Management and Environmental Protection Agency Abandoned Mine Lands Decision Support

NASA Technical Reports Server (NTRS)

Estep, Leland

2007-01-01

Presently, the BLM (Bureau of Land Management) has identified a multitude of abandoned mine sites in primarily Western states for cleanup. These sites are prioritized and appropriate cleanup has been called in to reclaim the sites. The task is great in needing considerable amounts of agency resources. For instance, in Colorado alone there exists an estimated 23,000 abandoned mines. The problem is not limited to Colorado or to the United States. Cooperation for reclamation is sought at local, state, and federal agency level to aid in identification, inventory, and cleanup efforts. Dangers posed by abandoned mines are recognized widely and will tend to increase with time because some of these areas are increasingly used for recreation and, in some cases, have been or are in the process of development. In some cases, mines are often vandalized once they are closed. The perpetrators leave them open, so others can then access the mines without realizing the danger posed. Abandoned mine workings often fill with water or oxygen-deficient air and dangerous gases following mining. If the workings are accidentally entered into, water or bad air can prove fatal to those underground. Moreover, mine residue drainage negatively impacts the local watershed ecology. Some of the major hazards that might be monitored by higher-resolution satellites include acid mine drainage, clogged streams, impoundments, slides, piles, embankments, hazardous equipment or facilities, surface burning, smoke from underground fires, and mine openings.

Major factors affecting in situ biodegradation rates of jet-fuel during large-scale biosparging project in sedimentary bedrock.

PubMed

Machackova, Jirina; Wittlingerova, Zdena; Vlk, Kvetoslav; Zima, Jaroslav

2012-01-01

Biodegradation of petroleum hydrocarbons (TPH), mainly jet fuel, had taken place at the former Soviet Army air base in the Czech Republic. The remediation of large-scale petroleum contamination of soil and groundwater has provided valuable information about biosparging efficiency in the sandstone sedimentary bedrock. In 1997 petroleum contamination was found to be present in soil and groundwater across an area of 28 hectares, divided for the clean-up purpose into smaller clean-up fields (several hectares). The total estimated quantity of TPH released to the environment was about 7,000 metric tons. Biosparging was applied as an innovative clean-up technology at the site and was operated over a 10-year period (1997-2008). Importance of a variety of factors that affect bacterial activity in unsaturated and saturated zones was widely studied on the site and influence of natural and technological factors on clean-up efficiency in heavily contaminates areas of clean-up fields (initial contaminant mass 111-452 metric ton/ha) was evaluated. Long-term monitoring of the groundwater temperature has shown seasonal rises and falls of temperature which have caused a fluctuation in biodegradation activity during clean-up. By contrast, an overall rise of average groundwater temperature was observed in the clean-up fields, most probably as a result of the biological activity during the clean-up process. The significant rise of biodegradation rates, observed after air sparging intensification, and strong linear correlation between the air injection rates and biodegradation activities have shown that the air injection rate is the principal factor in biodegradation efficiency in heavily contaminated areas. It has a far more important role for achieving a biodegradation activity than the contamination content which appeared to have had only a slight effect after the removal of about 75% of initial contamination.

Simultaneous determination of neonicotinoid insecticides in human serum and urine using diatomaceous earth-assisted extraction and liquid chromatography-tandem mass spectrometry.

PubMed

Yamamuro, Tadashi; Ohta, Hikoto; Aoyama, Mika; Watanabe, Daisuke

2014-10-15

A rapid and sensitive analytical method was developed for simultaneous determination of eight neonicotinoid insecticides (acetamiprid, clothianidin, dinotefuran, flonicamid, imidacloprid, nitenpyram, thiacloprid and thiamethoxam) and three specific metabolites of acetamiprid (N-desmethylacetamiprid, 5-(N-acetyl-N-methylaminomethyl)-2-chloropyridine and 5-(N-acetylaminomethyl)-2-chloropyridine) in human serum and urine. A diatomaceous earth-assisted extraction using Extrelut NT3 column with chloroform/2-propanol (3:1, v/v) as eluent was selected for the single step cleanup procedure for all the target compounds. Qualitative and quantitative analyses were conducted by liquid chromatography-tandem mass spectrometry with multiple reaction monitoring mode. The limits of detection and the limits of quantification of eleven compounds were in the ranges of 0.1-0.2ng/mL and 0.5-10ng/mL for serum, 0.1-1ng/mL and 1-10ng/mL for urine, respectively. The extraction recoveries were between 80.9% and 101.8% for serum samples, 91.9% and 106% for urine samples. The intra-day RSDs and the inter-day RSDs were less than 11.5% and 13.2% for serum, less than 8.3% and 8.8% for urine. The proposed procedure will be suitable for forensic investigations of human poisoning cases with neonicotinoid insecticides. This is the first report of simultaneous determination of eight neonicotinoids in serum and urine samples. Copyright © 2014. Published by Elsevier B.V.

Rapid determination of some psychotropic drugs in complex matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

PubMed

Asghari, Alireza; Fahimi, Ebrahim; Bazregar, Mohammad; Rajabi, Maryam; Boutorabi, Leila

2017-05-01

Simple and rapid determinations of some psychotropic drugs in some pharmaceutical wastewater and human plasma samples were successfully accomplished via the tandem dispersive liquid-liquid microextraction combined with high performance liquid chromatography-ultraviolet detection (TDLLME-HPLC-UV). TDLLME of the three psychotropic drugs clozapine, chlorpromazine, and thioridazine was easily performed through two consecutive dispersive liquid-liquid microextractions. By performing this convenient method, proper sample preconcentrations and clean-ups were achieved in just about 7min. In order to achieve the best extraction efficiency, the effective parameters involved were optimized. The optimal experimental conditions consisted of 100μL of CCl 4 (as the extraction organic solvent), and the pH values of 13 and 2 for the donor and acceptor phases, respectively. Under these optimum experimental conditions, the proposed TDLLME-HPLC-UV technique provided a good linearity in the range of 5-3000ngmL -1 for the three psychotropic drugs with the correlation of determinations (R 2 s) higher than 0.996. The limits of quantification (LOQs) and limits of detection (LODs) obtained were 5.0ngmL -1 and 1.0-1.5ngmL -1 , respectively. Also the proper enrichment factors (EFs) of 96, 99, and 88 for clozapine, chlorpromazine, and thioridazine, respectively, and good extraction repeatabilities (relative standard deviations below 9.3%, n=5) were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

Simultaneous determination of eugenol, isoeugenol and methyleugenol in fish fillet using gas chromatography coupled to tandem mass spectrometry.

PubMed

Ke, Changliang; Liu, Qi; Li, Liudong; Chen, Jiewen; Wang, Xunuo; Huang, Ke

2016-09-15

Gas chromatography (GC) coupled with triple quadrupole tandem mass spectrometry (MS/MS) operated in electron ionization mode (EI) has been shown to have advantages in the trace analysis of chemical compounds. Employing the instrument, a method has been built to simultaneously determine eugenol, isoeugenol' and methyleugenol, which have been widely used as fish anesthetic, in the fish fillet. Procedure for the sample preparation was achieved by using hexane extraction followed by phenyl solid phase extraction (SPE) cleanup, which was free of such steps as rotary evaporation and nitrogen blowing by taking the volatility of eugenol and its isomers into consideration. The method was validated by conducting recovery studies on fortified fish fillet samples at four concentrations. The linearity in the range of 5-500μg·L(-1) was forced through the origin giving a coefficient of determination (r(2)) greater than 0.9982. Limits of detection (LODs) for eugenol, isoeugenol' and methyleugenol were 0.4, 1.2' and 0.2μg·kg(-1), respectively. The limits of quantification (LOQs) were 1.2, 4' and 0.7μg·kg(-1) for eugenol, isoeugenol' and methyleugenol, respectively. The recoveries for eugenol and its isomers ranged from 76.4 to 99.9% with relative standard deviations (RSD) in a range from 2.18 to 15.5%. This method is quick, simple and suitable for determining the residues of eugenol, isoeugenol and methyleugenol simultaneously in batch samples of fish fillet. Copyright © 2016 Elsevier B.V. All rights reserved.

NUCLEAR CLEANUP: Progress Made at Rocky Flats, but Closure by 2006 Is Unlikely, and Costs May Increase

DTIC Science & Technology

2001-02-01

liquids or residues from process pipes and tanks. The contractor also dismantled plutonium - processing furnaces, stripped out contaminated process...Soil Cleanup Levels on the Scope and Cost of the 903 Pad Cleanup 30 Figures Figure 1: Workers in Protective Clothing Handling Plutonium - Contaminated ...activities—shipping nuclear materials such as plutonium - contaminated metals and powders—is expected to be completed in 2002. Another activity

Reactor water cleanup system

DOEpatents

Gluntz, D.M.; Taft, W.E.

1994-12-20

A reactor water cleanup system includes a reactor pressure vessel containing a reactor core submerged in reactor water. First and second parallel cleanup trains are provided for extracting portions of the reactor water from the pressure vessel, cleaning the extracted water, and returning the cleaned water to the pressure vessel. Each of the cleanup trains includes a heat exchanger for cooling the reactor water, and a cleaner for cleaning the cooled reactor water. A return line is disposed between the cleaner and the pressure vessel for channeling the cleaned water thereto in a first mode of operation. A portion of the cooled water is bypassed around the cleaner during a second mode of operation and returned through the pressure vessel for shutdown cooling. 1 figure.

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.

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

Dowell, Jonathan; Franco, Joe

The discussion of Hanford's River Corridor will cover work that has already been completed plus the work remaining to be done. This includes the buildings, waste sites, and groundwater plumes in the 300 Area; large-scale burial ground remediation in the 600 Area; plutonium production reactor dismantling and 'cocooning' along the river; preservation of the world's first full-scale plutonium production reactor; removal of more than 14 million tons of contaminated soil and debris along the Columbia River shoreline and throughout the River Corridor; and the excavation of buried waste sites in the river shore area. It also includes operating an EPA-permittedmore » low-level waste disposal facility in the central portion of the site. At the completions of cleanup in 2015, Hanford's River Corridor will be the largest closure project ever completed by the Department of Energy. Cleanup of the River Corridor has been one of Hanford's top priorities since the early 1990's. This urgency has been due to the proximity of hundreds of waste sites to the Columbia River. In addition, removal of the sludge from K West Basin, near the river, remains a high priority. This 220-square-mile area of the Hanford Site sits on the edge of the last free-flowing stretch of the Columbia River. The River Corridor portion of the Hanford Site includes the 100 and 300 Areas along the south shore of the Columbia River. The 100 Areas contain nine retired plutonium production reactors. These areas are also the location of numerous support facilities and solid and liquid waste disposal sites that have contaminated groundwater and soil. The 300 Area, located just north of the city of Richland, contains fuel fabrication facilities, nuclear research and development facilities, and their associated solid and liquid waste disposal sites that have contaminated groundwater and soil. In order to ensure that cleanup actions address all threats to human health and the environment, the River Corridor includes the adjacent areas that extend from the 100 Area and 300 Area to the Central Plateau. For sites in the River Corridor, remedial actions are expected to restore groundwater to drinking water standards and ensure that aquatic life in the Columbia River is protected by achieving ambient water quality standards. It is intended that these objectives be achieved, unless technically impracticable, within a reasonable timeframe. In those instances where remedial action objectives are not achievable in a reasonable time frame, or are determined to be technically impracticable, programs are being implemented to contain the plume, prevent exposure to contaminated groundwater, and evaluate further risk reduction opportunities as new technologies become available. River Corridor cleanup work also removes potential sources of contamination, which are close to the Columbia River, and places them on the Central Plateau for final disposal. The intent is to shrink the footprint of active cleanup to within the 75-square- mile area of the Central Plateau by removing excess facilities and remediating waste sites. Cleanup actions are supporting anticipated future land uses consistent with the Hanford Reach National Monument, where applicable, and the Hanford Comprehensive Land- Use Plan (DOE 1999). The River Corridor has been divided into six geographic decision areas to achieve source and groundwater remedy decisions. These decisions will provide comprehensive coverage for all areas within the River Corridor and will incorporate ongoing interim action cleanup activities. Cleanup levels will be achieved in order to support anticipated future land uses of conservation and preservation for most of this area and industrial use for the 300 Area. At the conclusion of cleanup actions, the federal government will implement long-term stewardship activities to ensure protection of human health and the environment. (authors)« less

Solid phase extraction with high polarity Carb/PSA as composite fillers prior to UPLC-MS/MS to determine six bisphenols and alkylphenols in trace level hotpot seasoning.

PubMed

Dong, Hao; Zeng, Xiaofang; Bai, Weidong

2018-08-30

The present study reports an ultra high-performance liquid chromatography tandem mass spectrometry method for the simultaneous determination of six bisphenols (bisphenol A, bisphenol B and bisphenol F) and alkylphenols (4-nonylphenol, 4-n-nonylphenol and octylphenol) in hotpot seasoning. Samples were dispersed in n-hexane after addition of internal standards bisphenol A-d 4 and 4-n-nonylphenol-d 4 . Sample solutions were then centrifuged, and the supernatants purified using solid phase extraction with high polarity Carb/PSA composite fillers. Six target analytes were separated on a Waters ACQUITY BEH C18 column by gradient elution with methanol and 0.05% ammonium hydroxide in water as the mobile phase, and determined under multiple reactions monitoring mode. The limits of detection and quantitation, matrix effect, recovery and precision of the method were investigated. Results were linear in the concentration range 0.1-250 µg/L for all compounds of interest, with R 2  > 0.9950. Limits of detection were in the range 0.1-0.4 μg/kg, and limits of quantitation were between 0.5 μg/kg and 1.0 μg/kg. The mean recoveries for negative samples at three spiked concentrations were in the range 87.9%-102.4%, and the intra-day precision and inter-day precision were in the ranges 2.1-8.2% and 4.8-11.2%, respectively. This method is accurate and sensitive, and had good clean-up characteristics, which might apply to screening and quantitation of target bisphenols and alkylphenols in hotpot seasoning. Copyright © 2018 Elsevier Ltd. All rights reserved.

Detection of β-Lactams and Chloramphenicol Residues in Raw Milk-Development and Application of an HPLC-DAD Method in Comparison with Microbial Inhibition Assays.

PubMed

Karageorgou, Eftychia; Christoforidou, Sofia; Ioannidou, Maria; Psomas, Evdoxios; Samouris, Georgios

2018-06-01

The present study was carried out to assess the detection sensitivity of four microbial inhibition assays (MIAs) in comparison with the results obtained by the High Performance Liquid Chromatography with Diode-Array Detection (HPLC-DAD) method for antibiotics of the β-lactam group and chloramphenicol in fortified raw milk samples. MIAs presented fairly good results when detecting β-lactams, whereas none were able to detect chloramphenicol at or above the permissible limits. HPLC analysis revealed high recoveries of examined compounds, whereas all detection limits observed were lower than their respective maximum residue limits (MRL) values. The extraction and clean-up procedure of antibiotics was performed by a modified matrix solid phase dispersion procedure using a mixture of Plexa by Agilent and QuEChERS as a sorbent. The HPLC method developed was validated, determining the accuracy, precision, linearity, decision limit, and detection capability. Both methods were used to monitor raw milk samples of several cows and sheep, obtained from producers in different regions of Greece, for the presence of examined antibiotic residues. Results obtained showed that MIAs could be used effectively and routinely to detect antibiotic residues in several milk types. However, in some cases, spoilage of milk samples revealed that the kits' sensitivity could be strongly affected, whereas this fact does not affect the effectiveness of HPLC-DAD analysis.

A Systems Engineering Analysis of Unmanned Maritime Systems for U.S. Coast Guard Missions

DTIC Science & Technology

2013-06-01

accidental, are apparent when considering the Fukushima Daiichi nuclear disaster and its follow -on radiation hazards [52]. In addition, recent increases in...on the maritime domain increases innovative approaches such as UMS will be vital in gaining awareness , especially in remote locations such as the...Horizon oil disaster clean-up employed a limited use of UMS, specifically Remotely Op- erated Vehicles [20]. As oil drilling increases throughout the

Recent advances in analytical methods for the determination of 4-alkylphenols and bisphenol A in solid environmental matrices: A critical review.

PubMed

Salgueiro-González, N; Castiglioni, S; Zuccato, E; Turnes-Carou, I; López-Mahía, P; Muniategui-Lorenzo, S

2018-09-18

The problem of endocrine disrupting compounds (EDCs) in the environment has become a worldwide concern in recent decades. Besides their toxicological effects at low concentrations and their widespread use in industrial and household applications, these pollutants pose a risk for non-target organisms and also for public safety. Analytical methods to determine these compounds at trace levels in different matrices are urgently needed. This review critically discusses trends in analytical methods for well-known EDCs like alkylphenols and bisphenol A in solid environmental matrices, including sediment and aquatic biological samples (from 2006 to 2018). Information about extraction, clean-up and determination is covered in detail, including analytical quality parameters (QA/QC). Conventional and novel analytical techniques are compared, with their advantages and drawbacks. Ultrasound assisted extraction followed by solid phase extraction clean-up is the most widely used procedure for sediment and aquatic biological samples, although softer extraction conditions have been employed for the latter. The use of liquid chromatography followed by tandem mass spectrometry has greatly increased in the last five years. The majority of these methods have been employed for the analysis of river sediments and bivalve molluscs because of their usefulness in aquatic ecosystem (bio)monitoring programs. Green, simple, fast analytical methods are now needed to determine these compounds in complex matrices. Copyright © 2018 Elsevier B.V. All rights reserved.

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

Residue analysis of sixty pesticides in red swamp crayfish using QuEChERS with high-performance liquid chromatography-tandem mass spectrometry

USDA-ARS?s Scientific Manuscript database

In this study, a multi-residue analytical method using QuEChERS extraction and dispersive solid-phase extraction (d-SPE) cleanup followed by high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/MS) was developed for rapid determination of 60 pesticide residues in whole crayfish a...

A Summary and Perspective of Recent IRIS Assessments and Impact on Planning Environmental Investigations

DTIC Science & Technology

2011-03-30

or remediation  Used with regulatory values to determine cleanup levels  Risk-based screening levels (aka PRGs, RBCs, RSLs) ►Screen sites early in...Final IRIS Values for Hydrogen Cyanide and Cyanide Salts (September 2010)  New Oral noncancer RfD = 0.0006 mg/kg- day; male reproduction effects

Immunoaffinity column cleanup with liquid chromatography using postcolumn bromination for the determination of aflatoxins in black and white sesame seed: single-laboratory validation.

PubMed

Liu, Guihua; Zhu, Zhou; Cheng, Jinquan; Senyuva, Hamide Z

2012-01-01

A single-laboratory validation was conducted to establish the effectiveness of an immunoaffinity column cleanup procedure followed by LC with fluorescence detection for the determination of aflatoxins B1, B2, G1, and G2 in sesame seeds. The sample is homogenized with 50% water (w/w) to form a slurry, then the test portion is extracted with methanol-water (60 + 40, v/v) using a high-speed blender. The sample extract is filtered, diluted with 15% Tween 20 in phosphate-buffered saline solution, and applied to an immunoaffinity column. Aflatoxins are removed with neat methanol, then directly determined by RP-LC with fluorescence detection using postcolumn bromination (Kobra cell). Test portions of blank white sesame seed slurry were spiked with a mixture of aflatoxins to give total levels of 4 and 10 microg/kg. Recoveries for individual and total aflatoxins ranged from 92.7 to 110.3% for spiked samples. Based on results for spiked sesame paste (triplicates at two levels), the RSD for repeatability (RSD(r)) averaged 1.1% for total aflatoxins and 1.4% for aflatoxin B1. The method was demonstrated to be applicable to naturally contaminated samples of black and white sesame seeds obtained from local markets in China.

THE POSITIVE IMPACTS OF AMERICAN REINVESTMENT AND RECOVERY ACT (ARRA) FUNDING TO THE WASTE MANAGEMENT PROGRAM ON HANFORD'S PLATEAU REMEDIATION PROJECT

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

BLACKFORD LT

In April 2009, the Department of Energy (DOE) Richland Operations Office (RL) was allocated $1.6 billion (B) in ARRA funding to be applied to cleanup projects at the Hanford Site. DOE-RL selected projects to receive ARRA funding based on 3-criteria: creating/saving jobs, reducing the footprint of the Hanford Site, and reducing life-cycle costs for cleanup. They further selected projects that were currently covered under regulatory documents and existing prime contracts, which allowed work to proceed quickly. CH2M HILL Plateau Remediation Company (CHPRC) is a prime contractor to the DOE focused on the environmental cleanup of the DOE Hanford Site Centralmore » Plateau. CHPRC was slated to receive $1.36B in ARRA funding. As of January, 2010, CHPRC has awarded over $200 million (M) in subcontracts (64% to small businesses), created more that 1,100 jobs, and touched more than 2,300 lives - all in support of long-term objectives for remediation of the Central Plateau, on or ahead of schedule. ARRA funding is being used to accelerate and augment cleanup activities already underway under the baseline Plateau Remediation Contract (PRC). This paper details challenges and accomplishments using ARRA funding to meet DOE-RL objectives of creating/saving jobs, expediting cleanup, and reducing lifecycle costs for cleanup during the first months of implementation.« less

Residues levels of organochlorine pesticide in cow's milk from industrial farms in Hidalgo, Mexico.

PubMed

Gutierrez, Rey; Ortiz, Rutilio; Vega, Salvador; Schettino, Beatriz; Ramirez, Maria L; Perez, Jose J

2013-01-01

A survey was carried out from 2008 to 2010 to determine the concentrations of 16 organochlorine pesticide residues (OPRs) from Tizayuca, Hidalgo, Mexico. Organochlorine residue determinations were made from milk fat, using chromatographic cleanup and analysis by gas chromatography with an electron capture detector. The OPR concentrations found were from below the detection limit (DL) to 0.91 ng g(-1) in 2008, DL to 0.38 ng g(-1) in 2009 and DL to 0.59 ng g(-1) in 2010. In general concentrations of organochlorine pesticides were higher in the wet season (3.37 ng g(-1) and 4.79 ng g(-1)) than the dry season (1.92 ng g(-1) and 2.71 ng g(-1)) for 2009 and 2010, due to control of pests in the pasture and sheds. According to Codex Alimentarius regulations, individual pesticides did not exceed the permissible limits, which for example were 10 μg kg(-)1 for alpha hexachlorocyclohexane (HCH) and endosulfan I, 20 μg kg(-1) for p,p'-DDT, and 6 μg kg(-1) for dieldrin, endrin and heptachlor. A reduction of organochlorine pesticide concentrations in cow's milk was noted, indicating that the Mexican government has achieved reduction or elimination of some organochlorine pesticides in response to global agreements on persistent organic pollutants.

Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group; determination of glyphosate, aminomethylphosphonic acid, and glufonsinate in water using online solid-phase extraction and high-performance liquid chromat

USGS Publications Warehouse

Lee, E.A.; Strahan, A.P.; Thurman, E.M.

2001-01-01

An analytical method for the determination of glyphosate, its principal degradation compound, aminomethylphosphonic acid (AMPA), and glufosinate in water with varying matrices has been developed. Four different sample matrices fortified at 0.2 and 2.0 ?g/L (micrograms per liter) were analyzed using precolumn derivatization with 9-fluorenylmethylchloroformate (FMOC). After derivatization, cleanup and concentration were accomplished using automated online solid-phase extraction followed by elution with the mobile phase allowing for direct injection into a liquid chromatograph/mass spectrometer (LC/MS). Analytical conditions for MS detection were optimized, and quantitation was carried out using the following representative ions: 390 and 168 for glyphosate; 332, 110, and 136 for AMPA; and 402, 180, and 206 for glufosinate. Matrix effects were minimized by utilizing standard addition for quantification and an isotope-labeled glyphosate (2-13C,15N) as the internal standard. Method detection limits (MDLs) were 0.084 ?g/L for glyphosate, 0.078 ?g/L for AMPA, and 0.057 ?g/L for glufosinate. The method reporting limits (MRLs) were set at 0.1 ?g/L for all three compounds. The mean recovery values ranged from 88.0 to 128.7 percent, and relative standard deviation values ranged from 5.6 to 32.6 percent.

Quantitative determination of four nitrofuran metabolites in meat by isotope dilution liquid chromatography-electrospray ionisation-tandem mass spectrometry.

PubMed

Mottier, Pascal; Khong, Seu-Ping; Gremaud, Eric; Richoz, Janique; Delatour, Thierry; Goldmann, Till; Guy, Philippe A

2005-03-04

A confirmatory method based on isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the low-level determination of residues of four nitrofuran veterinary drugs in meat, e.g., furazolidone, furaltadone, nitrofurantoin, and nitrofurazone. The procedure entails an acid-catalysed release of protein-bound metabolites, followed by their in situ conversion into the 2-nitrobenzaldehyde (NBA) imine-type derivatives. Liquid-liquid extraction and clean-up on a polymeric solid phase extraction cartridge are then performed before LC-MS/MS analysis by positive electrospray ionisation (ESI) applying multiple reaction monitoring of three transition reactions for each compound. Reliable quantitation is obtained by using one deuterated analogue per analyte (d4-NBA derivative) as internal standard (IS). Validation of the method in chicken meat was conducted following the European Union (EU) criteria for the analysis of veterinary drug residues in foods. The decision limits (CCalpha) were 0.11-0.21 microg/kg, and the detection capabilities (CCbeta) 0.19-0.36 microg/kg, thus below the minimum required performance limit (MRPL) set at 1 microg/kg by the EU. The method is robust and suitable for routine quality control operations, and more than 200 sample injections were performed without excessive pollution of the mass spectrometer or loss of LC column performance.

Superfund Green Remediation

EPA Pesticide Factsheets

Green remediation is the practice of considering all environmental effects of site cleanup and incorporating options – like the use of renewable energy resources – to maximize the environmental benefits of cleanups.

Health complaints among subjects involved in oil cleanup operations during oil spillage from a Greek tanker "Tasman Spirit".

PubMed

Meo, Sultan Ayoub; Al-Drees, Abdul Majeed; Rasheed, Shahzad; Meo, Imran Mu; Al-Saadi, Muslim M; Ghani, Hamza A; Alkandari, Jasem Ramadan

2009-01-01

Oil spillage in the sea water is a disaster for marine life and humans in the vicinity. The study aimed at investigating health complaints among subjects involved in oil cleanup operations during a spillage from a Greek oil tanker "Tasman Spirit". The project was conducted under the supervision of the Department of Physiology, College of Medicine, King Khalid University Hospital, King Saud University, Riyadh, Saudi Arabia. The study concerned the respiratory and general health complaints in 50 apparently healthy, non-smoking male workers exposed to crude oil during oil cleanup operations. The exposed group was matched with a similar number of male, non-smoking controls. The health complaints were evaluated based on a comprehensive interview. The subjects involved in oil cleanup operations had significantly higher rates of health complaints including cough (38%), runny nose (36%), eye irritation/redness (32%), sore throat (28%), headache (28%), nausea (24%) and general illness (18%), compared to their matched controls. Air pollution due to crude oil spillage into sea water may cause respiratory and general health complaints in workers involved in oil cleanup operations.

Streamlining Site Cleanup in New York City

EPA Pesticide Factsheets

This joint effort, supported by the New York State Department of Environmental Conservation (NYS DEC), advances the environmental cleanup goals of PlaNYC 2030, the city's comprehensive sustainability plan.

TECHNICAL APPROACHES TO CHARACTERIZING AND ...

EPA Pesticide Factsheets

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 need to base assessment and cleanup activities on the conditions of the particular sites with which they are dealing. A site assessment strategy should address: the type and extent of contamination, if any, that is present, the types of data needed to adequately assess the site; appropriate sampling and analytical methods to characterize the contamination; acceptable level of uncertainty and cleanup technologies that contain or treat the types of wastes present.This document includes references to state agency roles including the Voluntary Cleanup Program, public involvement and other guidances that may be used. Information

Mobile laboratories: An innovative and efficient solution for radiological characterization of sites under or after decommissioning.

PubMed

Goudeau, V; Daniel, B; Dubot, D

2017-04-21

During the operation and the decommissioning of a nuclear site the operator must assure the protection of the workers and the environment. It must furthermore identify and classify the various wastes, while optimizing the associated costs. At all stages of the decommissioning radiological measurements are performed to determine the initial situation, to monitor the demolition and clean-up, and to verify the final situation. Radiochemical analysis is crucial for the radiological evaluation process to optimize the clean-up operations and to the respect limits defined with the authorities. Even though these types of analysis are omnipresent in activities such as the exploitation, the monitoring, and the cleaning up of nuclear plants, some nuclear sites do not have their own radiochemical analysis laboratory. Mobile facilities can overcome this lack when nuclear facilities are dismantled, when contaminated sites are cleaned-up, or in a post-accident situation. The current operations for the characterization of radiological soils of CEA nuclear facilities, lead to a large increase of radiochemical analysis. To manage this high throughput of samples in a timely manner, the CEA has developed a new mobile laboratory for the clean-up of its soils, called SMaRT (Shelter for Monitoring and nucleAR chemisTry). This laboratory is dedicated to the preparation and the radiochemical analysis (alpha, beta, and gamma) of potentially contaminated samples. In this framework, CEA and Eichrom laboratories has signed a partnership agreement to extend the analytical capacities and bring on site optimized and validated methods for different problematic. Gamma-emitting radionuclides can usually be measured in situ as little or no sample preparation is required. Alpha and beta-emitting radionuclides are a different matter. Analytical chemistry laboratory facilities are required. Mobile and transportable laboratories equipped with the necessary tools can provide all that is needed. The main advantage of a mobile laboratory is its portability; the shelter can be placed in the vicinity of nuclear facilities under decommissioning, or of contaminated sites with infrastructures unsuitable for the reception and treatment of radioactive samples. Radiological analysis can then be performed without the disadvantages of radioactive material transport. This paper describes how this solution allows a fast response and control of costs, with a high analytical capacity. Copyright © 2017 Elsevier Ltd. All rights reserved.

Status of Environmental Management Initiatives to Accelerate the Reduction of Environmental Risks and Challenges Posed by the Legacy of the Cold War

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

None

2009-01-01

Fifty years of nuclear weapons production and energy research in the United States during the Cold War generated large amounts of radioactive wastes, spent nuclear fuel (SNF), excess plutonium and uranium, thousands of contaminated facilities, and contaminated soil and groundwater. During most of that half century, the Nation did not have the environmental regulatory structure or nuclear waste cleanup technologies that exist today. The result was a legacy of nuclear waste that was stored and disposed of in ways now considered unacceptable. Cleaning up and ultimately disposing of these wastes is the responsibility of the U.S. Department of Energy (DOE).more » In 1989, DOE established the Office of Environmental Management (EM) to solve the large scale and technically challenging risks posed by the world's largest nuclear cleanup. This required EM to build a new nuclear cleanup infrastructure, assemble and train a technically specialized workforce, and develop the technologies and tools required to safely decontaminate, disassemble, stabilize, disposition, and remediate unique radiation hazards. The sites where nuclear activities produced legacy waste and contamination include the original Manhattan Project sites--Los Alamos, New Mexico; Hanford, Washington; and Oak Ridge, Tennessee--as well as major Cold War sites, such as Savannah River Site, South Carolina; the Idaho National Laboratory, Idaho; Rocky Flats Plant, Colorado; and Fernald, Ohio. Today EM has responsibility for nuclear cleanup activities at 21 sites covering more than two million acres in 13 states, and employs more than 30,000 Federal and contractor employees, including scientists, engineers and hazardous waste technicians. This cleanup poses unique, technically complex problems, which must be solved under the most hazardous of conditions, and which will require billions of dollars a year for several more decades. The EM program focus during its first 10 years was on managing the most urgent risks and maintaining safety at each site while negotiating state and Federal environmental compliance agreements. The program also concentrated on characterizing waste and nuclear materials and assessing the magnitude and extent of environmental contamination. By the late 1990s, EM had made significant progress in identifying and characterizing the extent of contamination and cleanup required and began transitioning from primarily a characterization and stabilization program to an active cleanup and closure program. During that time, EM formulated multi-year cleanup and closure plans, which contributed to cleanup progress; however, reducing the overall environmental risk associated with the cleanup program remained a challenge. In response, the Secretary of Energy directed a review of the EM program be undertaken. The resulting 'Top-to Bottom Review' re-directed the program focus from managing risks to accelerating the reduction of these risks.« less

A multiresidue method for the analysis of 90 pesticides, 16 PAHs, and 22 PCBs in honey using QuEChERS-SPME.

PubMed

Al-Alam, Josephine; Fajloun, Ziad; Chbani, Asma; Millet, Maurice

2017-08-01

An optimized analytical method was developed for the simultaneous analysis of 90 pesticides, 16 polycyclic aromatic hydrocarbons, and 22 polychlorinated biphenyls. The method was based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction using acetonitrile followed by a dispersive solid-phase extraction cleanup using primary-secondary amine and octadecyl (C 18 ). The extract obtained was concentrated by evaporation and then reconstituted with acetonitrile to prepare it for chromatographic analysis by liquid chromatography-triple-quadrupole tandem mass spectrometry and gas chromatography-ion-trap tandem mass spectrometry, which was preceded by a preconcentration step using solid-phase microextraction with appropriate fibers. The combination of the two extraction steps ensured efficient extract cleanup. The use of the two analytical instruments allowed the analysis of a large number of pollutants with a high reliability rate. The method developed was validated for linearity, which was studied with use of matrix-matched calibration curves in the concentration range between 10 and 3000 ng g -1 . The correlation coefficient (R 2 ) obtained was higher than 0.98 for most of the target compounds, with a relative standard deviation lower than 20% for repeatability and reproducibility. The limits of detection and quantification were lower than 20 and 60 ng g -1 respectively for the compounds analyzed, and the recoveries were between 60% and 103% for most compounds. Finally, the method was tested for its efficiency on real samples by the analysis of three honey samples in which seven pesticides and nine polycyclic aromatic hydrocarbons were determined. Graphical Abstract ᅟ.

North Slope (Wahluke Slope) expedited response action cleanup plan

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

Not Available

The purpose of this action is to mitigate any threat to public health and the environment from hazards on the North Slope and meet the expedited response action (ERA) objective of cleanup to a degree requiring no further action. The ERA may be the final remediation of the 100-I-3 Operable Unit. A No Action record of decision (ROD) may be issued after remediation completion. The US Department of Energy (DOE) currently owns or administers approximately 140 mi{sup 2} (about 90,000 acres) of land north and east of the Columbia River (referred to as the North Slope) that is part ofmore » the Hanford Site. The North Slope, also commonly known as the Wahluke Slope, was not used for plutonium production or support facilities; it was used for military air defense of the Hanford Site and vicinity. The North Slope contained seven antiaircraft gun emplacements and three Nike-Ajax missile positions. These military positions were vacated in 1960--1961 as the defense requirements at Hanford changed. They were demolished in 1974. Prior to government control in 1943, the North Slope was homesteaded. Since the initiation of this ERA in the summer of 1992, DOE signed the modified Hanford Federal Agreement and Consent Order (Tri-Party Agreement) with the Washington Department of Ecology (Ecology) and the US Environmental Protection Agency (EPA), in which a milestone was set to complete remediation activities and a draft closeout report by October 1994. Remediation activities will make the North Slope area available for future non-DOE uses. Thirty-nine sites have undergone limited characterization to determine if significant environmental hazards exist. This plan documents the results of that characterization and evaluates the potential remediation alternatives.« less

Multi-residue analysis of 36 priority and emerging pollutants in marine echinoderms (Holothuria tubulosa) and marine sediments by solid-liquid extraction followed by dispersive solid phase extraction and liquid chromatography-tandem mass spectrometry analysis.

PubMed

Martín, J; Zafra-Gómez, A; Hidalgo, F; Ibáñez-Yuste, A J; Alonso, E; Vilchez, J L

2017-05-01

Marine echinoderms are filter-feeding invertebrates widely distributed along the coasts, and which are therefore extensively exposed to anthropogenic xenobiotics. They can serve as good sentinels for monitoring a large variety of contaminants in marine ecosystems. In this context, a multi-residue analytical method has been validated and applied to Holothuria tubulosa specimens and marine sediments for the determination of 36 organic compounds, which belong to some of the most problematic groups of emerging and priority pollutants (perfluoroalkyl compounds, estrogens, parabens, benzophenones, plasticizers, surfactants, brominated flame retardants and alkylphenols). Lyophilization of samples prior to solvent extraction and clean-up of extracts with C18, followed by liquid chromatography-tandem mass spectrometry analysis, is proposed. A Box-Behnken design was used for optimization of the most influential variables affecting the extraction and clean-up steps. For validation, matrix-matched calibration and recovery assay were applied. Linearity (% r 2 ) higher than 99%, recoveries between 80% and 114% (except in LAS and NP1EO), RSD (precision) lower than 15% and limits of quantification between 0.03 and 12.5ngg -1 dry weight (d.w.) were achieved. The method was applied to nine samples of Holothuria collected along the coast of Granada (Spain), and to marine sediments around the animals. The results demonstrated high bioaccumulation of certain pollutants. A total of 25 out of the 36 studied compounds were quantified, being surfactants, alkylphenols, perfluoroalkyl compounds, triclocarban and parabens the most frequently detected. Nonylphenol was found in the highest concentration (340 and 323ngg -1 d.w. in sediment and Holothuria samples, respectively). Copyright © 2017 Elsevier B.V. All rights reserved.

Pressurized liquid extraction using water/isopropanol coupled with solid-phase extraction cleanup for semivolatile organic compounds, polycyclic aromatic hydrocarbons (PAH), and alkylated PAH homolog groups in sediment

USGS Publications Warehouse

Burkhardt, M.R.; Zaugg, S.D.; Burbank, T.L.; Olson, M.C.; Iverson, J.L.

2005-01-01

Polycyclic aromatic hydrocarbons (PAH) are recognized as environmentally relevant for their potential adverse effects on human and ecosystem health. This paper describes a method to determine the distribution of PAH and alkylated homolog groups in sediment samples. Pressurized liquid extraction (PLE), coupled with solid-phase extraction (SPE) cleanup, was developed to decrease sample preparation time, to reduce solvent consumption, and to minimize background interferences for full-scan GC-MS analysis. Recoveries from spiked Ottawa sand, environmental stream sediment, and commercially available topsoil, fortified at 1.5-15 ??g per compound, averaged 94.6 ?? 7.8%, 90.7 ?? 5.8% and 92.8 ?? 12.8%, respectively. Initial method detection limits for single-component compounds ranged from 20 to 302 ??g/kg, based on 25 g samples. Results from 28 environmental sediment samples, excluding homologs, show 35 of 41 compounds (85.4%) were detected in at least one sample with concentrations ranging from 20 to 100,000 ??g/kg. The most frequently detected compound, 2,6-dimethylnaphthalene, was detected in 23 of the 28 (82%) environmental samples with a concentration ranging from 15 to 907 ??g/kg. The results from the 28 environmental sediment samples for the homolog series showed that 27 of 28 (96%) samples had at least one homolog series present at concentrations ranging from 20 to 89,000 ??g/kg. The most frequently detected homolog series, C2-alkylated naphthalene, was detected in 26 of the 28 (93%) environmental samples with a concentration ranging from 25 to 3900 ??g/kg. Results for a standard reference material using dichloromethane Soxhlet-based extraction also are compared. ?? 2005 Elsevier B.V. All rights reserved.

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

PubMed

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

2010-05-01

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

Memorandum of the Establishment of Cleanup Levels for CERCLA Sites with Radioactive Contamination

EPA Pesticide Factsheets

This memorandum presents clarifying guidance for establishing protective cleanup levels for radioactive contamination at Comprehensive Environmental Response, Compensation, and Liability Act of 1980 (CERCLA) sites.

Improving Sampling, Analysis, and Data Management for Site Investigation and Cleanup

EPA Pesticide Factsheets

The United States Environmental Protection Agency (EPA) supports the adoption of streamlined approaches to sampling, analysis, and data management activities conducted during site assessment, characterization, and cleanup.

Increased leukemia risk in Chernobyl cleanup workers

Cancer.gov

A new study found a significantly elevated risk for chronic lymphocytic leukemia among workers who were engaged in recovery and clean-up activities following the Chernobyl power plant accident in 1986.

Radiation Dose to Post-Chernobyl Cleanup Workers

Cancer.gov

Radiation dose calculation for post-Chernobyl Cleanup Workers in Ukraine - both external radiation exposure due to fallout and internal doses due to inhalation (I131 intake) or ingestion of contaminated foodstuffs.

The River Corridor Closure Contract How Washington Closure Hanford is Closing A Unique Department of Energy Project - 12425

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

Feist, E.T.

2012-07-01

Cleanup of the Hanford River Corridor has been one of Hanford Site's top priorities since the early 1990's. This urgency is due to the proximity of hundreds of waste sites to the Columbia River and the groundwater that continues to threaten the Columbia River. In April 2005, the U.S. Department of Energy, Richland Operations Office (DOE-RL) awarded the Hanford River Corridor Closure Contract (RCCC), a cost-plus incentive-fee closure contract with a 2015 end date and first of its kind at Hanford Site, to Washington Closure Hanford (WCH), a limited-liability company owned by URS, Bechtel National, and CH2M HILL. WCH ismore » a single-purpose company whose goal is to safely, compliantly, and efficiently accelerate cleanup in the Hanford River Corridor and reduce or eliminate future obligations to DOE-RL for maintaining long-term stewardship over the site. Accelerated performance of the work-scope while keeping a perspective on contract completion presents challenges that require proactive strategies to support the remaining work-scope through the end of the RCCC. This paper outlines the processes to address the challenges of completing work-scope while planning for contract termination. WCH is responsible for cleanup of the River Corridor 569.8 km{sup 2} (220 mi{sup 2}) of the 1,517.7 km{sup 2} (586 mi{sup 2}) Hanford Site's footprint reduction. At the end of calendar year 2011, WCH's closure implementation is well underway. Fieldwork is complete in three of the largest areas within the RCCC scope (Segments 1, 2, and 3), approximately 44.5% of the River Corridor (Figure 3). Working together, DOE-RL and WCH are in the process of completing the 'paper work' that will document the completion of the work-scope and allow DOE-RL to relieve WCH of contractual responsibilities and transition the completed areas to the Long-Term Stewardship Program, pending final action RODs. Within the next 4 years, WCH will continue to complete cleanup of the River Corridor following the completion goals. As field work-scope is completed, progressive reductions of business processes, physical facilities, and staff will occur. Organizations will collapse and flatten commensurate with workload. WCH employees will move on to new endeavors, proud of their accomplishments and the legacy they are leaving behind as being the first and largest environmental cleanup closure contract at Hanford. (authors)« less

Environmental Cleanup of the East Tennessee Technology Park Year One - Execution with Certainty SM - 13120

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

Schubert, A.L.

2013-07-01

On August 1, 2011, URS - CH2M Oak Ridge LLC (UCOR) began its five-year, $1.4 billion cleanup of the East Tennessee Technology Park (ETTP), located on the U.S. Department of Energy's (DOE) Oak Ridge Reservation in Tennessee. UCOR will close out cleanup operations that began in 1998 under a previous contract. When the Contract Base scope of work [1] is completed in 2016, the K-25 gaseous diffusion building will have been demolished and all waste dispositioned, demolition will have started on the K-27 gaseous diffusion building, all contact-handled and remote-handled transuranic waste in inventory (approximately 500 cubic meters) will havemore » been transferred to the Transuranic Waste Processing Center, previously designated 'No-Path-To-Disposition Waste' will have been dispositioned to the extent possible, and UCOR will have managed DOE Office of Environmental Management (EM)- owned facilities at ETTP, Oak Ridge National Laboratory (ORNL), and the Y-12 National Security Complex in a safe and cost-effective manner. Since assuming its responsibilities as the ETTP cleanup contractor, UCOR has completed its life-cycle Performance Measurement Baseline; received its Earned Value Management System (EVMS) certification; advanced the deactivation and demolition (D and D) of the K-25 gaseous diffusion building; recovered and completed the Tank W-1A and K-1070-B Burial Ground remediation projects; characterized, packaged, and shipped contact-handled transuranic waste to the Transuranic Waste Processing Center; disposed of more than 90,000 cubic yards of cleanup waste while managing the Environmental Management Waste Management Facility (EMWMF); and provided operations, surveillance, and maintenance activities at DOE EM facilities at ETTP, ORNL, and the Y-12 National Security Complex. Project performance as of December 31, 2012 has been excellent: - Cost Performance Index - 1.06; - Schedule Performance Index - 1.02. At the same time, since safety is the foundation of all cleanup work, UCOR's safety record goes hand in hand with its excellent project performance. Through calendar year 2012, UCOR's recordable injury rate was 0.33, and the company has worked close to 4 million hours without a lost work day injury. UCOR's safety record is one of the best in the DOE EM Complex. This performance was due, in large part, to the people and processes URS and CH2M HILL, the parent companies of UCOR, brought to the project. Key approaches included: - Selected and deployed experienced staff in key leadership positions throughout the organization; - Approached 'Transition' as the 'true' beginning of the cleanup project - kicking off a number of project initiatives such as Partnering, PMB development, D and D Plan execution, etc. - Established a project baseline for performance measurement and obtained EVMS certification in record time; - Determined material differences and changed conditions that warranted contract change - then quickly addressed these changes with the DOE client; - Aligned the project and the contract within one year - also done in record time; - Implemented Safety Trained Supervisor and Safety Conscious Work Environment Programs, and kicked off the pursuit of certification under DOE's Voluntary Protection Program. (authors)« less

Classification of Floating Chris Chemicals for the Development of a Spill Response Manual

DTIC Science & Technology

1989-01-01

Spill collection of the spent floating media in a static body of water was accomplished using existing oil spill cleanup equipment. The effectiveness...carbon depends on the size of particle required and type of carbon purchased. Regeneration of the spent carbon is difficult and may not lower costs...enhance the dispersion of a spill. Care must be taken to limit or prevent any caustic or hazardous spill material from personnel contact. Aeration

Nuclear radiation cleanup and uranium prospecting

DOEpatents

Mariella, Jr., Raymond P.; Dardenne, Yves M.

2016-02-02

Apparatus, systems, and methods for nuclear radiation cleanup and uranium prospecting include the steps of identifying an area; collecting samples; sample preparation; identification, assay, and analysis; and relating the samples to the area.

Nuclear radiation cleanup and uranium prospecting

DOEpatents

Mariella, Jr., Raymond P.; Dardenne, Yves M.

2017-01-03

Apparatus, systems, and methods for nuclear radiation cleanup and uranium prospecting include the steps of identifying an area; collecting samples; sample preparation; identification, assay, and analysis; and relating the samples to the area.

Cleanup Verification Package for the 300-18 Waste Site

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

J. M. Capron

This cleanup verification package documents completion of remedial action for the 300-18 waste site. This site was identified as containing radiologically contaminated soil, metal shavings, nuts, bolts, and concrete.

Green Remediation Best Management Practices: Mining Sites

EPA Pesticide Factsheets

This fact sheet describes best management practices (BMPs) that can be used to reduce the environmental footprint of cleanup activities associated with common project components, cleanup phases, and implementation of remediation technologies.

HANFORD SITE RIVER CORRIDOR CLEANUP

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

BAZZELL, K.D.

2006-02-01

In 2005, the US Department of Energy (DOE) launched the third generation of closure contracts, including the River Corridor Closure (RCC) Contract at Hanford. Over the past decade, significant progress has been made on cleaning up the river shore that bordes Hanford. However, the most important cleanup challenges lie ahead. In March 2005, DOE awarded the Hanford River Corridor Closure Contract to Washington Closure Hanford (WCH), a limited liability company owned by Washington Group International, Bechtel National and CH2M HILL. It is a single-purpose company whose goal is to safely and efficiently accelerate cleanup in the 544 km{sup 2} Hanfordmore » river corridor and reduce or eliminate future obligations to DOE for maintaining long-term stewardship over the site. The RCC Contract is a cost-plus-incentive-fee closure contract, which incentivizes the contractor to reduce cost and accelerate the schedule. At $1.9 billion and seven years, WCH has accelerated cleaning up Hanford's river corridor significantly compared to the $3.2 billion and 10 years originally estimated by the US Army Corps of Engineers. Predictable funding is one of the key features of the new contract, with funding set by contract at $183 million in fiscal year (FY) 2006 and peaking at $387 million in FY2012. Another feature of the contract allows for Washington Closure to perform up to 40% of the value of the contract and subcontract the balance. One of the major challenges in the next few years will be to identify and qualify sufficient subcontractors to meet the goal.« less

Online Hazardous Waste Cleanup Technical Resources

EPA Pesticide Factsheets

This issue paper is intended to give the reader examples of some online technical resources that can assist with hazardous waste cleanups in the Superfund, Resource Conservation and Recovery Act (RCRA), and Brownfields programs.

A Citizen's Guide to Drycleaner Cleanup

EPA Pesticide Factsheets

The State Coalition for Remediation of Drycleaners (SCRD) has prepared an easy-to-read guide explaining the drycleaner cleanup process and describing the technologies that are most commonly used to clean up contaminated drycleaner sites.

Tribal Lands Cleanup and Spill Prevention Programs

EPA Pesticide Factsheets

EPA takes strides to prevent and cleanup contamination and contaminated sites located on or near Tribal lands. Our programs work hand-in-hand with tribes to ensure we protect their health and the environment.

Hazardous Waste: Cleanup and Prevention.

ERIC Educational Resources Information Center

Vandas, Steve; Cronin, Nancy L.

1996-01-01

Describes the Superfund, a federal cleanup program created in response to growing public concern over the health and environmental risks posed by hazardous waste sites. Discusses sources, disposal, and movement and risk of hazardous waste. (JRH)

Workplace Safety: Indoor Environmental Quality

MedlinePlus

... Cleanup Tuberculosis Follow NIOSH Facebook Flickr Pinterest Twitter YouTube NIOSH Homepage NIOSH A-Z Workplace Safety & Health ... Cleanup Tuberculosis Follow NIOSH Facebook Flickr Pinterest Twitter YouTube NIOSH Homepage NIOSH A-Z Workplace Safety & Health ...

Burbank performs the scheduled extensive cleanup of ventilation systems

NASA Image and Video Library

2012-02-22

ISS030-E-093414 (22 Feb. 2012) --- NASA astronaut Dan Burbank, Expedition 30 commander, performs the scheduled extensive cleanup of ventilation systems in the Columbus laboratory of the International Space Station.

43 CFR 3931.30 - Suspension of operations and production.

Code of Federal Regulations, 2012 CFR

2012-10-01

... environmental studies or analysis; (2) To ensure that necessary environmental remediation or cleanup is being... environmental remediation or cleanup is being performed as a result of unwarranted or unexpected actions. (c...

43 CFR 3931.30 - Suspension of operations and production.

Code of Federal Regulations, 2013 CFR

2013-10-01

... environmental studies or analysis; (2) To ensure that necessary environmental remediation or cleanup is being... environmental remediation or cleanup is being performed as a result of unwarranted or unexpected actions. (c...

43 CFR 3931.30 - Suspension of operations and production.

Code of Federal Regulations, 2011 CFR

2011-10-01

... environmental studies or analysis; (2) To ensure that necessary environmental remediation or cleanup is being... environmental remediation or cleanup is being performed as a result of unwarranted or unexpected actions. (c...

43 CFR 3931.30 - Suspension of operations and production.

Code of Federal Regulations, 2014 CFR

2014-10-01

... environmental studies or analysis; (2) To ensure that necessary environmental remediation or cleanup is being... environmental remediation or cleanup is being performed as a result of unwarranted or unexpected actions. (c...

Molds in the Environment

MedlinePlus

... visit this page: About CDC.gov . Mold Cleanup & Remediation Homeowner’s and Renter’s Guide to Mold Cleanup After ... Home or Building with Mold Damage Prevention and Remediation Strategies for the Control and Removal of Fungal ...

Hazardous waste sites: voluntary industry cleanup proposed

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

Not Available

1984-02-27

A proposal that calls for the chemical industry to undertake voluntary cleanup of hazardous waste sites was presented recently to the Environmental Protection Agency and on Capitol Hill. And although still in draft form, the proposal has elicited a very favorable response. In its present form, the proposal calls for setting up a nonprofit holding company, supported by donations from the chemical industry, to plan and carry out cleanup operations. It is the result of nine months of discussion among representatives of industry, environmental groups, and former government personnel, carried out under the auspices of the Conservation Foundation to assessmore » what could be done to speed the cleanup of hazardous waste sites. Although still in draft form, the proposal already is getting excellent reviews. One Congressional staff member says that the idea of a voluntary program is excellent. And EPA sees it as a real opportunity to supplement its funds - which it has been saying are nowhere near adequte to clean up all the sites that it expects eventually to be placed on the national priorities list - and get the work done. All this, of course, would occur under the agency's watchful eye. Some in the environmental community fear that the mere discussion of a private cleanup exercise might be used as an argument for not reauthorizing Superfund or for not expanding the size of the fund. However, most see the voluntary cleanup as a supplement to, not a replacement for, the Superfund program.« less

Odour as a determinant of persistent symptoms after a chemical explosion, a longitudinal study

PubMed Central

TJALVIN, Gro; MAGERØY, Nils; BRÅTVEIT, Magne; LYGRE, Stein Håkon Låstad; HOLLUND, Bjørg Eli; MOEN, Bente Elisabeth

2016-01-01

Foul-smelling environmental pollution was a major concern following a chemical workplace explosion. Malodorous pollution has previously been associated with aggravated physical and psychological health, and in persons affected by a trauma, an incidence-related odour can act as a traumatic reminder. Olfaction may even be of significance in the development and persistence of post-traumatic stress symptoms (PTSS). The present longitudinal study assessed whether perceived smell related to malodorous environmental pollution in the aftermath of the explosion was a determinant of subjective health complaints (SHC) and PTSS among gainfully employed adults, when the malodorous pollution was present, and after pollution clean-up. Questionnaire data from validated instruments were analysed using mixed effects models. Individual odour scores were computed, and the participants (n=486) were divided into high and low odour score groups, respectively. Participants in the high odour score group (n=233) reported more SHC and PTSS than those in the low odour score group (n=253), before and even after the pollution was eliminated. These associations lasted for at least three years after the pollution was removed, and might indicate that prompt clean-up is important to avoid persistent health effects after malodorous chemical spills. PMID:27916759

Odour as a determinant of persistent symptoms after a chemical explosion, a longitudinal study.

PubMed

Tjalvin, Gro; Magerøy, Nils; Bråtveit, Magne; Lygre, Stein Håkon Låstad; Hollund, Bjørg Eli; Moen, Bente Elisabeth

2017-04-07

Foul-smelling environmental pollution was a major concern following a chemical workplace explosion. Malodorous pollution has previously been associated with aggravated physical and psychological health, and in persons affected by a trauma, an incidence-related odour can act as a traumatic reminder. Olfaction may even be of significance in the development and persistence of post-traumatic stress symptoms (PTSS). The present longitudinal study assessed whether perceived smell related to malodorous environmental pollution in the aftermath of the explosion was a determinant of subjective health complaints (SHC) and PTSS among gainfully employed adults, when the malodorous pollution was present, and after pollution clean-up. Questionnaire data from validated instruments were analysed using mixed effects models. Individual odour scores were computed, and the participants (n=486) were divided into high and low odour score groups, respectively. Participants in the high odour score group (n=233) reported more SHC and PTSS than those in the low odour score group (n=253), before and even after the pollution was eliminated. These associations lasted for at least three years after the pollution was removed, and might indicate that prompt clean-up is important to avoid persistent health effects after malodorous chemical spills.

Quantitation of fumonisin B1 and B2 in feed using FMOC pre-column derivatization with HPLC and fluorescence detection.

PubMed

Smith, Lori L; Francis, Kyle A; Johnson, Joseph T; Gaskill, Cynthia L

2017-11-01

Pre-column derivatization with 9-fluorenylmethyl chloroformate (FMOC-Cl) was determined to be effective for quantitation of fumonisins B 1 and B 2 in feed. Liquid-solid extraction, clean-up using immunoaffinity solid phase extraction chromatography, and FMOC-derivatization preceded analysis by reverse phase HPLC with fluorescence. Instrument response was unchanged in the presence of matrix, indicating no need to use matrix-matched calibrants. Furthermore, high method recoveries indicated calibrants do not need to undergo clean-up to account for analyte loss. Established method features include linear instrument response from 0.04-2.5µg/mL and stable derivatized calibrants over 7days. Fortified cornmeal method recoveries from 0.1-30.0μg/g were determined for FB 1 (75.1%-109%) and FB 2 (96.0%-115.2%). Inter-assay precision ranged from 1.0%-16.7%. Method accuracy was further confirmed using certified reference material. Inter-laboratory comparison with naturally-contaminated field corn demonstrated equivalent results with conventional derivatization. These results indicate FMOC derivatization is a suitable alternative for fumonisins B 1 and B 2 quantitation in corn-based feeds. Copyright © 2017 Elsevier Ltd. All rights reserved.

Multivariate Optimization for Extraction of Pyrethroids in Milk and Validation for GC-ECD and CG-MS/MS Analysis

PubMed Central

Zanchetti Meneghini, Leonardo; Rübensam, Gabriel; Claudino Bica, Vinicius; Ceccon, Amanda; Barreto, Fabiano; Flores Ferrão, Marco; Bergold, Ana Maria

2014-01-01

A simple and inexpensive method based on solvent extraction followed by low temperature clean-up was applied for determination of seven pyrethroids residues in bovine raw milk using gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) and gas chromatography with electron-capture detector (GC-ECD). Sample extraction procedure was established through the evaluation of seven different extraction protocols, evaluated in terms of analyte recovery and cleanup efficiency. Sample preparation optimization was based on Doehlert design using fifteen runs with three different variables. Response surface methodologies and polynomial analysis were used to define the best extraction conditions. Method validation was carried out based on SANCO guide parameters and assessed by multivariate analysis. Method performance was considered satisfactory since mean recoveries were between 87% and 101% for three distinct concentrations. Accuracy and precision were lower than ±20%, and led to no significant differences (p < 0.05) between results obtained by GC-ECD and GC-MS/MS techniques. The method has been applied to routine analysis for determination of pyrethroid residues in bovine raw milk in the Brazilian National Residue Control Plan since 2013, in which a total of 50 samples were analyzed. PMID:25380457

Patterns of hematological malignancies in Chernobyl clean-up workers (1996-2005).

PubMed

Gluzman, D; Imamura, N; Sklyarenko, L; Nadgornaya, V; Zavelevich, M; Machilo, V

2006-03-01

The question as to whether the incidence of leukemias and malignant lymphomas among the Chernobyl clean-up workers increased in 20 years after the catastrophe is still a point of much controversy. Precise diagnosis of the main forms of hematopoietic malignancies according to FAB classification and new WHO classification and comparison of these data with that in the general population will be helpful in estimating the relative contribution of the radiation factor to the overall incidence of such pathologies. The data on 218 consecutive cases of malignant diseases of hematopoietic and lymphoid tissues in Chernobyl clean-up workers diagnosed in 1996-2005 are given in comparison with the data of 2697 consecutive patients of general population of the same age group. The morphology and cytochemistry of bone marrow and peripheral blood cells were studied. Immunocytochemical techniques (APAAP, LSAB-AP) and the broad panel of monoclonal antibodies to lineage specific and differentiation antigens of leukocytes were employed for immunophenotyping leukemic cells. Various types of oncohematological diseases developing 10-20 years after Chernobyl accident were registered in a group of clean-up workers under study including myelodysplastic syndromes (MDS), acute leukemias (ALL and AML), chronic myelogenous leukemia (CML) and other chronic myeloproliferative diseases, chronic lymphocytic leukemia (B-CLL) and other chronic lymphoproliferative diseases of B and T cell origin. MDS percentage among patients of clean-up workers group tended to exceed MDS percentage in the group of patients representing the general population examined at the same period (4.58 vs. 3.70%). Among 34 AML cases, leukemia was preceded by MDS in seven patients. The relative contribution of CML to the total number of clean-up workers with leukemia was higher than the corresponding percentage value in general population examined at the same period (9.17 vs. 6.59%). B-CLL was a predominant form of hematopoietic malignancies in clean-up workers under study (25.68%). Nevertheless, B-CLL percentage in patients of clean-up workers group did not differ significantly from that in the patients of general population. The multiple myeloma percentage (7.79%) in the group of patients belonging to clean-up workers in our study turned out to be twice as much as in the patients of general population (4.0%). The verified diagnosis of tumors of hematopoietic and lymphoid tissue according to modern classification (EGIL, WHO) could be the prerequisite for further molecular genetic and analytical epidemiology study of leukemias that may be related to Chernobyl NPP accident consequences.

Green Remediation Best Management Practices: Integrating Renewable Energy into Site Cleanup

EPA Pesticide Factsheets

The U.S. Environmental Protection Agency (EPA) Principles for Greener Cleanups outline the Agency's policy for evaluating and minimizing the environmental 'footprint' of activities undertaken when cleaning up a contaminated site.

Using the Triad Approach to Streamline Brownfields Site Assessment and Cleanup

EPA Pesticide Factsheets

EPA's Brownfields Technology Support Center (BTSC) has prepared this document to provide an educational tool for site owners, project managers, and regulators to help streamline assessment and cleanup activities at brownfields sites.

Brief Guide to Mold, Moisture, and Your Home

MedlinePlus

... your eyes. How Do I Know When the Remediation or Cleanup is Finished? You must have completely ... water or moisture problem before the cleanup or remediation can be considered finished. You should have completed ...

76 FR 10018 - Environmental Management Site-Specific Advisory Board, Idaho National Laboratory

Federal Register 2010, 2011, 2012, 2013, 2014

2011-02-23

... Idaho's 2015 Cleanup Vision Government Budget Cycle American Recovery and Reinvestment Act Idaho Cleanup.... The Deputy Designated Federal Officer is empowered to conduct the meeting in a fashion that will...

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

Friesen, H.N.

This summary document presents results in a broad context; it is not limited to findings of the Nevada Applied Ecology Group. This book is organized to present the findings of the Nevada Applied Ecology Group and correlative programs in accordance with the originally stated objectives of the Nevada Applied Ecology Group. This plan, in essence, traces plutonium from its injection into the environment to movement in the ecosystem to development of cleanup techniques. Information on other radionuclides was also obtained and will be presented briefly. Chapter 1 presents a brief description of the ecological setting of the Test Range Complex.more » The results of investigations for plutonium distribution are presented in Chapter 2 for the area surrounding the Test Range Complex and in Chapter 3 for on-site locations. Chapters 4 and 5 present the results of investigations concerned with concentrations and movement, respectively, of plutonium in the ecosystem of the Test Range Complex, and Chapter 6 summarizes the potential hazard from this plutonium. Development of techniques for cleanup and treatment is presented in Chapter 7, and the inventory of radionuclides other than plutonium is presented briefly in Chapter 8.« less

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. Copyright © 2015. Published by Elsevier B.V.

Determination of 82 veterinary drugs in swine waste lagoon sludge by ultra-high performance liquid chromatography-tandem mass spectrometry.

PubMed

Li, Xiaowei; Guo, Ping; Shan, Yawen; Ke, Yuebin; Li, Hui; Fu, Qin; Wang, Yingyu; Liu, Tianhe; Xia, Xi

2017-05-26

This work reports the development of a multi-residue method for the identification and quantification of 82 veterinary drugs belonging to different chemical classes in swine waste lagoon. The proposed method applies a solid-phase extraction procedure with Oasis PRiME HLB cartridges that combines isolation of the compounds and sample clean-up in a single step. Analysis is performed by ultra-high performance liquid chromatography-tandem mass spectrometry, in one single injection with a chromatographic run time of only 9.5min. Linearity was studied in the range between 1 and 500μgkg -1 using standards prepared both in pure solvent and in the presence of matrix, showing coefficients of determination higher than 0.99 for all the analytes except for cefapirin in matrix. The average recoveries were in the range of 60-110% for most of the compounds tested with inter-day relative standard deviations below 17%. More than 97% of the investigated compounds had less or equal to a 5μgkg -1 quantitation limit in the studied matrix. Finally, the method was used with success to detect and quantify veterinary drugs residues in real samples with sulfonamides, quinolones, and tetracyclines being the most frequently determined compound groups. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of diflubenzuron and chlorbenzuron in fruits by combining acetonitrile-based extraction with dispersive liquid-liquid microextraction followed by high-performance liquid chromatography.

PubMed

Ruan, Chunqiang; Zhao, Xiang; Liu, Chenglan

2015-09-01

In this study, a simple and low-organic-solvent-consuming method combining an acetonitrile-partitioning extraction procedure followed by "quick, easy, cheap, effective, rugged and safe" cleanup with ionic-liquid-based dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection was developed for the determination of diflubenzuron and chlorbenzuron in grapes and pears. Ionic-liquid-based dispersive liquid-liquid microextraction was performed using the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate as the extractive solvent and acetonitrile extract as the dispersive solvent. The main factors influencing the efficiency of the dispersive liquid-liquid microextraction were evaluated, including the extractive solvent type and volume and the dispersive solvent volume. The validation parameters indicated the suitability of the method for routine analyses of benzoylurea insecticides in a large number of samples. The relative recoveries at three spiked levels ranged between 98.6 and 109.3% with relative standard deviations of less than 5.2%. The limit of detection was 0.005 mg/kg for the two insecticides. The proposed method was successfully used for the rapid determination of diflubenzuron and chlorbenzuron residues in real fruit samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of paraben preservatives in seafood using matrix solid-phase dispersion and on-line acetylation gas chromatography-mass spectrometry.

PubMed

Djatmika, Rosalina; Hsieh, Chih-Chung; Chen, Jhih-Ming; Ding, Wang-Hsien

2016-11-15

An effective method for determining four commonly detected paraben preservatives (methyl, ethyl, propyl and butyl paraben) in marketed seafood is presented. This method employs matrix solid-phase dispersion (MSPD) before identification and quantification of the paraben preservatives via on-line acetylation gas chromatography-mass spectrometry (GC-MS). Parameters affecting the extraction efficiency of MSPD were optimized through a Box-Behnken design method. Under optimal condition, 0.5-g of freeze-dried seafood was mixed with 0.5-g of anhydrous sodium sulfate, and dispersed with 1.0-g of Florisil using vortex. After that, the blend was transferred to a glass column containing 1.5-g of silica gel+C18 (w/w, 9:1), which acted as clean-up co-sorbents. Then, target analytes were eluted with 12mL of acetonitrile. The extract was then derivatized on-line in the GC injection-port through reaction with acetic anhydride, and the identity and quantity of the target analytes were determined by the GC-MS system. The limits of quantitation (LOQs) were 0.2 to 1.0ng/g (dry weight). Preliminary results showed that the total concentrations of four selected parabens ranged from 16.7 to 44.7ng/g (dry weight). Copyright © 2016 Elsevier B.V. All rights reserved.

Development and validation of a solid-phase extraction method coupled with HPLC-UV detection for the determination of biogenic amines in Chinese rice wine.

PubMed

Zhang, Ying; Li, Yan; Zhu, Xiao-Juan; Li, Min; Chen, Hao-Yu; Lv, Xiao-Ling; Zhang, Jian

2017-07-01

A reliable and accurate method for the determination of seven biogenic amines (BAs) was developed and validated with Chinese rice wine samples. The BAs were derivatised with dansyl chloride, cleaned up using solid-phase extraction (SPE) and separated by high-performance liquid chromatography (HPLC) coupled with ultraviolet (UV) detection. The optimised derivatisation reaction, conducted at pH 9.6 and 60°C for 30 min, ensured baseline separation and peak symmetry for each BA. SPE clean-up using Oasis MCX cartridges yielded good recovery rates for all BAs and effectively reduced matrix effects. The developed method shows good linearity with determination coefficients of more than 0.9989 over a concentration range of 0.1-100 mg l -1 . The limits of detection (LODs) for the investigated BAs ranged from 2.07 to 5.56 µg l -1 . The intra- and inter-day relative standard deviations (RSDs) ranged from 0.86% to 3.81% and from 2.13% to 3.82%, respectively. Spiking experiments showed that the overall recovery rates ranged from 85% to 113%. Thus, the proposed method was demonstrated as being suitable for simultaneous detection, with accurate and precise quantification, of BAs in Chinese rice wine.

Validation of an Analytical Method for Determination of Benzo[a]pyrene Bread using QuEChERS Method by GC-MS

PubMed Central

Eslamizad, Samira; Yazdanpanah, Hassan; Javidnia, Katayon; Sadeghi, Ramezan; Bayat, Mitra; Shahabipour, Sara; Khalighian, Najmeh; Kobarfard, Farzad

2016-01-01

A fast and simple modified QuEChERS (quick, easy, cheap, rugged and safe) extraction method based on spiked calibration curves and direct sample introduction was developed for determination of Benzo [a] pyrene (BaP) in bread by gas chromatography-mass spectrometry single quadrupole selected ion monitoring (GC/MS-SQ-SIM). Sample preparation includes: extraction of BaP into acetone followed by cleanup with dispersive solid phase extraction. The use of spiked samples for constructing the calibration curve substantially reduced adverse matrix-related effects. The average recovery of BaP at 6 concentration levels was in range of 95-120%. The method was proved to be reproducible with relative standard deviation less than 14.5% for all of the concentration levels. The limit of detection and limit of quantification were 0.3 ng/g and 0.5 ng/g, respectively. Correlation coefficient of 0.997 was obtained for spiked calibration standards over the concentration range of 0.5-20 ng/g. To the best of our knowledge, this is the first time that a QuEChERS method is used for the analysis of BaP in breads. The developed method was used for determination of BaP in 29 traditional (Sangak) and industrial (Senan) bread samples collected from Tehran in 2014. These results showed that two Sangak samples were contaminated with BaP. Therefore, a comprehensive survey for monitoring of BaP in Sangak bread samples seems to be needed. This is the first report concerning contamination of bread samples with BaP in Iran. PMID:27642317

Determination of ochratoxin A in grapes of Greek origin by immunoaffinity and high-performance liquid chromatography.

PubMed

Meletis, Konstantinos; Meniades-Meimaroglou, Sofia; Markaki, Panagiota

2007-11-01

A simple analytical method for ochratoxin A (OTA) determination in grapes is described, using aqueous methanolic extraction, an immunoaffinity column clean-up step and high-performance liquid chromatography with fluorescence detection. Mean recovery was 94% (RSD = 4.0%) with a detection limit of 0.4 ng g(-1) and quantification limit of 1.20 ng g(-1). Repeatability (r) and reproducibility (R) were 1.17 and 1.34, respectively. OTA determinations were applied to 50 grape samples (23 different varieties) originating from representative regions of Greece. Results showed the presence of OTA in 86% of samples tested (n = 50). Traces were found in 56% of samples but OTA was not detectable in 14% of samples. Traces were also found in 4% of red, organically grown samples. The most contaminated were three samples of red grapes, two from Central Greece (2.69 and 1.41 ng g(-1)), both table and wine-making grapes. The third sample (1.46 ng g(-1)), originating from the island of Samos, was used only in wine-making. Mean (1.06 ng g(-1)) and median (0.76 ng g(-1)) OTA concentrations in red grapes were slightly higher compared to the mean (0.82 ng g(-1)) and median (0.65 ng g(-1)) concentrations in white grape samples. The study shows that the potential risk for a person of 60 kg ranged from 0.9 to 9 ng kg(-1) bw day(-1) and is dependent on the quantity of grapes consumed daily.

Automated determination of polyamines by high-performance liquid chromatography with simple sample preparation.

PubMed

van Eijk, H M; Rooyakkers, D R; Deutz, N E

1996-04-12

Recently, a new fully endcapped reversed-phase packing material, Inertsil, was introduced, especially suitable for the determination of basic compounds. We used this packing material to separate ophthaldialdehyde (OPA) derivatives of amino acid derivatives completely from the OPA derivatives of spermine (SPM), spermidine (SPD), putrescine (PUT) and cadaverine (CAD). The obtained separation made the commonly used off-line extraction procedure redundant and thus an on-line sample clean-up was introduced. This enabled automation of the procedure resulting in a better reproducibility and a more efficient use of equipment. Furthermore, no studies are required to determine the extraction recovery. The present method has a cycle time of 30 min. A linear response for each polyamine was found up to 250 pmol, with an R2 ranging from 0.9981 (SPM) to 0.9998 (CAD). The limit of detection, calculated at a signal-to-noise ratio of 3, was 0.1 pmol, corresponding to a plasma concentration of 0.1 mumol/l. The coefficient of variation (C.V.) for the peak area was below 3% and for retention times below 0.5% (n = 15). In order to evaluate the applicability of the method, three different types of sample were chromatographed, e.g. urine (obtained from healthy human volunteers), pig plasma and sulfosalicylic acid homogenates of pig intestine biopsies. Tissue homogenates and urine-specimen could easily be quantitated, while plasma concentrations were just above the limit of detection, resulting in a plasma C.V. ranging from 4.8% (SPM) to 13.6% (SPD) and a tissue C.V. ranging from 2.1% (SPM) to 8.5% (CAD), The urinary C.V.s were not determined. In conclusion, the present method provides an easy way to measure polyamine concentrations for most applications.

Utilizing the right mix of environmental cleanup technologies

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

Whitaker, Wade; Bergren, Chris; Flora, Mary

2007-07-01

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 that are required by environmental regulations, to undergo characterization and, if needed, remediation.more » In the initial years of the SRS environmental cleanup program (early 1990's), 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, phyto-remediation, underground cutoff walls, dynamic underground stripping, soil fracturing, microbial degradation, baro-balls, electrical resistance heating, soil vapor extraction, and micro-blowers to more effectively treat contamination at lower costs. Additionally, SRS's remediation approach cost effectively maximizes cleanup as SRS works pro-actively 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 technologies. Remediating large, complex groundwater plumes using state of-the art technologies and approaches is a hallmark of years of experience and progress. Environmental restoration at SRS continues to be a challenging and dynamic process as new cleanup technologies and approaches are adopted. (authors)« less

Engineering Forum Issue Paper: Online Hazardous Waste Cleanup Technical Resources

EPA Pesticide Factsheets

This issue paper is intended to give the reader examples of some online technical resources that can assist with hazardous waste cleanups in the Superfund, Resource Conservation and Recovery Act (RCRA), and Brownfields programs.

24 CFR 598.215 - What are the purpose and content of the strategic plan?

Code of Federal Regulations, 2014 CFR

2014-04-01

... preserve the environment and historic landmarks, address “brownfields” clean-up and redevelopment, explore..., Environmental Cleanup Cost Deduction (i.e., “Brownfields Tax Incentive”), and the Work Opportunity Tax Credit...

24 CFR 598.215 - What are the purpose and content of the strategic plan?

Code of Federal Regulations, 2013 CFR

2013-04-01

... preserve the environment and historic landmarks, address “brownfields” clean-up and redevelopment, explore..., Environmental Cleanup Cost Deduction (i.e., “Brownfields Tax Incentive”), and the Work Opportunity Tax Credit...

24 CFR 598.215 - What are the purpose and content of the strategic plan?

Code of Federal Regulations, 2012 CFR

2012-04-01

... preserve the environment and historic landmarks, address “brownfields” clean-up and redevelopment, explore..., Environmental Cleanup Cost Deduction (i.e., “Brownfields Tax Incentive”), and the Work Opportunity Tax Credit...

EPA Completes Reviews of 14 New England Site Cleanups during FY’ 2017

EPA Pesticide Factsheets

EPA has completed comprehensive reviews of site cleanups at 14 National Priorities List Sites (Superfund Sites), including four Federal Facilities, across New England by performing required Five-Year Reviews of each site.

Report: EPA Needs to Track Compliance with Superfund Cleanup Requirements

EPA Pesticide Factsheets

Report #08-P-0141, April 28, 2008. According to EPA’s Superfund information system, there were 3,397 active Superfund enforcement instruments to ensure cleanups at National Priorities List sites as of September 30, 2007.

Introduction to Energy Conservation and Production at Waste Cleanup Sites

EPA Pesticide Factsheets

This issue paper, prepared by EPA's Engineering Forum under the Technical Support Project, provides an overview on the considerations for energy conservation and production during the design and (O&M) phases of waste cleanup projects.

EPA Begins Reviews of 24 New England Site Cleanups during Current Fiscal Year

EPA Pesticide Factsheets

EPA plans to conduct comprehensive reviews of site cleanups at 24 National Priorities List Sites (Superfund Sites), including two Federal Facilities, across New England by performing required Five-Year Reviews of sites.

The Great Oil Spill Cleanup Contest.

ERIC Educational Resources Information Center

Hampton, Elaine

1993-01-01

Presents an exciting way to acquaint students with current methods to clean up oil spills. Students also have the freedom to create new clean-up methods as they think through the problem and experiment to find effective solutions. (PR)

A modified QuEChERS method for the determination of some herbicides in yogurt and milk by high performance liquid chromatography.

PubMed

Li, Na; Lei, Lei; Nian, Li; Zhang, Rui; Wu, Shuting; Ren, Ruibing; Wang, Yeqiang; Zhang, Hanqi; Yu, Aimin

2013-02-15

A modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was applied to the extraction of triazines and phenylureas from milk and yogurt. The herbicides was extracted by the mixture of ethyl acetate and n-hexane and cleaned by primary secondary amine (10mg/mL). The frozen-out centrifugation was applied to further remove fatty. The proposed method can achieve efficient extraction and cleanup. Some experimental parameters, such as extraction method, extraction solvent and adsorbent, pH of sample solution, extraction time and amount of primary secondary amine and sodium chloride were investigated and optimized. The precision and absolute recoveries of eight herbicides vary from 0.07 to 5.86% and from 78.9 to 99.9%, respectively. The detection limits for simeton, monuron, chlorotoluron, simetryne, atrazine, karmex, ametryne and propazine range from 0.15 to 0.35 ng/mL. Copyright © 2012 Elsevier B.V. All rights reserved.

Simultaneous determination of fluoroquinolones in environmental water by liquid chromatography-tandem mass spectrometry with direct injection: A green approach.

PubMed

Denadai, Marina; Cass, Quezia Bezerra

2015-10-30

This work describes an on-line multi-residue method for simultaneous quantification of ciprofloxacin, enrofloxacin, gemifloxacin, moxifloxacin, norfloxacin and ofloxacin in superficial and wastewater samples. For that, an octyl restricted-access media bovine serum albumin column (RAM-BSA C8) was used for sample clean-up, enrichment and analysis with quantitation carried out by tandem mass spectrometry. For water samples volumes of only 500μL the method provided good selectivity, extraction efficiency, accuracy, and precision with quantification limits in the order of 20-150ngL(-1). Out of the six fluoroquinolones only ciprofloxacin (195ngL(-1)) and norfloxacin (270ngL(-1)) were quantified in an influent sample of the wastewater treatment plant (WWTP) of São Carlos (SP, Brazil). None were found in the superficial water samples analyzed. The capability of injecting native sample in an automated mode provides high productivity and represents a greener approach in environmental sample analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

Analysis of potential migrants from plastic materials in milk by liquid chromatography-mass spectrometry with liquid-liquid extraction and low-temperature purification.

PubMed

Bodai, Zsolt; Szabó, Bálint Sámuel; Novák, Márton; Hámori, Susanne; Nyiri, Zoltán; Rikker, Tamás; Eke, Zsuzsanna

2014-10-15

A simple and fast analytical method was developed for the determination of six UV stabilizers (Cyasorb UV-1164, Tinuvin P, Tinuvin 234, Tinuvin 326, Tinuvin 327, and Tinuvin 1577) and five antioxidants (Irgafos 168, Irganox 1010, Irganox 3114, Irganox 3790, and Irganox 565) in milk. For sample preparation liquid-liquid extraction with low-temperature purification combined with centrifugation was used to remove fats, proteins, and sugars. After the cleanup step, the sample was analyzed with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). External standard and matrix calibrations were tested. External calibration proved to be acceptable for Tinuvin P, Tinuvin 234, Tinuvin 326, Tinuvin 327, Irganox 3114, and Irganox 3790. The method was successfully validated with matrix calibration for all compounds. Method detection limits were between 0.25 and 10 μg/kg. Accuracies ranged from 93 to 109%, and intraday precisions were <13%.

Rapid determination of organochlorine pesticides and polychlorinated biphenyls, using selected ion monitoring mass spectrometry

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

Hargesheimer, E.E.

Methane chemical ionization (CI)-selected ion monitoring (SIM) mass spectrometry was used to identify and conclusively distinguish 19 organochlorine pesticides from polychlorinated biphenyls (PCBs) at parts-per-trillion to parts-per-billion levels in environmental water sample extracts with minimal sample cleanup. Two CI-SIM screens were developed. One set of ions scanned specifically for the presence of 4 classes of pesticides; diphenylmethane derivatives, bridged polycyclic chlorinated benzenes, and acetanilide pesticides. The second set of ions responded exclusively to PCBs with biphenyl moieties containing from 1 to 8 chlorine atoms. Eight commercial Aroclor mixtures were analyzed and distinguished from the pesticides groups. The detection limit formore » pesticides and PCBs by CI-SIM screening was 0.005 and 0.1 ppB, respectively. CI-SIM can be used as an alternative method for the analysis of biological or environmental samples containing interferences that complicate the detection of PCBs and chlorinated pesticides. 8 references, 6 figures, 6 tables.« less

High Throughput Determination of VX in Drinking Water by ...

EPA Pesticide Factsheets

Methods Report This document provides the standard operating procedure for determination of the chemical warfare agent VX (O-Ethyl S-2-Diisopropylamino-Ethyl Methylphosphonothioate) in drinking water by isotope dilution liquid chromatography tandem mass spectrometer (LC/MS/MS). This method was adapted from one that was initially developed by the Centers for Disease Control and Prevention, in the National Center for Environmental Health for the determination and quantitation of VX in aqueous matrices. This method is designed to support site-specific cleanup goals of environmental remediation activities following a homeland security incident involving this analyte.

Computer-Aided Remote Driving

NASA Technical Reports Server (NTRS)

Wilcox, Brian H.

1994-01-01

System for remote control of robotic land vehicle requires only small radio-communication bandwidth. Twin video cameras on vehicle create stereoscopic images. Operator views cross-polarized images on two cathode-ray tubes through correspondingly polarized spectacles. By use of cursor on frozen image, remote operator designates path. Vehicle proceeds to follow path, by use of limited degree of autonomous control to cope with unexpected conditions. System concept, called "computer-aided remote driving" (CARD), potentially useful in exploration of other planets, military surveillance, firefighting, and clean-up of hazardous materials.

Low-cost humic acid-bonded silica as an effective solid-phase extraction sorbent for convenient determination of aflatoxins in edible oils.

PubMed

Zhou, Neng-Zhi; Liu, Ping; Su, Xiao-Chuan; Liao, Yan-Hua; Lei, Ning-Sheng; Liang, Yong-Hong; Zhou, Shao-Huan; Lin, Wen-Si; Chen, Jie; Feng, Yu-Qi; Tang, Yang

2017-06-01

Aflatoxins (AFs) are highly toxic, mutagenic, carcinogenic, and teratogenic secondary metabolites produced by the toxigenic fungi Aspergillus flavus and Aspergillus parasiticus. AFs tend to contaminate a wide range of foods which is a serious and recurring food safety problem worldwide. Currently, immunoaffinity chromatography (IAC) has become the most conventional sample clean-up method for determining AFs in foodstuffs. However, IAC method is limited in the large-scale food analysis because it requires the use of expensive disposable cartridges and the IA procedure is time-consuming. Herein, to achieve the cost-effective determination of AFs in edible oils, we developed a promising solid-phase extraction (SPE) method based on commercially available humic acid-bonded silica (HAS) sorbent, followed by high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS) analysis. In HAS-SPE, AFs can be captured by the HAS sorbent with both hydrophobic and hydrophilic interactions, whereas the oil matrix was captured only with the hydrophobic interactions. The oil matrix can be sufficiently washed off with isopropanol, while the AFs were still retained on the SPE packing, thus achieving selective extraction of AFs and clean-up of oil matrices. Under the optimal conditions of HAS-SPE, satisfactory recoveries ranging from 82% to 106% for four AFs (B 1 , B 2 , G 1 , and G 2 ) were achieved in various oil matrices, containing blended oil, tea oil, rapeseed oil, peanut oil, sunflower seed oil, corn oil, blended olive oil, rice oil, soybean oil, and sesame oil. Only minor matrix effects ranging from 99% to 105% for four AFs were observed. Moreover, the LODs of AFs between 0.012 and 0.035 μg/kg completely meet the regulatory levels fixed by the EU, China or other countries. The methodology was further validated for assaying the naturally contaminated peanut oils, and consistent results between the HAS-SPE and the referenced IAC were obtained. In addition, HAS-SPE can directly treat diluted oil sample without liquid-liquid extraction and is automatable, thus making it simple and convenient for the large-scale determination of AFs in edible oils. Using this method, we successfully detected four AFs in the naturally contaminated peanut oils, which is, to the best of our knowledge, the first report about the determination of AFs in edible oils using HA-based SPE. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of phthalate esters in soil using a quick, easy, cheap, effective, rugged, and safe method followed by GC-MS.

PubMed

Liu, Qianjun; Chen, Di; Wu, Jiyuan; Yin, Guangcai; Lin, Qintie; Zhang, Min; Hu, Huawen

2018-04-01

A quick, easy, cheap, effective, rugged, and safe procedure was designed to extract pesticide residues from fruits and vegetables with a high percentage of water. It has not been used extensively for the extraction of phthalate esters from sediments, soils, and sludges. In this work, this procedure was combined with gas chromatography with mass spectrometry to determine 16 selected phthalate esters in soil. The extraction efficiency of the samples was improved by ultrasonic extraction and dissolution of the soil samples in ultra-pure water, which promoted the dispersion of the samples. Furthermore, we have simplified the extraction step and reduced the risk of organic solvent contamination by minimizing the use of organic solvents. Different extraction solvents and clean-up adsorbents were compared to optimize the procedure. Dichloromethane/n-hexane (1:1, v/v) and n-hexane/acetone (1:1, v/v) were selected as the extractants from the six extraction solvents tested. C18/primary secondary amine (1:1, m/m) was selected as the sorbent from the five clean-up adsorbents tested. The recoveries from the spiked soils ranged from 70.00 to 117.90% with relative standard deviation values of 0.67-4.62%. The proposed approach was satisfactorily applied for the determination of phthalate esters in 12 contaminated soil samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimization of a new method for extraction of cyanidin chloride and pelargonidin chloride anthocyanins with magnetic solid phase extraction and determination in fruit samples by HPLC with central composite design.

PubMed

Yari, Abdollah; Rashnoo, Saba

2017-11-01

Here, we are reporting a sensitive, simple and rapid method for the analysis of cyanidin chloride and pelargonidin chloride anthocyanins in cherry, sour cherry, pomegranate and barberry produced in Iran. The analytes were extracted with acetonitrile-hydrochloric acid (1% v/v) mixture under optimized pretreatment conditions. Clean-up of the extract from fruits was conducted by magnetic solid phase extraction using salicylic acid functionalized silica-coated magnetite nanoparticles (SCMNPs) as the adsorbent. The optimized conditions searched with central composite design. Working under optimum conditions specified as: SCMNPs modified with salicylic acid, sorbent contact time and sample 10min, mechanical stirring time 57.3min. HPLC with UV-detection was used for determination of the analytes. The limit of detection, LOD, obtained for the two anthocyanins were 0.02 and 0.03μgg -1 , respectively. The ranges of the spiked recoveries were 80.0-97.6 and 72.9-97.2%, with the relative standard deviations (RSD) of 2.1 and 2.5%, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation of [13C3]-melamine and [13C3]-cyanuric acid and their application to the analysis of melamine and cyanuric acid in meat and pet food using liquid chromatography-tandem mass spectrometry.

PubMed

Varelis, P; Jeskelis, R

2008-10-01

For the determination of melamine and cyanuric acid the labelled internal standards [(13)C(3)]-melamine and [(13)C(3)]-cyanuric acid were synthesized using the common substrate [(13)C(3)]-cyanuric chloride by reaction with ammonia and acidified water, respectively. Standards with excellent isotopic and chemical purities were obtained in acceptable yields. These compounds were used to develop an isotope dilution liquid chromatography/mass spectrometry (LC/MS) method to determine melamine and cyanuric acid in catfish, pork, chicken, and pet food. The method involved extraction into aqueous methanol, liquid-liquid extraction and ion exchange solid phase clean-up, with normal phase high-performance liquid chromatography (HPLC) in the so-called hydrophilic interaction mode. The method had a limit of detection (LOD) of 10 microg kg(-1) for both melamine and cyanuric acid in the four foods with a percentage coefficient of variation (CV) of less than 10%. The recovery of the method at this level was in the range of 87-110% and 96-110% for melamine and cyanuric acid, respectively.

Determination of perfluorinated alkylated substances in sediments and sediment core from the Gulf of Gdańsk, Baltic Sea.

PubMed

Falandysz, Jerzy; Rostkowski, Paweł; Jarzyńska, Grażyna; Falandysz, Jaromir J; Taniyasu, Sachi; Yamashita, Nobuyoshi

2012-01-01

Perfluorinated alkylated substances (PFAS) have been determined in surface sediments and sediment core from Gulf of Gdańsk, Baltic Sea. Perfluorooctanesulphonate (PFOS), perfluorohexanesulphonate (PFHxS), perfluorodecanoate (PFDA), perfluoronanoate (PFNA), perfluorooctanoate (PFOA), perfluoroheptanoate (PFHpA), perfluoroundecanote (PFUnDA), perfluorododecanoate (PFDoDA) and perfluorohexanoate (PFHxA) were quantified after isotopic dilution ((13)C(4) PFOS and (13)C(4) PFOA), liquid-liquid extractions by methanol and acetonitrile, cleanup by Envi-Carb, OasisWAX and Envi-Carb and final measurement by HPLC-MS/MS. PFOS, PFHxS, PFUnDA, PFDA, PFNA and PFOA were found in Baltic Sea sediments in concentrations exceeding the method limit of quantification (LOQ) of 2 pg/g. PFOS was detected in concentration up to 0.896 ng/g dry weight and PFHxS up to 0.326 ng/g dw, which shows on a weak pollution. PFOS (48-74%) or PFHxS (45-56%) dominated in PFAS composition of sediments surveyed. Supplemental materials are available for this article. Go to the publisher's online edition of the Journal of Environmental Science and Health, Part A to view the free supplemental file.

MSPD procedure for determining buprofezin, tetradifon, vinclozolin, and bifenthrin residues in propolis by gas chromatography-mass spectrometry.

PubMed

dos Santos, Thaíse Fernanda Santana; Aquino, Adriano; Dórea, Haroldo Silveira; Navickiene, Sandro

2008-03-01

A simple and effective extraction method based on matrix solid-phase dispersion (MSPD) was developed to determine bifenthrin, buprofezin, tetradifon, and vinclozolin in propolis using gas chromatography-mass spectrometry in selected ion monitoring mode (GC-MS, SIM). Different method conditions were evaluated, for example type of solid phase (C(18), alumina, silica, and Florisil), the amount of solid phase and eluent (n-hexane, dichloromethane, dichloromethane-n-hexane (8:2 and 1:1, v/v) and dichloromethane-ethyl acetate (9:1, 8:2 and 7:3, v/v)). The best results were obtained using 0.5 g propolis, 1.0 g silica as dispersant sorbent, 1.0 g Florisil as clean-up sorbent, and dichloromethane-ethyl acetate (9:1, v/v) as eluting solvent. The method was validated by analysis of propolis samples fortified at different concentration levels (0.25 to 1.0 mg kg(-1)). Average recoveries (four replicates) ranged from 67% to 175% with relative standard deviation between 5.6% and 12.1%. Detection and quantification limits ranged from 0.05 to 0.10 mg kg(-1) and 0.15 to 0.25 mg kg(-1) propolis, respectively.

A simple and green analytical method for determination of glyphosate in commercial formulations and water by diffuse reflectance spectroscopy

NASA Astrophysics Data System (ADS)

da Silva, Aline Santana; Fernandes, Flávio Cesar Bedatty; Tognolli, João Olímpio; Pezza, Leonardo; Pezza, Helena Redigolo

2011-09-01

This article describes a simple, inexpensive, and environmentally friendly method for the monitoring of glyphosate using diffuse reflectance spectroscopy. The proposed method is based on reflectance measurements of the colored compound produced from the spot test reaction between glyphosate and p-dimethylaminocinnamaldehyde ( p-DAC) in acid medium, using a filter paper as solid support. Experimental designs were used to optimize the analytical conditions. All reflectance measurements were carried out at 495 nm. Under optimal conditions, the glyphosate calibration graphs obtained by plotting the optical density of the reflectance signal (A R) against the concentration were linear in the range 50-500 μg mL -1, with a correlation coefficient of 0.9987. The limit of detection (LOD) for glyphosate was 7.28 μg mL -1. The technique was successfully applied to the direct determination of glyphosate in commercial formulations, as well as in water samples (river water, pure water and mineral drinking water) after a previous clean-up or pre-concentration step. Recoveries were in the ranges 93.2-102.6% and 91.3-102.9% for the commercial formulations and water samples, respectively.

Determination of six pesticides in the medicinal herb Cordia salicifolia by matrix solid-phase dispersion and gas chromatography/mass spectrometry.

PubMed

de Carvalho, Pedro Henrique Viana; Prata, Vanessa de Menezes; Alves, Péricles Barreto; Navickiene, Sandro

2009-01-01

A simple and effective extraction method based on matrix solid-phase dispersion was developed for acephate, chlorpropham, pyrimicarb, bifenthrin, tetradifon, and phosalone in leaves of the medicinal plant Cordia salicifolia, whose extracts are commercialized in Brazil as diuretic, appetite suppressant, and weight loss products. The determination method was GC/MS with selected-ion monitoring. Different parameters of the method were evaluated, such as type of solid phase (C18, alumina, silica gel, and Florisil) and the amount of solid phase and eluent (dichloromethane, ethyl acetate, chloroform, and cyclohexane). The best results were obtained using 0.5 g herb sample, 0.5 g neutral alumina as the dispersant sorbent, 0.5 g C18 as the cleanup sorbent, and cyclohexane-dichloromethane (3 + 1, v/v) as the eluting solvent. The method was validated using herb samples fortified with pesticides at different concentration levels (0.3, 0.5, and 1.0 mg/kg). Average recoveries (seven replicates) ranged from 67.7 to 129.9%, with relative standard deviations between 6.3 and 26%. Detection and quantitation limits for the herb ranged from 0.10 to 0.15 and 0.15 to 0.25 mg/kg, respectively.

A simple and green analytical method for determination of glyphosate in commercial formulations and water by diffuse reflectance spectroscopy.

PubMed

da Silva, Aline Santana; Fernandes, Flávio Cesar Bedatty; Tognolli, João Olímpio; Pezza, Leonardo; Pezza, Helena Redigolo

2011-09-01

This article describes a simple, inexpensive, and environmentally friendly method for the monitoring of glyphosate using diffuse reflectance spectroscopy. The proposed method is based on reflectance measurements of the colored compound produced from the spot test reaction between glyphosate and p-dimethylaminocinnamaldehyde (p-DAC) in acid medium, using a filter paper as solid support. Experimental designs were used to optimize the analytical conditions. All reflectance measurements were carried out at 495 nm. Under optimal conditions, the glyphosate calibration graphs obtained by plotting the optical density of the reflectance signal (AR) against the concentration were linear in the range 50-500 μg mL(-1), with a correlation coefficient of 0.9987. The limit of detection (LOD) for glyphosate was 7.28 μg mL(-1). The technique was successfully applied to the direct determination of glyphosate in commercial formulations, as well as in water samples (river water, pure water and mineral drinking water) after a previous clean-up or pre-concentration step. Recoveries were in the ranges 93.2-102.6% and 91.3-102.9% for the commercial formulations and water samples, respectively. Copyright © 2011 Elsevier B.V. All rights reserved.

Determination of ochratoxin A in traditional Chinese medicinal plants by HPLC-FLD.

PubMed

Yang, Lei; Wang, Linan; Pan, Jianyu; Xiang, Lan; Yang, Meihua; Logrieco, Antonio F

2010-07-01

Traditional Chinese medicinal plants (TCMPs), commonly used as spices, additives or foods, are also widely used in China to prevent and cure human disease. Due to their provenance, TCMPs may be contaminated by various fungal species, including ochratoxigenic fungi, during growth, collection, transportation and, especially, storage. A reliable method for the determination of ochratoxin A (OTA) in TCMPs of different origins was developed to monitor OTA levels in China. Analyses involved the extraction of OTA by methanol/water, immunoaffinity column (IAC) clean-up and HPLC quantification with fluorescence detection (FLD). Positive results were further confirmed by LC-ESI-MS/MS. The limit of detection (LOD) was 0.3 microg kg(-1), based on a signal-to-noise ratio of 3 : 1. Among the total of 57 TCMPs samples collected from six different areas, 31 were visibly moldy due to inappropriate storage; 26 sample, purchased from local TCMPs markets, were not visibly moldy. The results showed that 23 of the visibly moldy samples and two of the not visibly moldy were contaminated with OTA at levels ranging 1.2-158.7 and 2.5-5.6 microg kg(-1), respectively. This is the first report of the natural occurrence of OTA in TCMPs.

Determination of aminophenols and phenol in hair colorants by ultrasound-assisted solid-phase dispersion extraction coupled with ion chromatography.

PubMed

Zhong, Zhixiong; Li, Gongke; Wu, Rong; Zhu, Binghui; Luo, Zhibin

2014-08-01

A simple and reliable ultrasound-assisted solid-phase dispersion extraction coupled with ion chromatography was developed for the determination of aminophenols and phenol. The highly viscous hair colorant was dispersed in solvents using anhydrous sodium sulfite having dual functions of dispersant and antioxidant. The use of anhydrous sodium sulfite did not change the sample volume because it could completely dissolve in solution after matrix dispersion. The extraction and cleanup were combined in one single step for simplifying operation. The extraction process could be rapidly accomplished within 9 min with high sample throughput under the synergistic effects of vibration, ultrasound, and heating. Satisfactory linearity was observed with correlation coefficients higher than 0.9992, and the limits of detection varied from 0.02 to 0.09 mg/L. The applicability of the proposed method was demonstrated by measuring the concentrations of aminophenols and phenol in 32 different commercial hair color products. The recoveries ranged from 86.4-101.2% with the relative standard deviations in the range of 0.52-4.3%. The method offers an attractive alternative for the analysis of trace phenols in complex matrices. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Air-assisted liquid-liquid microextraction integrated with QuEChERS for determining endocrine-disrupting compounds in fish by high-performance liquid chromatography-tandem mass spectrometry.

PubMed

Luo, Zhoufei; Lu, Jing; Li, Haipu; Tu, Yi; Wan, Yuehao; Yang, Zhaoguang

2018-09-15

A new, sensitive, and rapid method based on the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) approach and air-assisted liquid-liquid microextraction (AALLME) technology was developed for the determination of 20 endocrine-disrupting compounds (EDCs) in fish by high-performance liquid chromatography-tandem mass spectrometry. The method first integrates AALLME into QuEChERS to achieve clean-up and enrichment of the EDCs in one step. A self-made glass tube was enfolded with plasticine to withstand the high centrifugal force. The established method was developed by optimization of the parameters. High linearities (R 2  > 0.9924) and recoveries (78.2-118.6%) at three spiked levels (5, 10, and 20 ng g -1 ), and low relative standard deviation values (1.1-14.5%) and limits of detection (0.03-0.80 ng g -1 ) were obtained. The method comparison shows that the proposed method is superior as it involves less organic solvent usage, simple operation and high efficiency. This method was successfully applied to different fishes for analyzing EDCs. Copyright © 2018 Elsevier Ltd. All rights reserved.

Risk-Based Decision Making Case Study: Application at a Superfund Cleanup.

ERIC Educational Resources Information Center

Blacker, Stanley; Goodman, Daniel

1994-01-01

Describes a case study comparing an integrated approach to Superfund cleanup with traditional approaches at a particular Superfund site. Emphasizes ways to save time and money while still achieving the desired risk reduction level. (LZ)

IMMUNOASSAY ANALYSIS FOR CHLORPYRIFOS IN FOODS

EPA Science Inventory

Chlorpyrifos is widely used in agriculture on fruits and vegetables. The tolerances for chlorpyrifos on produce range from 0.1-8.0 ppm. Residue detection is commonly performed by gas chromatography following various cleanup procedures. However, the required cleanup can make ...

Considering Traditional Ecological Knowledge (TEK) During the Cleanup Process

EPA Pesticide Factsheets

This memorandum provides direction to improve the decision-making process as it relates to site assessment, characterization, and cleanup activities, to ensure EPA's Office of Land and Emergency Management is considering TEK when tribes provide it to EPA.

Automated multi-plug filtration cleanup for liquid chromatographic-tandem mass spectrometric pesticide multi-residue analysis in representative crop commodities.

PubMed

Qin, Yuhong; Zhang, Jingru; Zhang, Yuan; Li, Fangbing; Han, Yongtao; Zou, Nan; Xu, Haowei; Qian, Meiyuan; Pan, Canping

2016-09-02

An automated multi-plug filtration cleanup (m-PFC) method on modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts was developed. The automatic device was aimed to reduce labor-consuming manual operation workload in the cleanup steps. It could control the volume and the speed of pulling and pushing cycles accurately. In this work, m-PFC was based on multi-walled carbon nanotubes (MWCNTs) mixed with other sorbents and anhydrous magnesium sulfate (MgSO4) in a packed tip for analysis of pesticide multi-residues in crop commodities followed by liquid chromatography with tandem mass spectrometric (LC-MS/MS) detection. It was validated by analyzing 25 pesticides in six representative matrices spiked at two concentration levels of 10 and 100μg/kg. Salts, sorbents, m-PFC procedure, automated pulling and pushing volume, automated pulling speed, and pushing speed for each matrix were optimized. After optimization, two general automated m-PFC methods were introduced to relatively simple (apple, citrus fruit, peanut) and relatively complex (spinach, leek, green tea) matrices. Spike recoveries were within 83 and 108% and 1-14% RSD for most analytes in the tested matrices. Matrix-matched calibrations were performed with the coefficients of determination >0.997 between concentration levels of 10 and 1000μg/kg. The developed method was successfully applied to the determination of pesticide residues in market samples. Copyright © 2016 Elsevier B.V. All rights reserved.

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

EPA Pesticide Factsheets

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

40 CFR 761.366 - Cleanup equipment.

Code of Federal Regulations, 2010 CFR

2010-07-01

... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Cleanup equipment. 761.366 Section 761.366 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT POLYCHLORINATED BIPHENYLS (PCBs) MANUFACTURING, PROCESSING, DISTRIBUTION IN COMMERCE, AND USE PROHIBITIONS Double...

40 CFR 761.120 - Scope.

Code of Federal Regulations, 2010 CFR

2010-07-01

... with the particular spill. These factors may mitigate expected exposures and risks or make cleanup to... spill situations in which site-specific risk factors may warrant additional cleanup to more stringent... numerical decontamination levels is clearly unwarranted because of risk-mitigating factors, that compliance...

40 CFR 761.120 - Scope.

Code of Federal Regulations, 2011 CFR

2011-07-01

... with the particular spill. These factors may mitigate expected exposures and risks or make cleanup to... spill situations in which site-specific risk factors may warrant additional cleanup to more stringent... numerical decontamination levels is clearly unwarranted because of risk-mitigating factors, that compliance...

Notification: CTS Asheville Superfund Site Update: Sampling, Monitoring, Communication and Opportunities for Cleanup Efficiencies

EPA Pesticide Factsheets

Project #OPE-FY14-0044, July 22, 2014. The EPA OIG plans to begin preliminary research of the EPA's sampling, monitoring, communication and opportunities for cleanup efficiencies for the CTS Asheville Superfund Site, North Carolina.

Plating Inc. Site Fact Sheet: EPA to Begin Cleanup of Hazardous Waste

EPA Pesticide Factsheets

Hazardous waste cleanup and local community outreach around the Plating Inc. site at 888 N. Prior Ave.in St. Paul. The former industrial facility specialized in zinc and chromate plating of aluminum and is now abandoned.

48 CFR 970.1504-1-9 - Special considerations: Cost-plus-award-fee.

Code of Federal Regulations, 2012 CFR

2012-10-01

....e., nuclear energy processing, industrial environmental cleanup); (iii) Construction of facilities... industrial/DOE settings (i.e., nuclear energy, chemical or petroleum processing, industrial environmental... industrial/DOE settings (i.e., nuclear energy, chemical processing, industrial environmental cleanup); (ii...

48 CFR 970.1504-1-9 - Special considerations: Cost-plus-award-fee.

Code of Federal Regulations, 2014 CFR

2014-10-01

....e., nuclear energy processing, industrial environmental cleanup); (iii) Construction of facilities... industrial/DOE settings (i.e., nuclear energy, chemical or petroleum processing, industrial environmental... industrial/DOE settings (i.e., nuclear energy, chemical processing, industrial environmental cleanup); (ii...

48 CFR 970.1504-1-9 - Special considerations: Cost-plus-award-fee.

Code of Federal Regulations, 2013 CFR

2013-10-01

....e., nuclear energy processing, industrial environmental cleanup); (iii) Construction of facilities... industrial/DOE settings (i.e., nuclear energy, chemical or petroleum processing, industrial environmental... industrial/DOE settings (i.e., nuclear energy, chemical processing, industrial environmental cleanup); (ii...

A Decision-Making Framework for Cleanup of Sites Impacted with Light Non-Aqueous Phase Liquids (LNAPL)

EPA Pesticide Factsheets

This document has been prepared by the Remediation Technologies Development Forum (RTDF) NAPL Cleanup Alliance to provide a guide to practicable and reasonable approaches for management of LNAPL petroleum hydrocarbons in the subsurface.