Sample records for sample clean-up step
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Goryacheva, I Yu; De Saeger, S; Lobeau, M; Eremin, S A; Barna-Vetró, I; Van Peteghem, C
2006-09-01
An approach for ochratoxin A (OTA) fast cost-effective screening based on clean-up tandem immunoassay columns was developed and optimized for OTA detection with a cut-off level of 10 microg kg(-1) in spices. Two procedures were tested and applied for OTA detection. Column with bottom detection immunolayer was optimized for OTA determination in Capsicum ssp. spices. A modified clean-up tandem immunoassay procedure with top detection immunolayer was successfully applied for all tested spices. Its main advantages were decreasing of the number of analysis steps and quantity of antibody and also minimizing of matrix effects. The total duration of the extraction and analysis was about 40 min for six samples. Chilli, red pepper, pili-pili, cayenne, paprika, nutmeg, ginger, white pepper and black pepper samples were analyzed for OTA contamination by the proposed clean-up tandem immunoassay procedures. Clean-up tandem immunoassay results were confirmed by HPLC-MS/MS with immunoaffinity column clean-up. Among 17 tested Capsicum ssp. spices, 6 samples (35%) contained OTA in a concentration exceeding the 10 microg kg(-1) limit discussed by the European Commission. All tested nutmeg (n=8), ginger (n=5), white pepper (n=7) and black pepper (n=6) samples did not contain OTA above this action level.
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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 (
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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.
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Goryacheva, Irina Yu; De Saeger, Sarah; Nesterenko, Irina S; Eremin, Sergei A; Van Peteghem, Carlos
2007-05-15
A feasible three-step method for ochratoxin A (OTA) rapid detection was developed and applied for OTA screening in high-coloured matrices such as liquorice, ginger, nutmeg, black pepper, white pepper and Capsicum spp. spices at a control level of 10mugkg(-1). The method was based on the clean-up tandem immunoassay column and involved three steps: extract application, washing step and application of chromogenic substrate. A significant simplification of the assay was reached by using an additional frit with conjugate inside the clean-up tandem immunoassay column. The time for analysis was less than 10min, including 5min for colour development. Results were visually evaluated as colour development for negative result or no colour development for positive result. The method was coupled with a simple methanol-based extraction. A total of 27 samples were screened for OTA with the proposed method. It was shown that two samples of red pepper and one sample of liquorice, pili-pili, chilli and cayenne were contaminated with OTA above the control level at 10mugkg(-1), but none of tested ginger, nutmeg, black pepper and white pepper.
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Mikolajczuk, Agnieszka; Przyk, Elzbieta Perez; Geypens, Benny; Berglund, Michael; Taylor, Philip
2010-03-01
Compound specific isotopic analysis (CSIA) can provide information about the origin of analysed compounds - in this case, polycyclic aromatic hydrocarbons (PAHs). In the study, PAHs were extracted from three dust samples: winter and summer filter dust and tunnel dust. The measurement was performed using the method validated in our laboratory using pure, solid compounds and EPA 610 reference assortment. CSIA required an appropriate clean-up method to avoid an unresolved complex in the gas chromatographic analysis usually found in the chromatography of PAHs. Extensive sample clean-up for this particular matrix was found to be necessary to obtain good gas chromatography-combustion-isotope ratio mass spectrometry analysis results. The sample purification method included two steps in which the sample is cleaned up and the aliphatic and aromatic hydrocarbons are separated. The concentration of PAHs in the measured samples was low; so a large volume injection technique (100 microl) was applied. The delta(VPDB)(13)C was measured with a final uncertainty smaller than 1 per thousand. Comparison of the delta(VPDB)(13)C signatures of PAHs extracted from different dust samples was feasible with this method and, doing so, significant differences were observed.
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Tubaon, Ria Marni; Haddad, Paul R; Quirino, Joselito P
2017-03-10
The presence of inorganic anions in a sample interferes with mass spectrometric (MS) analysis. Here, a simple method to remove these ions from a liquid sample in one-step is described. The inorganic anions present in a 50μL sample were extracted into a low pH solution inside a 200μm i.d.×33cm long capillary by the use of an electric field. The selective removal of unwanted anions and retention of target analytes was accomplished by control of the apparent electrophoretic velocities of anions and analytes at a boundary that separated the sample and extraction solution. No physical barrier (e.g., membrane) was required and with the boundary situated at the tip of the capillary, efficient removal of inorganic anions (e.g., >80% removal) and good recovery of target analytes (e.g., >80% recovery) were achieved. The time required for removal of the inorganic anions was found to depend on their initial concentrations. The removal process was investigated using different concentrations of bromide and nitrate (as potassium salts) and negatively chargeable drugs as target analytes. This micro-sample clean-up technique used no organic solvents and little consumables and was studied to the determination of 0.6μg/L arsenic and 8.3μg/L vanadium in 500mg/L sodium chloride using inductively coupled plasma MS and 50μM angiotensin I in 1000mg/L sodium chloride using electrospray ionisation MS. Micro-sample clean-up was performed for 45min at 3kV in both demonstrations. The calculated recoveries for the metals at trace levels were 110-130%, and for the peptide was 103.8%. Copyright © 2017 Elsevier B.V. All rights reserved.
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Gebbink, Wouter A; Ullah, Shahid; Sandblom, Oskar; Berger, Urs
2013-11-01
Polyfluoroalkyl phosphate mono-, di-, and tri-esters (mono-, di-, and triPAPs) are used to water- and grease-proof food packaging materials, and these chemicals are known precursors to perfluoroalkyl carboxylic acids (PFCAs). Existing analytical methods for PAPs lack sample clean-up steps in the sample preparation. In the present study, a method based on ultra performance liquid chromatography coupled to tandem mass spectrometry (UPLC/MS/MS) was developed and optimized for the analysis of mono-, di-, and triPAPs, including a clean-up step for the raw extracts. The method was applied to food samples and their PAP-containing packaging materials. The optimized UPLC/MS/MS method enabled the separation and identification of a total of 4 monoPAPs, 16 diPAPs, and 7 triPAPs in the technical mixture Zonyl®-RP. For sample clean-up, weak anion exchange solid phase extraction columns were tested. PAPs standard solutions spiked onto the columns were separated into a fraction containing neutral compounds (triPAPs) and a fraction with ionic compounds (mono- and diPAPs) with recoveries between 72-110%. Method limits of quantification for food samples were in the sub to low picogram per gram range. For quantitative analysis of PAPs, compound-specific labeled internal standards showed to be essential as sorption and matrix effects were observed. Mono-, di-, and/or triPAPs were detected in all food packaging materials obtained from the Swedish market. Up to nine diPAPs were detected in the food samples, with the 6:2/6:2 and 6:2/8:2 diPAPs as the dominant compounds. DiPAP concentrations in the food samples ranged from 0.9 to 36 pg/g, which was comparable to individual PFCA concentrations in the same samples. Consumption of food packed in PAP-containing materials could be an indirect source of human exposure to PFCAs.
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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.
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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.
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Impact of pH on the stability and the cross-reactivity of ochratoxin A and citrinin.
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.
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Impact of pH on the Stability and the Cross-Reactivity of Ochratoxin A and Citrinin
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
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Strengthening Clean Energy Technology Cooperation under the UNFCCC: Steps toward Implementation
DOE Office of Scientific and Technical Information (OSTI.GOV)
Benioff, R.; de Coninck, H.; Dhar, S.
2010-08-01
Development of a comprehensive and effective global clean technology cooperation framework will require years of experimenting and evaluation with new instruments and institutional arrangements before it is clear what works on which scale and in which region or country. In presenting concrete examples, this paper aims to set the first step in that process by highlighting successful models and innovative approaches that can inform efforts to ramp up clean energy technology cooperation. This paper reviews current mechanisms and international frameworks for global cooperation on clean energy technologies, both within and outside of the UNFCCC, and provides selected concrete options formore » scaling up global cooperation on clean energy technology RD&D, enabling environment, and financing.« less
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Pastor-Belda, Marta; Campillo, Natalia; Hernández-Córdoba, Manuel; Viñas, Pilar
2016-06-01
A rapid and simple procedure is reported for the determination of six ethylene glycol ethers in cleaning products and detergents using gas chromatography with mass spectrometry. The analytes were extracted from 2.0 g samples in acetonitrile (3 mL) and the extract was submitted to a clean-up step by QuEChERS method, using a mixture containing 0.3 g magnesium sulfate, 0.15 g primary/secondary amine, and 0.05 g C18 . The clean acetonitrile extract (1 μL) was injected into the chromatographic system. No matrix effect was observed, so the quantification of the samples was carried out against external standards. Detection limits were in the range 3.0-27 ng/g for the six ethylene glycol ethers. The recoveries obtained, using the optimized procedure, were in the 89.4-118% range, with relative standard deviations lower than 14%. Twenty-three different household cleaning products, including glass cleaner, degreaser, floor, softeners, and clothes and dishwashing detergents, were analyzed. Large interindividual variations were observed between samples and compounds. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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High-throughput automated microfluidic sample preparation for accurate microbial genomics
Kim, Soohong; De Jonghe, Joachim; Kulesa, Anthony B.; Feldman, David; Vatanen, Tommi; Bhattacharyya, Roby P.; Berdy, Brittany; Gomez, James; Nolan, Jill; Epstein, Slava; Blainey, Paul C.
2017-01-01
Low-cost shotgun DNA sequencing is transforming the microbial sciences. Sequencing instruments are so effective that sample preparation is now the key limiting factor. Here, we introduce a microfluidic sample preparation platform that integrates the key steps in cells to sequence library sample preparation for up to 96 samples and reduces DNA input requirements 100-fold while maintaining or improving data quality. The general-purpose microarchitecture we demonstrate supports workflows with arbitrary numbers of reaction and clean-up or capture steps. By reducing the sample quantity requirements, we enabled low-input (∼10,000 cells) whole-genome shotgun (WGS) sequencing of Mycobacterium tuberculosis and soil micro-colonies with superior results. We also leveraged the enhanced throughput to sequence ∼400 clinical Pseudomonas aeruginosa libraries and demonstrate excellent single-nucleotide polymorphism detection performance that explained phenotypically observed antibiotic resistance. Fully-integrated lab-on-chip sample preparation overcomes technical barriers to enable broader deployment of genomics across many basic research and translational applications. PMID:28128213
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Determination of etoxazole residues in fruits and vegetables by SPE clean-up and HPLC-DAD.
Malhat, Farag; Badawy, Hany; Barakat, Dalia; Saber, Ayman
2013-01-01
A method for determination of etoxazole residues in apples, strawberries and green beans was developed and validated. The analyte was extracted with acetonitrile from foodstuff and a charcoal-celite cartridge was used for clean-up of raw extracts. Reversed phase high performance liquid chromatography with photodiode array detector (HPLC-DAD) was used for the determination and quantification of etoxazole residues in the studied samples. The calibration graphs of etoxazole in a solvent or three blank matrixes were linear within the tested intervals 0.01-2 mg L(-1), with correlation coefficient of determination >0.999. The combined solid phase extraction (SPE) clean-up and the chromatographic method steps were sensitive and reliable for simultaneous determination of etoxazole residues in the studied samples. The average recoveries of etoxazole in the tested foodstuffs were between 93.4 to 102% at spiking levels of 0.01, 0.10, and 0.50 mg kg(-1), with relative standard deviations ranging from 2.8 to 4.7%, in agreement with directives for method validation in residue analyses. The limit of detection (LOD) of the HPLC-DAD system was 100 pg. The limit of quantification of the entire method was 0.01 mg kg(-1).
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Zulfiqar, Adnan; Morgan, Geraint; Turner, Nicholas W
2014-10-07
A method capable of screening for multiple steroids in urine has been developed, using a series of twelve structurally similar, and commercially relevant compounds as target analytes. A molecularly imprinted solid phase extraction clean-up step was used to make the sample suitable for injection onto a GC×GC-MS setup. Significant improvements compared to a commercially available C-18 material were observed. Each individual steroid was able to be separated and identified, using both the retention profile and diagnostic fragmentation ion monitoring abilities of the comprehensive chromatographic-mass spectrometry method. Effective LODs of between 11.7 and 27.0 pg were calculated for individual steroids, effectively equivalent to concentration levels of between 0.234 and 0.540 ng mL(-1) in urine, while the application of multiple screen was demonstrated using a 10 ng mL(-1) mixed sample. The nature of this study also removes the need for sample derivitisation which speeds up the screening process.
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Plasma surface cleaning in a microwave plasma source
DOE Office of Scientific and Technical Information (OSTI.GOV)
Tsai, C.C.; Nelson, W.D.; Haselton, H.H.
1994-03-01
A microwave electron cyclotron resonance (ECR) plasma source has been operated to produce reactive plasmas of oxygen and its mixture with argon. Aluminum samples (0.95 cm by 1.9 cm) were coated with thin films (<20 {mu}m in thickness) of Shell Vitrea oil and cleaned by using such reactive plasmas. The plasma cleaning was done in discharge conditions of microwave power up to 1300 W, radio frequency power up to 200 W, biased potential up to 400 V, gas pressures up to 5 mtorr, and operating time up to 35 min. The surface texture of the postcleaned samples has been examinedmore » visually. Mass loss of the samples after plasma cleaning was measured to estimate cleaning rates. Measured clean rates of low-pressure (0.5-mtorr) argon/oxygen plasmas were as high as 2.7 {mu}m/min. X-ray photoelectron spectroscopy (XPS) was used to determine cleanliness of the sample surfaces after plasma cleaning. The XPS study on polished samples confirmed the effectiveness of plasma cleaning in achieving atomic level of surface cleanliness. In this technical memorandum plasma properties, cleaning phenomena, and significant results are reported and discussed.« less
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Clime, Liviu; Hoa, Xuyen D; Corneau, Nathalie; Morton, Keith J; Luebbert, Christian; Mounier, Maxence; Brassard, Daniel; Geissler, Matthias; Bidawid, Sabah; Farber, Jeff; Veres, Teodor
2015-02-01
Detecting pathogenic bacteria in food or other biological samples with lab-on-a-chip (LOC) devices requires several sample preparation steps prior to analysis which commonly involves cleaning complex sample matrices of large debris. This often underestimated step is important to prevent these larger particles from clogging devices and to preserve initial concentrations when LOC techniques are used to concentrate or isolate smaller target microorganisms for downstream analysis. In this context, we developed a novel microfluidic system for membrane-free cleaning of biological samples from debris particles by combining hydrodynamic focusing and inertial lateral migration effects. The microfluidic device is fabricated using thermoplastic elastomers being compatible with thermoforming fabrication techniques leading to low-cost single-use devices. Microfluidic chip design and pumping protocols are optimized by investigating diffusive losses numerically with coupled Navier-Stokes and convective-diffusion theoretical models. Stability of inertial lateral migration and separation of debris is assessed through fluorescence microscopy measurements with labelled particles serving as a model system. Efficiency of debris cleaning is experimentally investigated by monitoring microchip outlets with in situ optical turbidity sensors, while retention of targeted pathogens (i.e., Listeria monocytogenes) within the sample stream is assessed through bacterial culture techniques. Optimized pumping protocols can remove up to 50 % of debris from ground beef samples while percentage for preserved microorganisms can account for 95 % in relatively clean samples. However, comparison between inoculated turbid and clean samples (i.e., with and without ground beef debris) indicate some degree of interference between debris inertial lateral migration and hydrodynamic focusing of small microorganisms. Although this interference can lead to significant decrease in chip performance through loss of target bacteria, it remains possible to reach 70 % for sample recovery and more than 50 % for debris removal even in the most turbid samples tested. Due to the relatively simple design, the robustness of the inertial migration effect itself, the high operational flow rates and fabrication methods that leverage low-cost materials, the proposed device can have an impact on a wide range of applications where high-throughput separation of particles and biological species is of interest.
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NASA Technical Reports Server (NTRS)
Schmeling, M.; Burnett, D. S.; Allton, J. H.; Rodriquez, M.; Tripa, C. E.; Veryovkin, I. V.
2013-01-01
The Genesis mission was the first mission returning solar material to Earth since the Apollo program [1,2]. Unfortunately the return of the space craft on September 8, 2004 resulted in a crash landing, which shattered the samples into small fragments and exposed them to desert soil and other debris. Thus only small fragments of the original collectors are available, each having different degrees of surface contamination. Thorough surface cleaning is required to allow for subsequent analysis of solar wind material embedded within. An initial cleaning procedure was developed in coordination with Johnson Space Center which focused on removing larger sized particulates and a thin film organic contamination acquired during collection in space [3]. However, many of the samples have additional residues and more rigorous and/or innovative cleaning steps might be necessary. These cleaning steps must affect only the surface to avoid leaching and re-distribution of solar wind material from the bulk of the collectors. To aid in development and identification of the most appropriate cleaning procedures each sample has to be thoroughly inspected before and after each cleaning step. Laboratory based total reflection X-ray fluorescence (TXRF) spectrometry lends itself to this task as it is a non-destructive and surface sensitive analytical method permitting analysis of elements from aluminum onward present at and near the surface of a flat substrate [4]. The suitability of TXRF has been demonstrated for several Genesis solar wind samples before and after various cleaning methods including acid treatment, gas cluster ion beam, and CO2 snow jet [5 - 7]. The latter one is non-invasive and did show some promise on one sample [5]. To investigate the feasibility of CO2 snow jet cleaning further, several flown Genesis samples were selected to be characterized before and after CO2 snow application with sample 61052 being discussed below.
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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.
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The purpose of this SOP is to define the steps involved in cleaning the electronic data generated from data entry of the Follow Up Questionnaire. It applies to electronic data corresponding to the Follow Up Questionnaire that was scanned and verified by the data staff during the...
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The purpose of this SOP is to define the steps involved in cleaning the electronic data generated from data entry of the Follow Up Questionnaire. It applies to electronic data corresponding to the Follow Up Questionnaire that was scanned and verified by the Data Staff during the...
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The purpose of this SOP is to define the steps involved in cleaning the electronic data generated from data entry of the Food Diary Follow Up Questionnaire. It applies to electronic data corresponding to the Food Diary Follow Up Questionnaire that was scanned and verified by the...
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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.
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Jank, Louise; Martins, Magda Targa; Arsand, Juliana Bazzan; Hoff, Rodrigo Barcellos; Barreto, Fabiano; Pizzolato, Tânia Mara
2015-01-01
This study describes the development and validation procedures for scope extension of a method for the determination of β-lactam antibiotic residues (ampicillin, amoxicillin, penicillin G, penicillin V, oxacillin, cloxacillin, dicloxacillin, nafcillin, ceftiofur, cefquinome, cefoperazone, cephapirine, cefalexin and cephalonium) in bovine milk. Sample preparation was performed by liquid-liquid extraction (LLE) followed by two clean-up steps, including low temperature purification (LTP) and a solid phase dispersion clean-up. Extracts were analysed using a liquid chromatography-electrospray-tandem mass spectrometry system (LC-ESI-MS/MS). Chromatographic separation was performed in a C18 column, using methanol and water (both with 0.1% of formic acid) as mobile phase. Method validation was performed according to the criteria of Commission Decision 2002/657/EC. Main validation parameters such as linearity, limit of detection, decision limit (CCα), detection capability (CCβ), accuracy, and repeatability were determined and were shown to be adequate. The method was applied to real samples (more than 250) and two milk samples had levels above maximum residues limits (MRLs) for cloxacillin - CLX and cefapirin - CFAP.
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Islas, Gabriela; Hernandez, Prisciliano
2017-01-01
To achieve analytical success, it is necessary to develop thorough clean-up procedures to extract analytes from the matrix. Dispersive solid phase extraction (DSPE) has been used as a pretreatment technique for the analysis of several compounds. This technique is based on the dispersion of a solid sorbent in liquid samples in the extraction isolation and clean-up of different analytes from complex matrices. DSPE has found a wide range of applications in several fields, and it is considered to be a selective, robust, and versatile technique. The applications of dispersive techniques in the analysis of veterinary drugs in different matrices involve magnetic sorbents, molecularly imprinted polymers, carbon-based nanomaterials, and the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method. Techniques based on DSPE permit minimization of additional steps such as precipitation, centrifugation, and filtration, which decreases the manipulation of the sample. In this review, we describe the main procedures used for synthesis, characterization, and application of this pretreatment technique and how it has been applied to food analysis. PMID:29181027
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The purpose of this SOP is to define the steps involved in cleaning the electronic data generated from data entry of the Food Diary Follow Up Questionnaire. It applies to electronic data corresponding to the Food Diary Follow Up Questionnaire that was scanned and verified by the...
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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.
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Mycotoxin analysis: an update.
Krska, Rudolf; Schubert-Ullrich, Patricia; Molinelli, Alexandra; Sulyok, Michael; MacDonald, Susan; Crews, Colin
2008-02-01
Mycotoxin contamination of cereals and related products used for feed can cause intoxication, especially in farm animals. Therefore, efficient analytical tools for the qualitative and quantitative analysis of toxic fungal metabolites in feed are required. Current methods usually include an extraction step, a clean-up step to reduce or eliminate unwanted co-extracted matrix components and a separation step with suitably specific detection ability. Quantitative methods of analysis for most mycotoxins use immunoaffinity clean-up with high-performance liquid chromatography (HPLC) separation in combination with UV and/or fluorescence detection. Screening of samples contaminated with mycotoxins is frequently performed by thin layer chromatography (TLC), which yields qualitative or semi-quantitative results. Nowadays, enzyme-linked immunosorbent assays (ELISA) are often used for rapid screening. A number of promising methods, such as fluorescence polarization immunoassays, dipsticks, and even newer methods such as biosensors and non-invasive techniques based on infrared spectroscopy, have shown great potential for mycotoxin analysis. Currently, there is a strong trend towards the use of multi-mycotoxin methods for the simultaneous analysis of several of the important Fusarium mycotoxins, which is best achieved by LC-MS/MS (liquid chromatography with tandem mass spectrometry). This review focuses on recent developments in the determination of mycotoxins with a special emphasis on LC-MS/MS and emerging rapid methods.
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Pareja, Lucía; Cesio, Verónica; Heinzen, Horacio; Fernández-Alba, Amadeo R
2011-02-15
Four different extraction and clean-up protocols based on the QuEChERS method were compared for the development of an optimized sample preparation procedure for the multiresidue analysis of 16 commonly applied herbicides in rice crops using LC-QqQ/MS. Additionally the methods were evaluated for the analysis of 26 insecticides and fungicides currently used in rice crops. The methods comprise, in general, the hydratation of the sample with water followed by the extraction with acetonitrile, phase separation with the addition of different salts and finally a clean-up step with various sorbents. Matrix effects were evaluated for the 4 studied methods using LC-QqQ/MS. Additionally LC-TOF/MS was used to compare the co-extractants obtained with the four assayed methodologies. Thirty-six pesticides presented good performance with recoveries in the range 70-120% and relative standard deviations below 20% using 7.5 g of milled polished rice and the buffered acetate QuEChERS method without clean-up at both fortification levels: 10 and 300 μg kg(-1). The other six pesticides presented low recovery rates, nevertheless all these analytes could be analyzed with at least one of the other three studied procedures. Copyright © 2010. Published by Elsevier B.V.
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Analysis of Aircraft Fuels and Related Materials
1982-09-01
content by the Karl Fischer method . Each 2040 solvent sample represented a different step in a clean-up procedure conducted by Aero Propulsion...izes a potentiometric titration with alcoholic silver nitrate. This method has a minimum detectability of 1 ppm. It has a re- peatability of 0.1 ppm... Method 163-80, which util- izes a potentiometric titration with alcoholic silver nitrate. This method has a minimum detectability of 1 ppm and has a
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Navarro, P; Cortazar, E; Bartolomé, L; Deusto, M; Raposo, J C; Zuloaga, O; Arana, G; Etxebarria, N
2006-09-22
The feasibility of different clean-up procedures was studied for the determination of polycyclic aromatic hydrocarbons (PAHs) in biota samples such as oysters, mussels and fish liver. In this sense, once the samples were extracted--essentially with acetone and in a microwave system--and before they could be analysed by gas chromatography-mass spectrometry (GC-MS), three different approaches were studied for the clean-up step: solid phase extraction (SPE), microwave-assisted saponification (MAS) and gel permeation chromatography (GPC). The main aim of this work was to maximise the recoveries of PAHs and to minimise the presence of interfering compounds in the last extract. In the case of SPE, Florisil cartridges of 1, 2 and 5 g, and silica cartridges of 5 g were studied. In that case, and with oysters and mussels, microwave-assisted extraction and 5 g Florisil cartridges provided good results. In addition, the concentrations obtained for Standard Reference Material (SRM) NIST 2977 (mussel tissue) were in good agreement with the certified values. In the case of microwave-assisted saponification, the extracts were not as clean as those obtained with 5 g Florisil and this fact lead to overestimate the concentration of the heaviest PAHs. Finally, the cleanest extracts were obtained by GPC. The method was successfully applied to mussels, oysters and hake liver, and the results obtained for NIST 2977 (mussel tissue) were within the confidence interval of the certified reference material for most of the certified analytes.
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Cleaning Puparia for Forensic Analysis.
Higley, Leon G; Brosius, Tierney R; Reinhard, Karl J; Carter, David
2016-09-01
We tested procedures for removing adipocere from insect samples to allow identification. An acceptable procedure was determined: (i) Samples were sorted in petri dishes with 75% alcohol to remove any larvae, adult insects, or other soft-bodied material. (ii) Samples of up to 24 puparia were placed in a vial with 15 mL of 95% acetone, capped, and vortexed for a total of 30-90 sec in 10- to 15-sec bursts. This step removed large masses of adipocere or soil from specimen. (iii) Specimens were removed from acetone and placed in a vial of 15 mL of 2% potassium hydroxide (KOH) and vortexed in 10- to 15-sec bursts until all puparia appeared clean (with our samples this required a total of 60-120 sec). (iv) Specimens were removed from the 2% KOH, placed in 75% ethanol, and examined microscopically. (v) Material was stored in 75% ethanol for identification and long-term preservation. © 2016 American Academy of Forensic Sciences.
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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.
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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.
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Pilot Plant Testing of Hot Gas Building Decontamination Process
1987-10-30
last hours of the cooldown (after water traps in the line were installed) showed no detectable contamination from this station. 1 60 CwC -So 0) 0 o j...Since we will not require refrigeration, additional generators probably 0 qlill not be required. Water is trucked to the site. Agent contaminated water ...surface. The gauze was handled by forceps during all of the sampling steps to prevent contamination after the solvent extraction clean-up of the gauze pads
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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
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Evaluation of two methods to determine glyphosate and AMPA in soils of Argentina
NASA Astrophysics Data System (ADS)
De Geronimo, Eduardo; Lorenzon, Claudio; Iwasita, Barbara; Faggioli, Valeria; Aparicio, Virginia; Costa, Jose Luis
2017-04-01
Argentine agricultural production is fundamentally based on a technological package combining no-tillage and the dependence of glyphosate applications to control weeds in transgenic crops (soybean, maize and cotton). Therefore, glyphosate is the most employed herbicide in the country, where 180 to 200 million liters are applied every year. Due to its widespread use, it is important to assess its impact on the environment and, therefore, reliable analytical methods are mandatory. Glyphosate molecule exhibits unique physical and chemical characteristics which difficult its quantification, especially in soils with high organic matter content, such as the central eastern Argentine soils, where strong interferences are normally observed. The objective of this work was to compare two methods for extraction and quantification of glyphosate and AMPA in samples of 8 representative soils of Argentina. The first analytical method (method 1) was based on the use of phosphate buffer as extracting solution and dichloromethane to minimize matrix organic content. In the second method (method 2), potassium hydroxide was used to extract the analytes followed by a clean-up step using solid phase extraction (SPE) to minimize strong interferences. Sensitivity, recoveries, matrix effects and robustness were evaluated. Both methodologies involved a derivatization with 9-fluorenyl-methyl-chloroformate (FMOC) in borate buffer and detection based on ultra-high-pressure liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Recoveries obtained from soil samples spiked at 0.1 and 1 mg kg-1 and were satisfactory in both methods (70% - 120%). However, there was a remarkable difference regarding the matrix effect, being the SPE clean-up step (method 2) insufficient to remove the interferences. Whereas the dilution and the clean-up with dichloromethane (method 1) were more effective minimizing the ionic suppression. Moreover, method 1 had fewer steps in the protocol of sample processing than method 2. This can be highly valuable in the routine lab work due to the reduction of potential undesired errors such as the loss of analyte or sample contamination. In addition, the substitution of SPE by another alternative involved a considerable reduction of analytical costs in method 1. We conclude that method 1 seemed to be simpler and cheaper than method 2, as well as reliable to quantify glyphosate in Argentinean soils. We hope that this experience can be useful to simplify the protocols of glyphosate quantification and contribute to the understanding of the fate of this herbicide in the environment.
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Genesis Solar Wind Collector Cleaning Assessment: Update on 60336 Sample Case Study
NASA Technical Reports Server (NTRS)
Goreva, Y. S.; Allums, K. K.; Gonzalez, C. P.; Jurewicz, A. J.; Burnett, D. S.; Allton, J. H.; Kuhlman, K. R.; Woolum, D.
2015-01-01
To maximize the scientific return of Genesis Solar Wind return mission it is necessary to characterize and remove a crash-derived particle and thin film surface contamination. A small subset of Genesis mission collector fragments are being subjected to extensive study via various techniques. Here we present an update on the sample 60336, a Czochralski silicon (Si-CZ) based wafer from the bulk array (B/C). This sample has undergone multiple cleaning steps (see the table below): UPW spin wash, aggressive chemical cleanings (including aqua regia, hot xylene and RCA1), as well as optical and chemical (EDS, ToF-SIMS) imaging. Contamination appeared on the surface of 60336 after the initial 2007 UPW cleaning. Aqua regia and hot xylene treatment (8/13/2013) did little to remove contaminants. The sample was UPW cleaned for the third time and imaged (9/16/13). The UPW removed the dark stains that were visible on the sample. However, some features, like "the Flounder" (a large, 100 micron feature in Fig. 1b) appeared largely intact, resisting all previous cleaning efforts. These features were likely from mobilized adhesive, derived from the Post-It notes used to stabilize samples for transport from Utah after the hard landing. To remove this contamination, an RCA step 1 organic cleaning (RCA1) was employed. Although we are still uncertain on the nature of the Flounder and why it is resistant to UPW and aqua regia/hot xylene treatment, we have found RCA1 to be suitable for its removal. It is likely that the glue from sticky pads used during collector recovery may have been a source for resistant organic contamination [9]; however [8] shows that UPW reaction with crash-derived organic contamination does not make particle removal more difficult.
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Jourdil, Jean François; Bartoli, Mireille; Stanke-Labesque, Françoise
2009-11-01
Raltegravir is the first antiretroviral agent to target the human immunodeficiency virus-1 (HIV-1) integrase. It is indicated, in association with other antiretrovirals, in the treatment of acquired immunodeficiency syndrome (AIDS) in antiretroviral treatment-experienced adult patients with viral resistance. To evaluate the feasibility of raltegravir therapeutic drug monitoring, we developed a rapid and specific analytical method for the quantification of raltegravir in human plasma by online sample clean-up liquid chromatography-tandem mass spectrometry (LC-MS/MS). After protein precipitation (with 100 microL of acetonitrile/methanol (50/50)) of 25 microL of plasma, fast online matrix-clean-up was performed using a column switching program. The chromatographic step was optimized to separate raltegravir and its glucuronide metabolite (G-raltegravir). Multiple reaction monitoring (MRM) was used for detection of raltegravir and G-raltegravir. In the absence of G-raltegravir standard, G-raltegravir identification was confirmed by beta-glucuronidase pre-treatment. A total analysis of 3.8 min was needed to separate raltegravir to G-raltegravir. The method was linear between 10 and 3000 ng/mL for raltegravir. Analytical recovery was 94+/-1%. Variation coefficients ranged between 5% and 8.4%. Pre-treatment of plasma from a patient under raltegravir treatment with beta-glucuronidase suppressed G-raltegravir peak. We describe a fast online LC-MS/MS assay that is valid and reliable for the quantification of raltegravir, despite the lack of specificity that could occur in MRM scanning mode experiments.
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ERIC Educational Resources Information Center
Musgrave, Chuck; Spencer-Workman, Sarah
2000-01-01
Provides a nine-step process in designing athletic facility laundry rooms that are attractive and functional. Steps include determining the level of laundry services needed, ensuring adequate storage and compatible delivery systems, selecting laundry equipment, and choosing suitable flooring. (GR)
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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.
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New approach of a transient ICP-MS measurement method for samples with high salinity.
Hein, Christina; Sander, Jonas Michael; Kautenburger, Ralf
2017-03-01
In the near future it is necessary to establish a disposal for high level nuclear waste (HLW) in deep and stable geological formations. In Germany typical host rocks are salt or claystone. Suitable clay formations exist in the south and in the north of Germany. The geochemical conditions of these clay formations show a strong difference. In the northern ionic strengths of the pore water up to 5M are observed. The determination of parameters like K d values during sorption experiments of metal ions like uranium or europium as homologues for trivalent actinides onto clay stones are very important for long term safety analysis. The measurement of the low concentrated, not sorbed analytes commonly takes place by inductively coupled plasma mass spectrometry (ICP-MS). A direct measurement of high saline samples like seawater with more than 1% total dissolved salt content is not possible. Alternatives like sample clean up, preconcentration or strong dilution have more disadvantages than advantages for example more preparation steps or additional and expensive components. With a small modification of the ICP-MS sample introduction system and a home-made reprogramming of the autosampler a transient analysing method was developed which is suitable for measuring metal ions like europium and uranium in high saline sample matrices up to 5M (NaCl). Comparisons at low ionic strength between the default and the transient measurement show the latter performs similarly well to the default measurement. Additionally no time consuming sample clean-up or expensive online dilution or matrix removal systems are necessary and the analysation shows a high sensitivity due to the data processing based on the peak area. Copyright © 2016 Elsevier B.V. All rights reserved.
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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.
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DOE Office of Scientific and Technical Information (OSTI.GOV)
Sharma, Ritin; Dill, Brian; Chourey, Karuna
2012-01-01
The expanding use of surfactants for proteome sample preparations has prompted the need to systematically optimize the application and removal of these MS-deleterious agents prior to proteome measurements. Here we compare four different detergent clean-up methods (Trichloroacetic acid (TCA) precipitation, Chloroform/Methanol/Water (CMW) extraction, commercial detergent removal spin column method (DRS) and filter-aided sample preparation(FASP)) with respect to varying amounts of protein biomass in the samples, and provide efficiency benchmarks with respect to protein, peptide, and spectral identifications for each method. Our results show that for protein limited samples, FASP outperforms the other three clean-up methods, while at high protein amountmore » all the methods are comparable. This information was used in a dual strategy of comparing molecular weight based fractionated and unfractionated lysates from three increasingly complex samples (Escherichia coli, a five microbial isolate mixture, and a natural microbial community groundwater sample), which were all lysed with SDS and cleaned up using FASP. The two approaches complemented each other by enhancing the number of protein identifications by 8%-25% across the three samples and provided broad pathway coverage.« less
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Schwaighofer, Andreas; Kuligowski, Julia; Quintás, Guillermo; Mayer, Helmut K; Lendl, Bernhard
2018-06-30
Analysis of proteins in bovine milk is usually tackled by time-consuming analytical approaches involving wet-chemical, multi-step sample clean-up procedures. The use of external cavity-quantum cascade laser (EC-QCL) based IR spectroscopy was evaluated as an alternative screening tool for direct and simultaneous quantification of individual proteins (i.e. casein and β-lactoglobulin) and total protein content in commercial bovine milk samples. Mid-IR spectra of protein standard mixtures were used for building partial least squares (PLS) regression models. A sample set comprising different milk types (pasteurized; differently processed extended shelf life, ESL; ultra-high temperature, UHT) was analysed and results were compared to reference methods. Concentration values of the QCL-IR spectroscopy approach obtained within several minutes are in good agreement with reference methods involving multiple sample preparation steps. The potential application as a fast screening method for estimating the heat load applied to liquid milk is demonstrated. Copyright © 2018 Elsevier Ltd. All rights reserved.
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Rapid determination of actinides in asphalt samples
Maxwell, Sherrod L.; Culligan, Brian K.; Hutchison, Jay B.
2014-01-12
A new rapid method for the determination of actinides in asphalt samples has been developed that can be used in emergency response situations or for routine analysis If a radiological dispersive device (RDD), Improvised Nuclear Device (IND) or a nuclear accident such as the accident at the Fukushima Nuclear Power Plant in March, 2011 occurs, there will be an urgent need for rapid analyses of many different environmental matrices, including asphalt materials, to support dose mitigation and environmental clean up. The new method for the determination of actinides in asphalt utilizes a rapid furnace step to destroy bitumen and organicsmore » present in the asphalt and sodium hydroxide fusion to digest the remaining sample. Sample preconcentration steps are used to collect the actinides and a new stacked TRU Resin + DGA Resin column method is employed to separate the actinide isotopes in the asphalt samples. The TRU Resin plus DGA Resin separation approach, which allows sequential separation of plutonium, uranium, americium and curium isotopes in asphalt samples, can be applied to soil samples as well.« less
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Luyckx, K; Dewulf, J; Van Weyenberg, S; Herman, L; Zoons, J; Vervaet, E; Heyndrickx, M; De Reu, K
2015-04-01
Cleaning and disinfection of the broiler stable environment is an essential part of farm hygiene management. Adequate cleaning and disinfection is essential for prevention and control of animal diseases and zoonoses. The goal of this study was to shed light on the dynamics of microbiological and non-microbiological parameters during the successive steps of cleaning and disinfection and to select the most suitable sampling methods and parameters to evaluate cleaning and disinfection in broiler houses. The effectiveness of cleaning and disinfection protocols was measured in six broiler houses on two farms through visual inspection, adenosine triphosphate hygiene monitoring and microbiological analyses. Samples were taken at three time points: 1) before cleaning, 2) after cleaning, and 3) after disinfection. Before cleaning and after disinfection, air samples were taken in addition to agar contact plates and swab samples taken from various sampling points for enumeration of total aerobic flora, Enterococcus spp., and Escherichia coli and the detection of E. coli and Salmonella. After cleaning, air samples, swab samples, and adenosine triphosphate swabs were taken and a visual score was also assigned for each sampling point. The mean total aerobic flora determined by swab samples decreased from 7.7±1.4 to 5.7±1.2 log CFU/625 cm2 after cleaning and to 4.2±1.6 log CFU/625 cm2 after disinfection. Agar contact plates were used as the standard for evaluating cleaning and disinfection, but in this study they were found to be less suitable than swabs for enumeration. In addition to measuring total aerobic flora, Enterococcus spp. seemed to be a better hygiene indicator to evaluate cleaning and disinfection protocols than E. coli. All stables were Salmonella negative, but the detection of its indicator organism E. coli provided additional information for evaluating cleaning and disinfection protocols. Adenosine triphosphate analyses gave additional information about the hygiene level of the different sampling points. © 2015 Poultry Science Association Inc.
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Lambropoulou, Dimitra A; Konstantinou, Ioannis K; Albanis, Triantafyllos A
2006-07-28
In the present study a combined analytical method involving ultrasonic extraction (USE), sulfuric acid clean-up and headspace solid-phase microextraction (HS-SPME) was developed for the determination of chlorinated pesticides (CPs) in bird livers. Extraction of CPs from 1g of liver was performed by ultrasonication for 30 min using 20 mL of solvent mixture (n-hexane:acetone (4:1, v/v)). The extract was subsequently subjected to a clean-up step for lipid removal. A comparative study on several clean-up procedures prior to the HS-SPME enrichment step was performed in order to achieve maximum recovery and optimal clean-up efficiency, which would provide suitable limits of detection in the gas chromatographic analysis. For this purpose, destructive (sulfuric acid or sodium hydroxide treatment) and non-destructive (alumina column) clean-up procedures has been assayed. The treatment of the extract with 40% (v/v) H2SO4 prior to HS-SPME process showed the best performance since lower detection limits and higher extraction efficiencies were obtained. The method detection limit ranged from 0.5 to 1.0 ng g(-1) wet weight and peak areas were proportional to analyte concentrations (r2>0.990) in the range of 5-500 ng g(-1) wet wt. The method was found to be reproducible (R.S.D.<10%) and effective under the operational conditions proposed and was applied successfully to the analysis of CPs in liver tissues of various bird species from Greece.
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Evaluation of a Biological Pathogen Decontamination Protocol for Animal Feed Mills.
Huss, Anne R; Cochrane, Roger A; Deliephan, Aiswariya; Stark, Charles R; Jones, Cassandra K
2015-09-01
Animal feed and ingredients are potential vectors of pathogenic bacteria. Contaminated ingredients can contaminate facility equipment, leading to cross-contamination of other products. This experiment was conducted to evaluate a standardized protocol for decontamination of an animal feed manufacturing facility using Enterococcus faecium (ATCC 31282) as an indicator. A pelleted swine diet inoculated with E. faecium was manufactured, and environmental samples (swabs, replicate organism detection and counting plates, and air samples) were collected (i) before inoculation (baseline data), (ii) after production of inoculated feed, (iii) after physical removal of organic material using pressurized air, (iv) after application of a chemical sanitizer containing a quaternary ammonium-glutaraldehyde blend, (v) after application of a chemical sanitizer containing sodium hypochlorite, (vi) after facility heat-up to 60 8 C for 24 h, (vii) for 48 h, and (viii) for 72 h. Air samples collected outside the facility confirmed pathogen containment; E. faecium levels were equal to or lower than baseline levels at each sample location. The decontamination step and its associated interactions were the only variables that affected E. faecium incidence (P < 0.0001 versus P > 0.22). After production of the inoculated diet, 85.7% of environmental samples were positive for E. faecium. Physical cleaning of equipment had no effect on contamination (P = 0.32). Chemical cleaning with a quaternary ammonium-glutaraldehyde blend and sodium hypochlorite each significantly reduced E. faecium contamination (P < 0.0001) to 28.6 and 2.4% of tested surfaces, respectively. All samples were negative for E. faecium after 48 h of heating. Both wet chemical cleaning and facility heating but not physical cleaning resulted in substantial E. faecium decontamination. These results confirmed both successful containment and decontamination of biological pathogens in the tested pilot-scale feed mill.
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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
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Solid-Phase Extraction (SPE): Principles and Applications in Food Samples.
Ötles, Semih; Kartal, Canan
2016-01-01
Solid-Phase Extraction (SPE) is a sample preparation method that is practised on numerous application fields due to its many advantages compared to other traditional methods. SPE was invented as an alternative to liquid/liquid extraction and eliminated multiple disadvantages, such as usage of large amount of solvent, extended operation time/procedure steps, potential sources of error, and high cost. Moreover, SPE can be plied to the samples combined with other analytical methods and sample preparation techniques optionally. SPE technique is a useful tool for many purposes through its versatility. Isolation, concentration, purification and clean-up are the main approaches in the practices of this method. Food structures represent a complicated matrix and can be formed into different physical stages, such as solid, viscous or liquid. Therefore, sample preparation step particularly has an important role for the determination of specific compounds in foods. SPE offers many opportunities not only for analysis of a large diversity of food samples but also for optimization and advances. This review aims to provide a comprehensive overview on basic principles of SPE and its applications for many analytes in food matrix.
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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...
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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.
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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.
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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.
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Baghdady, Yehia Z; Schug, Kevin A
2016-01-01
Accurate and specific analysis of target molecules in complex biological matrices remains a significant challenge, especially when ultra-trace detection limits are required. Liquid chromatography with mass spectrometry is often the method of choice for bioanalysis. Conventional sample preparation and clean-up methods prior to the analysis of biological fluids such as liquid-liquid extraction, solid-phase extraction, or protein precipitation are time-consuming, tedious, and can negatively affect target recovery and detection sensitivity. An alternative or complementary strategy is the use of an off-line or on-line in situ derivatization technique. In situ derivatization can be incorporated to directly derivatize target analytes in their native biological matrices, without any prior sample clean-up methods, to substitute or even enhance the extraction and preconcentration efficiency of these traditional sample preparation methods. Designed appropriately, it can reduce the number of sample preparation steps necessary prior to analysis. Moreover, in situ derivatization can be used to enhance the performance of the developed liquid chromatography with mass spectrometry-based bioanalysis methods regarding stability, chromatographic separation, selectivity, and ionization efficiency. This review presents an overview of the commonly used in situ derivatization techniques coupled to liquid chromatography with mass spectrometry-based bioanalysis to guide and to stimulate future research. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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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.
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Jackson, Darryl D.; Hollen, Robert M.
1983-01-01
A new automatable cleaning apparatus which makes use of a method of very thoroughly and quickly cleaning a gauze electrode used in chemical analyses is given. The method generates very little waste solution, and this is very important in analyzing radioactive materials, especially in aqueous solutions. The cleaning apparatus can be used in a larger, fully automated controlled potential coulometric apparatus. About 99.98% of a 5 mg. plutonium sample was removed in less than 3 minutes, using only about 60 ml. of rinse solution and two main rinse steps.
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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.
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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.
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Martelli, Francesca; Gosling, Rebecca J; Callaby, Rebecca; Davies, Rob
2017-04-01
In the European Union, statutory control of Salmonella is in place in the chicken and turkey sectors, but not in the duck sector. In this study, 14 Salmonella-positive duck farms were sampled before and after cleaning and disinfection, and once the houses had been restocked with a new flock. The cleaning and disinfection programmes used were subdivided into two main categories: ones in which a final formaldehyde disinfection step was included (1) and ones in which it was not included (2). Several types of samples were collected during the study, and faecal samples were those more frequently positive (62% of faecal samples were positive for Salmonella in comparison to 2-23% of samples from all the other sample categories) (P < 0.001). Independently of the cleaning and disinfection programme used, there was a statistically significant (P < 0.001) reduction in the percentage of Salmonella-positive samples between before cleaning and disinfection (41.1%) and after cleaning and disinfection (3.1%). After restocking, the number of Salmonella-positive samples increased significantly (P < 0.001), with 65.3% of the samples tested being positive for Salmonella. Farms in which disinfection programme 1 was used were 5.34 times less likely to have samples positive for Salmonella after cleaning and disinfection than farms which implemented programme 2. Formaldehyde acts effectively against Salmonella even in the presence of some residual organic matter. Limited residual contamination on farms after cleaning and disinfection represents a risk of infection for young ducklings, and thorough cleaning and disinfection procedures should be implemented to reduce the carry-over of infection between flocks.
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Ochratoxin A in cocoa and chocolate sampled in Canada.
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)).
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Immunochromatographic assay of cadmium levels in oysters.
Nishi, Kosuke; Kim, In-Hae; Itai, Takaaki; Sugahara, Takuya; Takeyama, Haruko; Ohkawa, Hideo
2012-08-15
Oysters are one of foodstuffs containing a relatively high amount of cadmium. Here we report on establishment of an immunochromatographic assay (ICA) method of cadmium levels in oysters. Cadmium was extracted with 0.l mol L(-1) HCl from oysters and cleaned up from other metals by the use of an anion-exchange column. The behavior of five metals Mn, Fe, Cu, Zn, and Cd was monitored at each step of extraction and clean-up procedure for the ICA method in an inductively coupled plasma-mass spectrometry (ICP-MS) analysis. The results revealed that a simple extraction method with the HCl solution was efficient enough to extract almost all of cadmium from oysters. Clean-up with an anion-exchange column presented almost no loss of cadmium adsorbed on the column and an efficient removal of metals other than cadmium. When a spiked recovery test was performed in the ICA method, the recovery ranged from 98% to 112% with relative standard deviations between 5.9% and 9.2%. The measured values of cadmium in various oyster samples in the ICA method were favorably correlated with those in ICP-MS analysis (r(2)=0.97). Overall results indicate that the ICA method established in the present study is an adequate and reliable detection method for cadmium levels in oysters. Copyright © 2012 Elsevier B.V. All rights reserved.
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Cleaning of titanium substrates after application in a bioreactor.
Fingerle, Mathias; Köhler, Oliver; Rösch, Christina; Kratz, Fabian; Scheibe, Christian; Davoudi, Neda; Müller-Renno, Christine; Ziegler, Christiane; Huster, Manuel; Schlegel, Christin; Ulber, Roland; Bohley, Martin; Aurich, Jan C
2015-03-10
Plain and microstructured cp-titanium samples were studied as possible biofilm reactor substrates. The biofilms were grown by exposition of the titanium samples to bacteria in a flow cell. As bacteria the rod shaped gram negative Pseudomonas fluorescens and the spherical gram negative Paracoccus seriniphilus were chosen. Afterward, the samples were cleaned in subsequent steps: First, with a standard solvent based cleaning procedure with acetone, isopropanol, and ultrapure water and second by oxygen plasma sputtering. It will be demonstrated by means of x-ray photoelectron spectroscopy, fluorescence microscopy, and confocal laser scanning microscopy that oxygen plasma cleaning is a necessary and reliant tool to fully clean and restore titanium surfaces contaminated with a biofilm. The microstructured surfaces act beneficial to biofilm growth, while still being fully restorable after biofilm contamination. Scanning electron microscopy images additionally show, that the plasma process does not affect the microstructures. The presented data show the importance of the cleaning procedure. Just using solvents does not remove the biofilm and all its components reliably while a cleaning process by oxygen plasma regenerates the surfaces.
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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.
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Rep. Sarbanes, John P. [D-MD-3
2009-06-04
House - 06/26/2009 Referred to the Subcommittee on Government Management, Organization, and Procurement. (All Actions) Tracker: This bill has the status IntroducedHere are the steps for Status of Legislation:
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Safety in the Chemical Laboratory: Flood Control.
ERIC Educational Resources Information Center
Pollard, Bruce D.
1983-01-01
Describes events leading to a flood in the Wehr Chemistry Laboratory at Marquette University, discussing steps taken to minimize damage upon discovery. Analyzes the problem of flooding in the chemical laboratory and outlines seven steps of flood control: prevention; minimization; early detection; stopping the flood; evaluation; clean-up; and…
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Jackson, D.D.; Hollen, R.M.
1981-02-27
A method of very thoroughly and quikcly cleaning a guaze electrode used in chemical analyses is given, as well as an automobile cleaning apparatus which makes use of the method. The method generates very little waste solution, and this is very important in analyzing radioactive materials, especially in aqueous solutions. The cleaning apparatus can be used in a larger, fully automated controlled potential coulometric apparatus. About 99.98% of a 5 mg plutonium sample was removed in less than 3 minutes, using only about 60 ml of rinse solution and two main rinse steps.
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On-farm comparisons of different cleaning protocols in broiler houses.
Luyckx, K Y; Van Weyenberg, S; Dewulf, J; Herman, L; Zoons, J; Vervaet, E; Heyndrickx, M; De Reu, K
2015-08-01
The present study evaluated the effectiveness of 4 cleaning protocols designed to reduce the bacteriological infection pressure on broiler farms and prevent food-borne zoonoses. Additionally, difficult to clean locations and possible sources of infection were identified. Cleaning and disinfection rounds were evaluated in 12 broiler houses on 5 farms through microbiological analyses and adenosine triphosphate hygiene monitoring. Samples were taken at 3 different times: before cleaning, after cleaning, and after disinfection. At each sampling time, swabs were taken from various locations for enumeration of the total aerobic flora and Enterococcus species pluralis ( SPP:). In addition, before cleaning and after disinfection, testing for Escherichia coli and Salmonella was carried out. Finally, adenosine triphosphate swabs and agar contact plates for total aerobic flora counts were taken after cleaning and disinfection, respectively. Total aerobic flora and Enterococcus spp. counts on the swab samples showed that cleaning protocols which were preceded by an overnight soaking with water caused a higher bacterial reduction compared to protocols without a preceding soaking step. Moreover, soaking of broiler houses leads to less water consumption and reduced working time during high pressure cleaning. No differences were found between protocols using cold or warm water during cleaning. Drinking cups, drain holes, and floor cracks were identified as critical locations for cleaning and disinfection in broiler houses. © 2015 Poultry Science Association Inc.
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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.
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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.
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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.
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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.
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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...
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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.
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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.
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Sen. Mikulski, Barbara A. [D-MD
2011-05-12
Senate - 05/12/2011 Read twice and referred to the Committee on Homeland Security and Governmental Affairs. (All Actions) Tracker: This bill has the status IntroducedHere are the steps for Status of Legislation:
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Six Easy Steps to Online Success
ERIC Educational Resources Information Center
Rose, Richard
2011-01-01
Against his better instincts, the author, an educator at West Texas A&M University, shares his school's recipe for developing a successful online learning program. He discusses six easy steps to online success. These include: (1) clean up one's act; (2) answers in 24 hours; (3) plenty of structure; (4) format phone conferences at midterm; (5) do…
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NASA Astrophysics Data System (ADS)
Lee, Yujin; You, Eun-Ah; Ha, Young-Geun
2018-07-01
Despite the considerable demand for bioinspired superhydrophobic surfaces with highly transparent, self-cleaning, and self-healable properties, a facile and scalable fabrication method for multifunctional superhydrophobic films with strong chemical networks has rarely been established. Here, we report a rationally designed facile one-step construction of covalently networked, transparent, self-cleaning, and self-healable superhydrophobic films via a one-step preparation and single-reaction process of multi-components. As coating materials for achieving the one-step fabrication of multifunctional superhydrophobic films, we included two different sizes of Al2O3 nanoparticles for hierarchical micro/nano dual-scale structures and transparent films, fluoroalkylsilane for both low surface energy and covalent binding functions, and aluminum nitrate for aluminum oxide networked films. On the basis of stability tests for the robust film composition, the optimized, covalently linked superhydrophobic composite films with a high water contact angle (>160°) and low sliding angle (<1°) showed excellent thermal stability (up to 400 °C), transparency (≈80%), self-healing, self-cleaning, and waterproof abilities. Therefore, the rationally designed, covalently networked superhydrophobic composite films, fabricated via a one-step solution-based process, can be further utilized for various optical and optoelectronic applications.
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Development and validation of an LC-UV method for the determination of sulfonamides in animal feeds.
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.
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NASA Astrophysics Data System (ADS)
Abdel-Kareem, Omar; Harith, M. A.
2008-07-01
Cleaning of copper embroidery threads on archaeological textiles is still a complicated conservation process, as most textile conservators believe that the advantages of using traditional cleaning techniques are less than their disadvantages. In this study, the uses of laser cleaning method and two modified recipes of wet cleaning methods were evaluated for cleaning of the corroded archaeological Egyptian copper embroidery threads on an archaeological Egyptian textile fabric. Some corroded copper thread samples were cleaned using modified recipes of wet cleaning method; other corroded copper thread samples were cleaned with Q-switched Nd:YAG laser radiation of wavelength 532 nm. All tested metal thread samples before and after cleaning were investigated using a light microscope and a scanning electron microscope with an energy dispersive X-ray analysis unit. Also the laser-induced breakdown spectroscopy (LIBS) technique was used for the elemental analysis of laser-cleaned samples to follow up the laser cleaning procedure. The results show that laser cleaning is the most effective method among all tested methods in the cleaning of corroded copper threads. It can be used safely in removing the corrosion products without any damage to both metal strips and fibrous core. The tested laser cleaning technique has solved the problems caused by other traditional cleaning techniques that are commonly used in the cleaning of metal threads on museum textiles.
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NASA Astrophysics Data System (ADS)
Rettberg, P.; Horneck, G.; Fritze, D.; Stackebrandt, E.; Kminek, G.
The first step in the implementation of planetary protection guidelines encompasses a qualitative and quantitative inventory of the bioburden of spacecraft assembly facilities. In such an artificial environment mainly microorganisms are to be expected that are brought in by the humans themselves and that are able to withstand the controlled air circulation, the low relative humidity, the moderately high temperature and the low-nutrient conditions in the clean rooms of the assembly facilities. With informations about the composition of these microbial communities the development and/or optimization of adequate cleaning and sterilization procedures for spacecraft preparation before launch will be possible. The bioburden assessment in spacecraft assembly facilities requires a standardized procedure for sampling the air and surfaces in the facilities as well as of the spacecraft, a transfer of the biological samples under controlled conditions to the analyzing laboratory and a scientifically approved set of methods for analysis. In the ESA project MiDiv we started to investigate the bioburden of spacecrafts using the satellites SMART-1 and ROSETTA as test objects. The analysis of the samples included so far cultivation on different media at different pH and temperatures with and without oxygen with and without pasteurization, establishment of a culture collection of bacteria and partial 16S rRNA gene analysis. The results of these preliminary measurements, the total number of microorganisms, the numbers of colony forming units, differentiated according to the subgroups of aerobes, facultative anaerobes and anaerobes, and the phylogenetic classification, will be assessed with respect to the physiological potential of the identified microorganisms to withstand the different cleaning and sterilizing procedures used up to now for planetary protection measures. In the next step the ability of selected microorganisms to survive has to tested under environmental conditions as they occur for example on Mars.
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Next steps in the development of ecological soil clean-up values for metals.
Wentsel, Randall; Fairbrother, Anne
2014-07-01
This special series in Integrated Environmental Assessment Management presents the results from 6 workgroups that were formed at the workshop on Ecological Soil Levels-Next Steps in the Development of Metal Clean-Up Values (17-21 September 2012, Sundance, Utah). This introductory article presents an overview of the issues assessors face when conducting risk assessments for metals in soils, key US Environmental Protection Agency (USEPA) documents on metals risk assessment, and discusses the importance of leveraging from recent major terrestrial research projects, primarily to address Registration, Evaluation, Authorization and Restriction of Chemical Substances (REACH) requirements in Europe, that have significantly advanced our understanding of the behavior and toxicity of metals in soils. These projects developed large data sets that are useful for the risk assessment of metals in soil environments. The workshop attendees met to work toward developing a process for establishing ecological soil clean-up values (Eco-SCVs). The goal of the workshop was to progress from ecological soil screening values (Eco-SSLs) to final clean-up values by providing regulators with the methods and processes to incorporate bioavailability, normalize toxicity thresholds, address food-web issues, and incorporate background concentrations. The REACH data sets were used by workshop participants as case studies in the development of the ecological standards for soils. The workshop attendees discussed scientific advancements in bioavailability, soil biota and wildlife case studies, soil processes, and food-chain modeling. In addition, one of the workgroups discussed the processes needed to frame the topics to gain regulatory acceptance as a directive or guidance by Canada, the USEPA, or the United States. © 2013 SETAC.
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Demand driven salt clean-up in a molten salt fast reactor - Defining a priority list.
Merk, B; Litskevich, D; Gregg, R; Mount, A R
2018-01-01
The PUREX technology based on aqueous processes is currently the leading reprocessing technology in nuclear energy systems. It seems to be the most developed and established process for light water reactor fuel and the use of solid fuel. However, demand driven development of the nuclear system opens the way to liquid fuelled reactors, and disruptive technology development through the application of an integrated fuel cycle with a direct link to reactor operation. The possibilities of this new concept for innovative reprocessing technology development are analysed, the boundary conditions are discussed, and the economic as well as the neutron physical optimization parameters of the process are elucidated. Reactor physical knowledge of the influence of different elements on the neutron economy of the reactor is required. Using an innovative study approach, an element priority list for the salt clean-up is developed, which indicates that separation of Neodymium and Caesium is desirable, as they contribute almost 50% to the loss of criticality. Separating Zirconium and Samarium in addition from the fuel salt would remove nearly 80% of the loss of criticality due to fission products. The theoretical study is followed by a qualitative discussion of the different, demand driven optimization strategies which could satisfy the conflicting interests of sustainable reactor operation, efficient chemical processing for the salt clean-up, and the related economic as well as chemical engineering consequences. A new, innovative approach of balancing the throughput through salt processing based on a low number of separation process steps is developed. Next steps for the development of an economically viable salt clean-up process are identified.
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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.
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Plasma surface cleaning using microwave plasmas
DOE Office of Scientific and Technical Information (OSTI.GOV)
Tsai, C.C.; Haselton, H.H.; Nelson, W.D.
1993-11-01
In a microwave electron cyclotron resonance (ECR) plasma source, reactive plasmas of oxygen and its mixture with argon are used for plasma-cleaning experiments. Aluminum test samples (0.95 {times} 1.9 cm) were coated with thin films ({le} 20 {mu}m in thickness) of Shell Vitrea oil and cleaned by using such reactive plasmas. The plasma cleaning was done in various discharge conditions with fixed microwave power, rf power, biased potential, gas pressures (0.5 and 5 mtorr), and operating time up to 35 min. The status of plasma cleaning has been monitored by using mass spectroscopy. Mass loss of the samples after plasmamore » cleaning was measured to estimate cleaning rates. Measured clean rates of low pressure (0.5 mtorr) argon/oxygen plasmas were as high as 2.7 {mu}/min. X-ray photoelectron spectroscopy was used to determine cleanliness of the sample surfaces and confirm the effectiveness of plasma cleaning in achieving atomic levels of surface cleanliness. In this paper, significant results are reported and discussed.« less
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Blanch, Gracia Patricia; Morales, Francisco José; Moreno, Fernando de la Peña; del Castillo, María Luisa Ruiz
2013-01-01
A new method based on off-line coupling of LC with GC in replacement of conventional sample preparation techniques is proposed to analyze acrylamide in coffee brews. The method involves the preseparation of the sample by LC, the collection of the selected fraction, its concentration under nitrogen, and subsequent analysis by GC coupled with MS. The composition of the LC mobile phase and the flow rate were studied to select those conditions that allowed separation of acrylamide without coeluting compounds. Under the conditions selected recoveries close to 100% were achieved while LODs and LOQs equal to 5 and 10 μg/L for acrylamide in brewed coffee were obtained. The method developed enabled the reliable detection of acrylamide in spiked coffee beverage samples without further clean-up steps or sample manipulation. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Roegner, Amber F.; Schirmer, Macarena Pírez; Puschner, Birgit; Brena, Beatriz; Gonzalez-Sapienza, Gualberto
2014-01-01
The freshwater cyanotoxins, microcystins (MCs), pose a global public health threat as potent hepatotoxins in cyanobacterial blooms; their persistence in drinking and recreational water has been associated with potential chronic effects in addition to acute intoxications. Rapid and accurate detection of the over 80 structural congeners is challenged by the rigorous and time consuming clean up required to overcome interference found in raw water samples. MALDI-MS has shown promise for rapid quantification of individual congeners in raw water samples, with very low operative cost, but so far limited sensitivity and lack of available and versatile internal standards (ISs) has limited its use. Two easily synthesized S-hydroxyethyl–Cys(7)-MC-LR and –RR ISs were used to generate linear standard curves in a reflectron MALDI instrument, reproducible across several orders of magnitude for MC –LR, - RR and –YR. Minimum quantification limits in direct water samples with no clean up or concentration step involved were consistently below 7 μg/L, with recoveries from spiked samples between 80 and 119%. This method improves sensitivity by 30 fold over previous reports of quantitative MALDI-TOF applications to MCs and provides a salient option for rapid throughput analysis for multiple MC congeners in untreated raw surface water blooms as a means to identify source public health threats and target intervention strategies within a watershed. As demonstrated by analysis of a set of samples from Uruguay, utilizing the reaction of different MC congeners with alternate sulfhydryl compounds, the m/z of the IS can be customized to avoid overlap with interfering compounds in local surface water samples. PMID:24388801
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DOE Office of Scientific and Technical Information (OSTI.GOV)
Hannemann, L.W.
1995-12-31
Austin is the only city in attainment that has chosen to join the Clean Cities program. A recent emissions inventory completed by the City`s Air Quality Program shows that the largest single contributor to Austin`s deteriorating air quality is on-road mobile sources. Implementing the Clean Cities Program is one proactive step they are taking to keep the air clean. Although Austin Clean Cities chose to be fuel neutral they have found that propane and natural gas are the natural choices for them to use. The author was asked to address the potential pitfalls in setting up a Clean Cities program,more » and 20/20 hindsight reveals that Austin had a few housekeeping chores to attend to before starting the real work. There are lots of little details necessary to get an organization like this up and running and then keeping it healthy. These details need to be identified and addressed upfront and before any real work can be done. The advantage is that one gets a network that is able to gather, evaluate and disseminate information, and one gets a clean city.« less
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Barahona, Francisco; Turiel, Esther; Cormack, Peter A G; Martín-Esteban, Antonio
2011-01-01
In this work, the synthesis of molecularly imprinted polymer microspheres with narrow particle size distributions and core-shell morphology by a two-step precipitation polymerization procedure is described. Polydivinylbenzene (poly DVB-80) core particles were used as seed particles in the production of molecularly imprinted polymer shells by copolymerization of divinylbenzene-80 with methacrylic acid in the presence of thiabendazole (TBZ) and an appropriate porogen. Thereafter, polymer particles were packed into refillable stainless steel HPLC columns used in the development of an inline molecularly imprinted SPE method for the determination of TBZ in citrus fruits and orange juice samples. Under optimized chromatographic conditions, recoveries of TBZ within the range 81.1-106.4%, depending upon the sample, were obtained, with RSDs lower than 10%. This novel method permits the unequivocal determination of TBZ in the samples under study, according to the maximum residue levels allowed within Europe, in less than 20 min and without any need for a clean-up step in the analytical protocol. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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4 Steps to Combat Malware Enterprisewide
ERIC Educational Resources Information Center
Zeltser, Lenny
2011-01-01
Too often, organizations make the mistake of treating malware infections as a series of independent occurrences. Each time a malicious program is discovered, IT simply cleans up or rebuilds the affected host, and then moves on with routine operational tasks. Yet, this approach doesn't allow the institution to keep up with the increasingly…
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Hijnen, W A M; Castillo, C; Brouwer-Hanzens, A H; Harmsen, D J H; Cornelissen, E R; van der Kooij, D
2012-12-01
Cleaning of high pressure RO/NF membranes is an important operational tool to control biofouling. Quantitative information on the efficacy of cleaning agents and protocols to remove biomass is scarce. Therefore, a laboratory cleaning test to assess the efficiency of cleaning procedures to remove attached biomass was developed. The major components of the test are (i) production of uniform biofilm samples, (ii) the quantification of the biomass concentrations with robust parameters and (iii) a simple test procedure with optimal exposure of the biofilm samples to the chemicals. The results showed that PVC-P is a suitable substratum for the production of uniform biofilm samples. ATP and carbohydrates (CH) as major components of the biofilm matrix for nucleotides (living bacterial cells) and extracellular polymeric substances EPS, respectively, were selected as robust biomass parameters. The removal of ATP and CH with the NaOH/Sodium Dodecyl Sulfate (SDS) mixture, selected as a standard treatment at pH 12.0, was reproducible. The resistance of the EPS matrix against chemical cleaning was demonstrated by a low CH removal (32.8 ± 6.0%) compared to the ATP removal (70.5 ± 15.1%). The inverse relationship of biomass removal with the CH to ATP ratio (μg/ng) of the biofilms demonstrated the influence of the biomass characteristics on cleaning. None of the 27 chemicals tested (analytical-grade and commercial brands) in single step or in double-step treatments were significantly more effective than NaOH/SDS. Oxidizing agents NaOCl and H(2)O(2), the latter in combination with SDS, both tested as common agents in biofilm control, showed a significantly higher efficiency (70%) to remove biofilms. In the test, simultaneously, the efficiency of agents to remove precipitated minerals such as Fe can be assessed. Validation tests with Cleaning in Place (CIP) in 8 and 2.5-inch RO membrane pilot plant experiments showed similar ranking of the cleaning efficiency of cleaning protocols as determined in the laboratory tests. Further studies with the laboratory test are required to study the effect of cleaning conditions such as duration, temperature, shear forces as well as chemical conditions (concentrations, alternative agents or mixtures and sequence of application) on the efficiency to remove attached biomass. Copyright © 2012 Elsevier Ltd. All rights reserved.
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Settlement with Marina will Result in Cleaner Air on Block Island
A marina in Block Island, R.I., has reduced its emissions and taken steps to comply with federal clean air laws following an inspection and follow-up action from the US Environmental Protection Agency.
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Fan, S; Zou, J H; Miao, H; Zhao, Y F; Chen, H J; Zhao, R; Wu, Y N
2013-01-01
A liquid chromatography-linear ion-trap spectrometry (LC-MS³) method using β-receptor molecular-imprinted polymer (MIP) solid-phase extraction (SPE) as clean-up was developed to determine simultaneously and confirmatively residues of 25 β₂-agonists and 21 β-blockers in urine samples. Urine samples were subjected to enzymatic hydrolysis by β-glucoronidase/arylsulphatase, and then extracted with perchloric acid. Sample clean-up was performed using β-receptor MIP SPE. A Supelco Ascentis® express Rp-Amide column was used to separate the analytes, and MS³ detection used an electrospray ionisation source in positive-ion mode. Recovery studies were carried out using blank urine samples fortified with the 46 analytes at the levels of 0.5, 1.0 and 2.0 μg l⁻¹. Recoveries were obtained ranging from 60.1% to 109.9% with relative standard deviations (RSDs, n = 7) from 0.5% to 19.4%. The limits of detection (LODs) and limits of quantitation (LOQs) of the 46 analytes in urine were 0.02-0.18 and 0.05-0.60 μg l⁻¹, respectively. As a result of the selective clean-up by MIP SPE and MS³ detection of the target drugs, the sensitivity and accuracy of the present method was high enough for monitoring β₂-agonist and β-blocker residues in urine samples. Satisfactory results were obtained in the process of the determination of positive urine samples.
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Assessment of test methods for evaluating effectiveness of cleaning flexible endoscopes.
Washburn, Rebecca E; Pietsch, Jennifer J
2018-06-01
Strict adherence to each step of reprocessing is imperative to removing potentially infectious agents. Multiple methods for verifying proper reprocessing exist; however, each presents challenges and limitations, and best practice within the industry has not been established. Our goal was to evaluate endoscope cleaning verification tests with particular interest in the evaluation of the manual cleaning step. The results of the cleaning verification tests were compared with microbial culturing to see if a positive cleaning verification test would be predictive of microbial growth. This study was conducted at 2 high-volume endoscopy units within a multisite health care system. Each of the 90 endoscopes were tested for adenosine triphosphate, protein, microbial growth via agar plate, and rapid gram-negative culture via assay. The endoscopes were tested in 3 locations: the instrument channel, control knob, and elevator mechanism. This analysis showed substantial level of agreement between protein detection postmanual cleaning and protein detection post-high-level disinfection at the control head for scopes sampled sequentially. This study suggests that if protein is detected postmanual cleaning, there is a significant likelihood that protein will also be detected post-high-level disinfection. It also infers that a cleaning verification test is not predictive of microbial growth. Copyright © 2018 Association for Professionals in Infection Control and Epidemiology, Inc. Published by Elsevier Inc. All rights reserved.
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Demand driven salt clean-up in a molten salt fast reactor – Defining a priority list
Litskevich, D.; Gregg, R.; Mount, A. R.
2018-01-01
The PUREX technology based on aqueous processes is currently the leading reprocessing technology in nuclear energy systems. It seems to be the most developed and established process for light water reactor fuel and the use of solid fuel. However, demand driven development of the nuclear system opens the way to liquid fuelled reactors, and disruptive technology development through the application of an integrated fuel cycle with a direct link to reactor operation. The possibilities of this new concept for innovative reprocessing technology development are analysed, the boundary conditions are discussed, and the economic as well as the neutron physical optimization parameters of the process are elucidated. Reactor physical knowledge of the influence of different elements on the neutron economy of the reactor is required. Using an innovative study approach, an element priority list for the salt clean-up is developed, which indicates that separation of Neodymium and Caesium is desirable, as they contribute almost 50% to the loss of criticality. Separating Zirconium and Samarium in addition from the fuel salt would remove nearly 80% of the loss of criticality due to fission products. The theoretical study is followed by a qualitative discussion of the different, demand driven optimization strategies which could satisfy the conflicting interests of sustainable reactor operation, efficient chemical processing for the salt clean-up, and the related economic as well as chemical engineering consequences. A new, innovative approach of balancing the throughput through salt processing based on a low number of separation process steps is developed. Next steps for the development of an economically viable salt clean-up process are identified. PMID:29494604
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Study on the lifetime of Mo/Si multilayer optics with pulsed EUV-source at the ETS
NASA Astrophysics Data System (ADS)
Schürmann, Mark; Yulin, Sergiy; Nesterenko, Viatcheslav; Feigl, Torsten; Kaiser, Norbert; Tkachenko, Boris; Schürmann, Max C.
2011-06-01
As EUV lithography is on its way into production stage, studies of optics contamination and cleaning under realistic conditions become more and more important. Due to this fact an Exposure Test Stand (ETS) has been constructed at XTREME technologies GmbH in collaboration with Fraunhofer IOF and with financial support of Intel Corporation. This test stand is equipped with a pulsed DPP source and allows for the simultaneous exposure of several samples. In the standard set-up four samples with an exposed area larger than 35 mm2 per sample can be exposed at a homogeneous intensity of 0.25 mW/mm2. A recent update of the ETS allows for simultaneous exposures of two samples with intensities up to 1.0 mW/mm2. The first application of this alternative set-up was a comparative study of carbon contamination rates induced by EUV radiation from the pulsed source with contamination rates induced by quasicontinuous synchrotron radiation. A modified gas-inlet system allows for the introduction of a second gas to the exposure chamber. This possibility was applied to investigate the efficiency of EUV-induced cleaning with different gas mixtures. In particular the enhancement of EUV-induced cleaning by addition of a second gas to the cleaning gas was studied.
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Lozowicka, Bozena; Ilyasova, Gulzhakhan; Kaczynski, Piotr; Jankowska, Magdalena; Rutkowska, Ewa; Hrynko, Izabela; Mojsak, Patrycja; Szabunko, Julia
2016-05-01
For the first time three methods: matrix solid phase dispersion (MSPD), original and modified QuEChERS, with and without clean up step were studied in order to evaluate the extraction efficiency of various classes of pesticides from solid and liquid high sucrose content matrices. Determinations over four hundred pesticides were performed by gas and liquid chromatography with triple quadrupole mass spectrometry (GC/LC/MS/MS) using multiple reaction monitoring. The proposed methods were validated on sugar beets and their technological product beet molasses. In general, the recoveries obtained for the original QuEChERS and MSPD method were lower (<70%) than for the modified QuEChERS without clean up in sugar beet and with clean up in beet molasses. Among these methods, high extraction yields were achieved as recommended in SANCO/12571/2013, with repeatability of 4.4-19.2% and within-laboratory reproducibility of 7.1-18.4% for citrate QuEChERS, whereas greater ruggedness were observed for MSPD. The limit of quantification (LOQ) at (the lowest MRL=0.01mgkg(-1)e.g. for oxamyl()) or below (0.005mgkg(-1)) the regulatory maximum residue level for the pesticides were achieved. The expanded measurement uncertainty was not higher than 30% for all target analytes. Matrix effects were compared and observed for both matrices at both gas and liquid chromatography. The most compounds showed signal enhancement and it was compensated by using matrix-matched calibration and modified QuEChERS characterized lower matrix effects. The confirmation of suitability citrate QuEChERS optimized method was to use for routine testing of several dozen samples determination and residue of epoxiconazole and tebuconazole (both at 0.01mgkg(-1)) in the samples of beet molasses and cyfluthrin (0.06mgkg(-1)) in sugar beet were found. Copyright © 2016 Elsevier B.V. All rights reserved.
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Self-cleaning of Surfaces: the Role of Surface Wettability and Dust Types
NASA Astrophysics Data System (ADS)
Quan, Yun-Yun; Zhang, Li-Zhi; Qi, Rong-Hui; Cai, Rong-Rong
2016-12-01
The self-cleaning property is usually connected to superhydrophobic surfaces (SHSs) where the dust particles can be easily removed by the rolling motion of droplets. It seems that superhydrophobicity (its durability is questionable nowadays) is a necessity. However here, it is disclosed that self-cleaning can also be realized on an ordinary surface by droplet impinging. The effects of surface wettability and the types of dust particles are considered. The self-cleaning is realized by two steps: (1) the pickup of particles by the water-air interface of an impinging droplet, (2) the release of the impinging droplets from the surface. It can be observed that only the trailing edges of the droplets can pick up particles when the droplets recoil from the inclined surfaces. The hydrophilic surface can also achieve self-cleaning under some conditions. This interesting finding may be helpful for the successful implementation of self-cleaning with common surfaces.
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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...
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Lian, Ziru; Li, Hai-Bei; Wang, Jiangtao
2016-08-01
An innovative and effective extraction procedure based on molecularly imprinted solid-phase extraction (MISPE) was developed for the isolation of gonyautoxins 2,3 (GTX2,3) from Alexandrium minutum sample. Molecularly imprinted polymer microspheres were prepared by suspension polymerization and and were employed as sorbents for the solid-phase extraction of GTX2,3. An off-line MISPE protocol was optimized. Subsequently, the extract samples from A. minutum were analyzed. The results showed that the interference matrices in the extract were obviously cleaned up by MISPE procedures. This outcome enabled the direct extraction of GTX2,3 in A. minutum samples with extraction efficiency as high as 83 %, rather significantly, without any need for a cleanup step prior to the extraction. Furthermore, computational approach also provided direct evidences of the high selective isolation of GTX2,3 from the microalgal extracts.
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Baggiani, C; Giovannoli, C; Anfossi, L; Tozzi, C
2001-12-14
A molecularly imprinted polymer (MIP) was synthesized using the herbicide 2,4,5-trichlorophenoxyacetic acid as a template, 4-vinylpyridine as an interacting monomer, ethylendimethacrylate as a cross-linker and a methanol-water mixture as a porogen. The binding properties and the selectivity of the polymer towards the template were investigated by frontal and zonal liquid chromatography. The polymer was used as a solid-phase extraction material for the clean-up of the template molecule and some related herbicides (2,4-dichlorophenoxyacetic acid, fenoprop, dichlorprop) from river water samples at a concentration level of ng/ml with quantitative recoveries comparable with those obtained with a traditional C18 reversed-phase column when analyzed by capillary electrophoresis. The results obtained show that the MIP-based approach to the solid-phase extraction is comparable with the more traditional solid-phase extraction with C18 reversed-phase columns in terms of recovery, but it is superior in terms of sample clean-up.
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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.
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An Organic Decontamination Method for Sampling Devices used in Life-detection Studies
NASA Technical Reports Server (NTRS)
Eigenbrode, Jennifer; Maule, Jake; Wainwright, Norm; Steele, Andrew; Amundsen, Hans E.F.
2008-01-01
Organic decontamination of sampling and storage devices are crucial steps for life-detection, habitability, and ecological investigations of extremophiles living in the most inhospitable niches of Earth, Mars and elsewhere. However, one of the main stumbling blocks for Mars-analogue life-detection studies in terrestrial remote field-sites is the capability to clean instruments and sampling devices to organic levels consistent with null values. Here we present a new seven-step, multi-reagent cleaning and decontamination protocol that was adapted and tested on a glacial ice-coring device and on a rover-guided scoop used for sediment sampling both deployed multiple times during two field seasons of the Arctic Mars Analog Svalbard Expedition AMASE). The effectiveness of the protocols for both devices was tested by (1)in situ metabolic measurements via APT, (2)in situ lipopolysacchride (LPS) quantifications via low-level endotoxin assays, and(3) laboratory-based molecular detection via gas chromatography-mass spectrometry. Our results show that the combination and step-wise application of disinfectants with oxidative and solvation properties for sterilization are effective at removing cellular remnants and other organic traces to levels necessary for molecular organic- and life-detection studies. The validation of this seven-step protocol - specifically for ice sampling - allows us to proceed with confidence in kmskia4 analogue investigations of icy environments. However, results from a rover scoop test showed that this protocol is also suitable for null-level decontamination of sample acquisition devices. Thus, this protocol may be applicable to a variety of sampling devices and analytical instrumentation used for future astrobiology missions to Enceladus, and Europa, as well as for sample-return missions.
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DOE Office of Scientific and Technical Information (OSTI.GOV)
Neufeld, R. D.; Bern, J.; Erdogan, H.
1979-11-15
Activities are underway to investigate basic phenomena that would assist demonstration and commercial sized coal conversion facilities in the environmentally acceptable disposal of process solid waste residuals. The approach taken is to consider only those residuals coming from the conversion technology itself, i.e. from gasification, liquefaction, and hot-clean-up steps as well as residuals from the wastewater treatment train. Residuals from the coal mining and coal grinding steps will not be considered in detail since those materials are being handled in some manner in the private sector. Laboratory evalations have been conducted on solid waste samples of fly ash from anmore » existing Capman gasifier. ASTM-A and EPA-EP leaching procedures have been completed on sieved size fractions of the above wastes. Data indicate that smaller size fractions pose greater contamination potential than do larger size particles with a transition zone occurring at particle sizes of about 0.05 inches in diameter. Ames testing of such residuals is reported. Similar studies are under way with samples of H-Coal solid waste residuals.« less
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Evaluation of Various Cleaning Methods to Remove Bacillus Spores from Spacecraft Hardware Materials
NASA Technical Reports Server (NTRS)
Venkateswaran, Kasthuri; Chung, Shirley; Allton, Judith; Kern, Roger
2004-01-01
A detailed study was made of the biological cleaning effectiveness, defined in terms of the ability to remove bacterial spores, of a number of methods used to clean hardware surfaces. Aluminum (Al 6061) and titanium (Ti 6Al-4V) were chosen for the study as they were deemed the two materials most likely to be used in spacecraft extraterrestrial sampler construction. None of the cleaning protocols tested completely removed viable spores from the surface of the aluminum. In contrast, titanium was capable of being cleaned to sterility by two methods, the JPL standard and the commercial SAMS cleaning process. Further investigation showed that the passivation step employed in the JPL standard method is an effective surface sterilant on both metals but not compatible with aluminum. It is recommended that titanium (Ti 6Al-4V) be considered superior to aluminum (Al 6061) for use in spacecraft sampling hardware, both for its potential to be cleaned to sterilization and for its ability to withstand the most effective cleaning protocols.
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Viguet-Carrin, S; Gineyts, E; Bertholon, C; Delmas, P D
2009-01-01
A rapid high performance liquid chromatographic method was developed including an internal standard for the measurement of mature and senescent crosslinks concentration in non-demineralized bone hydrolysates. To avoid the demineralization which is a tedious step, we developed a method based on the use of a solid-phase extraction procedure to clean-up the samples. It resulted in sensitive and accurate measurements: the detection limits as low as 0.2 pmol for the pyridimium crosslinks and 0.02 pmol for the pentosidine. The inter- and intra-assay coefficients of variation were as low as 5% and 2%, respectively, for all crosslinks.
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Dudley, E; El-Shakawi, S; Games, D E; Newton, R P
2000-03-01
A chromatographic separation of nucleosides from urine has been developed in order to facilitate their mass spectrometric analysis for clinical diagnosis. A number of chromatographic resins were studied in order to develop an effective and efficient purification procedure. The optimized sequential protocol comprises a centrifugation, acidification and neutralization step, followed by application of an affinity chromatographic column and finally further separation on an acidic cation exchange column and a basic anion exchanger. This scheme shows effective clean-up of a standard radiolabelled nucleoside with a recovery of 92.5%, and recovery of nucleosides added to urine samples before extraction showed recoveries of 72-82%.
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Mechanical vs. manual cleaning of hospital beds: a prospective intervention study.
Hopman, J; Nillesen, M; de Both, E; Witte, J; Teerenstra, S; Hulscher, M; Voss, A
2015-06-01
Cleaning regimens for hospital beds were evaluated in the context of a rising prevalence of highly resistant micro-organisms and increasing financial pressure on healthcare systems. Dutch hospitals have to choose between standardized, mechanical bed-washers advised in national guidance and manual cleaning. To evaluate the quality of mechanical and manual bed-cleaning regimens. The multi-faceted analysis of bed-cleaning regimens consisted of three steps. In Step 1, the training of the domestic service team was evaluated. In Step 2, the cleaning quality of manual and mechanical regimens was assessed. Soiled beds, obtained at random, from different departments were evaluated using microbiological analysis (N = 40) and ATP (N = 20). ATP and microbiological contamination were measured in five predetermined locations on all beds. In Step 3, manual cleaning was introduced over a two-month pilot study at the surgical short-stay unit, and beds from other departments were processed according to the 'gold standard' mechanical cleaning. ATP levels were evaluated in three locations on 300 beds after cleaning. Training was found to improve the quality of cleaning significantly. Mechanical cleaning resulted in significantly lower ATP levels than manual cleaning. Mechanical cleaning shows less variation and results in consistently lower ATP levels than manual cleaning. Copyright © 2015 The Healthcare Infection Society. Published by Elsevier Ltd. All rights reserved.
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Chiesa, L M; Labella, G F; Giorgi, A; Panseri, S; Pavlovic, R; Bonacci, S; Arioli, F
2016-07-01
Bee products, such as honey, are widely consumed as food and consumer interest is currently oriented towards organic foods. Regarding this, the European Commission establishes that the qualification of organic honey and other beekeeping products as being from organic production is closely bound with the characteristics of hive treatments as well as the quality of the environment. Agricultural contamination with pesticides is a challenging problem that needs to be fully addressed, in particular in the field of organic production systems. In this study, the occurrence of different classes of contaminants selected as representative of potential contamination sources were investigated in 59 organic honeys: organochlorines, OCs; organophosphates, OPs; polychlorobiphenyls, PCBs and polybromodiphenylethers, PBDEs. A method based on Accelerated Solvent Extraction with "in line" clean-up and GC-MS/MS detection was developed to detect contaminants. Residues of many pesticides were found in most of the samples investigated. The majority of honey samples contained at least one of the pesticides, even if their concentrations were found to be lower than its MRL. Diazinon, Mevinphos, Coumaphos, Chlorpyrifos and Quinoxyfen were the residues frequently detected in samples coming from the apple and citrus orchard areas. Furthermore, the results of the present study show that the presence of the residue in organic honey may also be affected by the geographical area (e.g. the presence of an agricultural system) confirming honey bee and beehive matrices as appropriate sentinels for monitoring contamination in the environment. The optimised method proved to be simple and rapid, requiring small sample sizes and minimising solvent consumption, due to the ASE having an "in line" clean-up step. Copyright © 2016 Elsevier Ltd. All rights reserved.
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Nicoara, Simona C.; Turner, Nicholas W.; Minnikin, David E.; Lee, Oona Y.-C.; O'Sullivan, Denise M.; McNerney, Ruth; Mutetwa, Reggie; Corbett, Liz E.; Morgan, Geraint H.
2015-01-01
A proof of principle gas chromatography–mass spectrometry method is presented, in combination with clean up assays, aiming to improve the analysis of methyl mycocerosate tuberculosis biomarkers from sputum. Methyl mycocerosates are generated from the transesterification of phthiocerol dimycocerosates (PDIMs), extracted in petroleum ether from sputum of tuberculosis suspect patients. When a high matrix background is present in the sputum extracts, the identification of the chromatographic peaks corresponding to the methyl derivatives of PDIMs analytes may be hindered by the closely eluting methyl ether of cholesterol, usually an abundant matrix constituent frequently present in sputum samples. The purification procedures involving solid phase extraction (SPE) based methods with both commercial Isolute-Florisil cartridges, and purpose designed molecularly imprinted polymeric materials (MIPs), resulted in cleaner chromatograms, while the mycocerosates are still present. The clean-up performed on solutions of PDIMs and cholesterol standards in petroleum ether show that, depending on the solvent mix and on the type of SPE used, the recovery of PDIMs is between 64 and 70%, whilst most of the cholesterol is removed from the system. When applied to petroleum ether extracts from representative sputum samples, the clean-up procedures resulted in recoveries of 36–68% for PDIMs, allowing some superior detection of the target analytes. PMID:25728371
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NASA Astrophysics Data System (ADS)
Hesheng, Shi; Junzhang, Zhu; Huaning, Qiu; yu, Shu; Jianyao, Wu; Zulie, Long
Timing of oil or gas emplacements is a new subject in isotopic geochronology and petroleum geology. Hamilton et al. expounded the principle of the illite K-Ar age: Illite is often the last or one of the latest mineral cements to form prior to hydrocarbon accumulation. Since the displacement of formation water by hydrocarbons will cause silicate diagenesis to cease, K-Ar ages for illite will constrain the timing of this event, and also constrain the maximum age of formation of the trap structure. In this study, the possibility of authigenic illites 40Ar- 39Ar dating has been investigated. The illite samples were separated from the Tertiary sandstones in three rich oil reservoir belts within the Huizhou sag by cleaning, fracturing by cycled cooling-heating, soxhlet-extraction with solvents of benzene and methanol and separating with centrifugal machine. If oil is present in the separated samples, ionized organic fragments with m/e ratios of 36 to 40 covering the argon isotopes will be yielded by the ion source of a mass spectrometer, resulting in wrong argon isotopic analyses and wrong 40Ar- 39Ar ages. The preliminary experiments of illite by heating did show the presence of ionized organic fragments with m/e ratios of 36 to 44. In order to clean up the organic gases completely and obtain reliable analysis results, a special purification apparatus has been established by Qiu et al. and proved valid by the sequent illite analyses. All the illite samples by 40Ar- 39Ar IR-laser stepwise heating yield stair-up age spectra in lower laser steps and plateaux in higher laser steps. The youngest apparent ages corresponding to the beginning steps are reasonable to be interpreted for the hydrocarbon accumulation ages. The weighted mean ages of the illites from the Zhuhai and Zhujiang Formations are (12.1 ± 1.1) Ma and (9.9 ± 1.2) Ma, respectively. Therefore, the critical emplacement of petroleum accumulation in Zhujiang Formation in Huizhou sag took place in ca 10 Ma. Late fault activity strengthened the entrance of hydrocarbon fluids into the oil systems based on the data of the studies of the fault evolvement history, petroleum system combinations, and homogeneous temperatures of fluid inclusions.
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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.
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Optimisation of olive oil phenol extraction conditions using a high-power probe ultrasonication.
Jerman Klen, T; Mozetič Vodopivec, B
2012-10-15
A new method of ultrasound probe assisted liquid-liquid extraction (US-LLE) combined with a freeze-based fat precipitation clean-up and HPLC-DAD-FLD-MS detection is described for extra virgin olive oil (EVOO) phenol analysis. Three extraction variables (solvent type; 100%, 80%, 50% methanol, sonication time; 5, 10, 20 min, extraction steps; 1-5) and two clean-up methods (n-hexane washing vs. low temperature fat precipitation) were studied and optimised with aim to maximise extracts' phenol recoveries. A three-step extraction of 10 min with pure methanol (5 mL) resulted in the highest phenol content of freeze-based defatted extracts (667 μg GAE g(-1)) from 10 g of EVOO, providing much higher efficiency (up to 68%) and repeatability (up to 51%) vs. its non-sonicated counterpart (LLE-agitation) and n-hexane washing. In addition, the overall method provided high linearity (r(2)≥0.97), precision (RSD: 0.4-9.3%) and sensitivity with LODs/LOQs ranging from 0.03 to 0.16 μg g(-1) and 0.10-0.51 μg g(-1) of EVOO, respectively. Copyright © 2012 Elsevier Ltd. All rights reserved.
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ANALYSIS OF SAMPLES FROM TANK 5F CHEMICAL CLEANING
DOE Office of Scientific and Technical Information (OSTI.GOV)
Poirier, M.; Fink, S.
2011-03-07
The Savannah River Site (SRS) is preparing Tank 5F for closure. The first step in preparing the tank for closure is mechanical sludge removal. Following mechanical sludge removal, SRS performed chemical cleaning with oxalic acid to remove the sludge heel. Personnel are currently assessing the effectiveness of the chemical cleaning. SRS personnel collected liquid samples during chemical cleaning and submitted them to Savannah River National Laboratory (SRNL) for analysis. Following chemical cleaning, they collected a solid sample (also known as 'process sample') and submitted it to SRNL for analysis. The authors analyzed these samples to assess the effectiveness of themore » chemical cleaning process. The conclusions from this work are: (1) With the exception of iron, the dissolution of sludge components from Tank 5F agreed with results from the actual waste demonstration performed in 2007. The fraction of iron removed from Tank 5F by chemical cleaning was significantly less than the fraction removed in the SRNL demonstrations. The likely cause of this difference is the high pH following the first oxalic acid strike. (2) Most of the sludge mass remaining in the tank is iron and nickel. (3) The remaining sludge contains approximately 26 kg of barium, 37 kg of chromium, and 37 kg of mercury. (4) Most of the radioactivity remaining in the residual material is beta emitters and {sup 90}Sr. (5) The chemical cleaning removed more than {approx} 90% of the uranium isotopes and {sup 137}Cs. (6) The chemical cleaning removed {approx} 70% of the neptunium, {approx} 83% of the {sup 90}Sr, and {approx} 21% of the {sup 60}Co. (7) The chemical cleaning removed less than 10% of the plutonium, americium, and curium isotopes. (8) The chemical cleaning removed more than 90% of the aluminium, calcium, and sodium from the tank. (9) The cleaning operations removed 61% of lithium, 88% of non-radioactive strontium, and 65% of zirconium. The {sup 90}Sr and non-radioactive strontium were measured by different methods, and the differences in the fraction removed are not statistically significant. (10) Chemical cleaning removed 10-50% of the barium, chromium, iron, magnesium, manganese, and silicon. (11) Chemical cleaning removed only {approx}1% of the nickel.« less
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NASA Astrophysics Data System (ADS)
Larsen, B. R.; Brussol, C.; Kotzias, D.; Veltkamp, T.; Zwaagstra, O.; Slanina, J.
A method has been developed for the preparation of samples for radiocarbon ( 14C) measurements of carbonyl compounds in the atmosphere. Sampling on 25 ml 2,4-dinitrophenylhydrazine (DNPH)- coated silica gel cartridges can be carried out with up to 10.000 ℓ of ambient air with no adverse effects on sample integrity. Methods for the selective clean-up of the extracts have been investigated. This is a necessary step in preparing ambient carbonyl samples for a measurement of the radiocarbon ( 14C) content. The method which gave the best results include extraction of the DNPH cartridge with CH 3CN and purification of the carbonyl hydrazones over activated silica gel to remove excess DNPH and non target compounds. This method has been validated with laboratory samples and has been proved to give reliable results The radiocarbon data from the first field experiment showed that ambient air over a semi-rural test site in Ispra, Italy on a late summer day contained mainly five carbonyls (formaldehyde>acetaldehyde>acetone>propanal>butanal) of a mixed biogenic (41-57%) and anthropogenic (43-59%) origin. The method will be used in future monitoring of radiocarbon ( 14C) on a number of test sites in Europe.
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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.
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Impact of egg disinfection of hatching eggs on the eggshell microbiome and bacterial load.
Olsen, R; Kudirkiene, E; Thøfner, I; Pors, S; Karlskov-Mortensen, P; Li, L; Papasolomontos, S; Angastiniotou, C; Christensen, J
2017-09-01
Disinfection of hatching eggs is essential to ensure high quality production of broilers. Different protocols are followed in different hatcheries; however, only limited scientific evidence on how the disinfection procedures impact the microbiome is available. The aim of the present study was to characterize the microbiome and aerobic bacterial load of hatching eggs before disinfection and during the subsequent disinfection steps. The study included a group of visibly clean and a group of visibly dirty eggs. For dirty eggs, an initial wash in chlorine was performed, hereafter all eggs were submitted to two times fumigation and finally spray disinfection. The eggshell microbiome was characterized by sequencing of the total amount of 16S rRNA extracted from each sample, consisting of shell surface swabs of five eggs from the same group. In addition, the number of colony forming units (cfu) under aerobic conditions was established for each disinfection step. The disinfection procedure reduced the bacterial load from more than 104 cfu (initially visibly clean eggs) and 105 cfu (initially visibly dirty eggs) to less than 10 cfu per sample after disinfection for both groups of eggs. The microbiome of both initially visibly clean and initially visibly dirty eggs had the highest abundances of the phyla Firmicutes, Proteobacteria and Bacteroidetes. Within the phyla Firmicutes the relative abundances of Clostridiales decreased while Lactobacillus increased from before to after final disinfection. In conclusion, the investigated disinfection procedure is effective in reducing the bacterial load, and by adding a chlorine wash for initially visibly dirty eggs, the microbiome of initially visibly clean and initially visibly dirty eggs had a highly similar microflora after the final disinfection step. © 2017 Poultry Science Association Inc.
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Clean Up Your School Custodial Program.
ERIC Educational Resources Information Center
Steller, Arthur W.; Pell, Carroll
1986-01-01
Administrators can improve their school's custodial program by following steps that increase productivity, reduce costs, and provide long-term benefits of higher cleanliness standards. Administrators should work toward improved building cleanliness by insisting on a school board policy that establishes objectives for the custodial department.…
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A Module Experimental Process System Development Unit (MEPSDU). [flat plate solar arrays
NASA Technical Reports Server (NTRS)
1981-01-01
The development of a cost effective process sequence that has the potential for the production of flat plate photovoltaic modules which meet the price goal in 1986 of 70 cents or less per Watt peak is described. The major accomplishments include (1) an improved AR coating technique; (2) the use of sand blast back clean-up to reduce clean up costs and to allow much of the Al paste to serve as a back conductor; and (3) the development of wave soldering for use with solar cells. Cells were processed to evaluate different process steps, a cell and minimodule test plan was prepared and data were collected for preliminary Samics cost analysis.
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Qu, Zhipeng; Bai, Xiuzhi; Zhang, Ting; Yang, Zhaoguang
2017-03-01
An efficient sample extraction and clean-up method was developed for simultaneous determination of five amide herbicides (alachlor, acetochlor, propisochlor, metazachlor, and butachlor) in fish samples. The protocol consisted of ultrasound-assisted solvent extraction and solid-phase extraction clean-up. In detail, aliquots of homogenized fish flesh were thoroughly mixed with 20 mL of n-hexane and then extracted with ultrasonication for 40 min. Each sample was centrifuged and the supernatant was collected for the subsequent clean-up. For the sample preparation, the above supernatant was processed with a C 18 column with 3 mL of dichloromethane/n-hexane (1:1, v/v) as the eluant. Then the samples were analyzed by gas chromatography with electron capture detection. The correlation coefficients of the five calibration curves were 0.9976-0.9998 (n = 3). The limits of detection (S/N = 3, n = 11) and limits of quantification (S/N = 10, n = 11) were 0.19-0.42 and 0.63-1.39 μg/kg, respectively. The recoveries of this method were 71.2-92.6% with good precision (<4.7% relative standard deviations, n = 6). The developed method was successfully applied to monitor the five amide herbicides in fish samples collected from different cities. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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NASA Astrophysics Data System (ADS)
Mbukwa, Elbert A.; Msagati, Titus A. M.; Mamba, Bhekie B.
Harmful algal blooms (HABs) are increasingly becoming of great concern to water resources worldwide due to indiscriminate waste disposal habits resulting in water pollution and eutrophication. When cyanobacterial cells lyse (burst) they release toxins called microcystins (MCs) that are well known for their hepatotoxicity (causing liver damage) and have been found in eutrophic lakes, rivers, wastewater ponds and other water reservoirs. Prolonged exposure to low concentrated MCs are equally of health importance as they are known to be bioaccumulative and even at such low concentration do exhibit toxic effects to aquatic animals, wildlife and human liver cells. The application of common treatment processes for drinking water sourced from HABs infested reservoirs have the potential to cause algal cell lyses releasing low to higher amounts of MCs in finished water. Trace microcystins in water/tissue can be analyzed and quantified using Liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) following solid-phase extraction (SPE) sample clean-up procedures. However, extracting MCs from algal samples which are rich in chlorophyll pigments and other organic matrices the SPE method suffers a number of drawbacks, including cartridge clogging, long procedural steps and use of larger volumes of extraction solvents. We applied a supported liquid membrane (SLM) based technique as an alternative sample clean-up method for LC-ESI-MS analysis of MCs from both water and algal cells. Four (4) MC variants (MC-RR, -YR, -LR and -WR) from lyophilized cells of Microcystis aeruginosa and water collected from a wastewater pond were identified) and quantified using LC-ESI-MS following a SLM extraction and liquid partitioning step, however, MC-WR was not detected from water extracts. Within 45 min of SLM extraction all studied MCs were extracted and pre-concentrated in approximately 15 μL of an acceptor phase at an optimal pH 2.02 of the donor phase (sample). The highest total quantifiable intracellular and extracellular MCs were 37.039 ± 0.087 μg/g DW and 5.123 ± 0.018 μg/L, respectively. The concentrations of MC-RR were the highest from all samples studied recording maximum values of 21.579 ± 0.066 μg/g DW and 3.199 ± 0.012 μg/L for intracellular and extracellular quantities, respectively.
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Modified cleaning method for biomineralized components
NASA Astrophysics Data System (ADS)
Tsutsui, Hideto; Jordan, Richard W.
2018-02-01
The extraction and concentration of biomineralized components from sediment or living materials is time consuming and laborious and often involves steps that remove either the calcareous or siliceous part, in addition to organic matter. However, a relatively quick and easy method using a commercial cleaning fluid for kitchen drains, sometimes combined with a kerosene soaking step, can produce remarkable results. In this study, the method is applied to sediments and living materials bearing calcareous (e.g., coccoliths, foraminiferal tests, holothurian ossicles, ichthyoliths, and fish otoliths) and siliceous (e.g., diatom valves, silicoflagellate skeletons, and sponge spicules) components. The method preserves both components in the same sample, without etching or partial dissolution, but is not applicable to unmineralized components such as dinoflagellate thecae, tintinnid loricae, pollen, or plant fragments.
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ERIC Educational Resources Information Center
Lind, Georgia J.
2004-01-01
A hands on activity involving density, frequency and biomass using transects, quadrats and a local good deed by cleaning up the neighborhood while practicing important techniques in ecology is detailed. The activity is designed for KCC-STEP, whose primary goal is to expand the scientific knowledge and research experiences of their students, who…
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Hoffman, G.L.; Fishman, M. J.; Garbarino, J.R.
1996-01-01
Water samples for trace-metal determinations routinely have been prepared in open laboratories. For example, the U.S. Geological Survey method I-3485-85 (Extraction Procedure, for Water- Suspended Sediment) is performed in a laboratory hood on a laboratory bench without any special precautions to control airborne contamination. This method tends to be contamination prone for several trace metals primarily because the samples are transferred, acidified, digested, and filtered in an open laboratory environment. To reduce trace-metal contamination of digested water samples, procedures were established that rely on minimizing sample-transfer steps and using a class-100 clean bench during sample filtration. This new procedure involves the following steps: 1. The sample is acidified with HCl directly in the original water-sample bottle. 2. The water-sample bottle with the cap secured is heated in a laboratory oven. 3. The digestate is filtered in a class-100 laminar-flow clean bench. The exact conditions used (that is, oven temperature, time of heating, and filtration methods) for this digestion procedure are described. Comparisons between the previous U.S Geological Survey open-beaker method I-3485-85 and the new in-bottle procedure for synthetic and field-collected water samples are given. When the new procedure is used, blank concentrations for most trace metals determined are reduced significantly.
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Bodero, Marcia; Bovee, Toine F H; Wang, Si; Hoogenboom, Ron L A P; Klijnstra, Mirjam D; Portier, Liza; Hendriksen, Peter J M; Gerssen, Arjen
2018-02-01
The neuro-2a bioassay is considered as one of the most promising cell-based in vitro bioassays for the broad screening of seafood products for the presence of marine biotoxins. The neuro-2a assay has been shown to detect a wide array of toxins like paralytic shellfish poisons (PSPs), ciguatoxins, and also lipophilic marine biotoxins (LMBs). However, the neuro-2a assay is rarely used for routine testing of samples due to matrix effects that, for example, lead to false positives when testing for LMBs. As a result there are only limited data on validation and evaluation of its performance on real samples. In the present study, the standard extraction procedure for LMBs was adjusted by introducing an additional clean-up step with n-hexane. Recovery losses due to this extra step were less than 10%. This wash step was a crucial addition in order to eliminate false-positive outcomes due to matrix effects. Next, the applicability of this assay was assessed by testing a broad range of shellfish samples contaminated with various LMBs, including diarrhetic shellfish toxins/poisons (DSPs). For comparison, the samples were also analysed by LC-MS/MS. Standards of all regulated LMBs were tested, including analogues of some of these toxins. The neuro-2a cells showed good sensitivity towards all compounds. Extracts of 87 samples, both blank and contaminated with various toxins, were tested. The neuro-2a outcomes were in line with those of LC-MS/MS analysis and support the applicability of this assay for the screening of samples for LMBs. However, for use in a daily routine setting, the test might be further improved and we discuss several recommended modifications which should be considered before a full validation is carried out.
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Grande-Martínez, Ángel; Arrebola, Francisco Javier; Moreno, Laura Díaz; Vidal, José Luis Martínez; Frenich, Antonia Garrido
2015-01-01
A rapid and sensitive multiresidue method was developed and validated for the determination of around 100 pesticides in dry samples (rice and wheat flour) by ultra-performance LC coupled to a triple quadrupole mass analyzer working in tandem mode (UPLC/QqQ-MS/MS). The sample preparation step was optimized for both matrixes. Pesticides were extracted from rice samples using aqueous ethyl acetate, while aqueous acetonitrile extraction [modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method] was used for wheat flour matrixes. In both cases the extracts were then cleaned up by dispersive solid phase extraction with MgSO4 and primary secondary amine+C18 sorbents. A further cleanup step with Florisil was necessary to remove fat in wheat flour. The method was validated at two concentration levels (3.6 and 40 μg/kg for most compounds), obtaining recoveries ranging from 70 to 120%, intraday and interday precision values≤20% expressed as RSDs, and expanded uncertainty values≤50%. The LOQ values ranged between 3.6 and 20 μg/kg, although it was set at 3.6 μg/kg for the majority of the pesticides. The method was applied to the analysis of 20 real samples, and no pesticides were detected.
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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.
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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.
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NASA Technical Reports Server (NTRS)
Tevebaugh, M. D.
1971-01-01
An experimental portable system used to control surgically induced infections is described. The system consists of a portable clean room comprised of a laminar flow filter system consistent with Federal standards; a helmet-shoulder pad assembly; a communication system; a helmet ventilation system; a transparent walled enclosure; and surgical gowns. Guidelines for the set up and operation of such equipment are given along with corrective steps to use in case of system malfunctions. Cleaning procedures, maintenance requirements, and disassembly and transfer particulars are included.
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USING WASTE TO CLEAN UP THE ENVIRONMENT: CELLULOSIC ETHANOL, THE FUTURE OF FUELS
In the process of converting municipal solid waste (MSW) into ethanol we optimized the first two major steps of pretreatment and enzymatic hydrolysis stages to enhance the sugar yield and to reduce the cost. For the pretreatment process, we tested different parameters of react...
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NASA Technical Reports Server (NTRS)
Ayap, Shanti; Fisher, Forest; Gladden, Roy; Khanampompan, Teerapat
2008-01-01
This software tool saves time and reduces risk by automating two labor-intensive and error-prone post-processing steps required for every DKF [DSN (Deep Space Network) Keyword File] that MRO (Mars Reconnaissance Orbiter) produces, and is being extended to post-process the corresponding TSOE (Text Sequence Of Events) as well. The need for this post-processing step stems from limitations in the seq-gen modeling resulting in incorrect DKF generation that is then cleaned up in post-processing.
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NASA Astrophysics Data System (ADS)
Gold, A. U.; Sullivan, S. M.; Manning, C. L. B.; Ledley, T. S.; Youngman, E.; Taylor, J.; Niepold, F., III; Kirk, K.; Lockwood, J.; Bruckner, M. Z.; Fox, S.
2017-12-01
The impacts of climate change are a critical societal challenge of the 21st century. Educating students about the globally connected climate system is key in supporting the development of mitigation and adaptation strategies. Systems thinking is required for students to understand the complex, dynamic climate systems and the role that humans play within them. The interdisciplinary nature of climate science challenges educators, who often don't have formal training in climate science, to identify resources that are scientifically accurate before weaving them together into units that teach about the climate system. The Climate Literacy and Energy Awareness Network (CLEAN) supports this work by providing over 700 peer-reviewed, classroom-ready resources on climate and energy topics. The resource collection itself provide only limited instructional guidance, so educators need to weave the resources together to build multi-dimensional lessons that develop systems thinking skills. The Next Generation Science Standards (NGSS) science standards encourage educators to teach science in a 3-dimensional approach that trains students in systems thinking. The CLEAN project strives to help educators design NGSS-style, three-dimensional lessons about the climate system. Two approaches are currently being modeled on the CLEAN web portal. The first is described in the CLEAN NGSS "Get Started Guide" which follows a step-by-step process starting with the Disciplinary Core Idea and then interweaves the Cross-Cutting Concepts (CCC) and the Science and Engineering Practices (SEP) based on the teaching strategy chosen for the lesson or unit topic. The second model uses a climate topic as a starting place and the SEP as the guide through a four-step lesson sequence called "Earth Systems Investigations". Both models use CLEAN reviewed lessons as the core activity but provide the necessary framework for classroom implementation. Sample lessons that were developed following these two approaches are provided on the CLEAN web portal (cleanet.org).
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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.
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Hurst, Jerod J; Wallace, Josh S; Aga, Diana S
2018-04-01
Ionophore antimicrobials are heavily used in the livestock industries, both for preventing animal infection by coccidia protozoa and for increasing feed efficiency. Ionophores are excreted mostly unmetabolized and are released into the environment when manure is land-applied to fertilize croplands. Here, an analytical method was optimized to study the occurrences of five ionophore residues (monensin, lasalocid, maduramycin, salinomycin, and narasin) in dairy manure after solid-liquid separation and further treatment of the liquid manure by a membrane-based treatment system. Ionophore residues from the separated solid manure (dewatered manure) and suspended solids of manure slurry samples were extracted using ultrasonication with methanol, followed by sample clean-up using solid phase extraction (SPE) and subsequent analysis via liquid chromatography-tandem mass spectrometry (LC-MS/MS). The use of an ethyl acetate and methanol (1:1 v:v) mixture as an SPE eluent resulted in higher recoveries and lower method quantitation limits (MQL), when compared to using methanol. Overall recoveries from separated solid manure ranged from 73 to 134%. Liquid manure fractions were diluted with Nanopure™ water and cleaned up using SPE, where recoveries ranged from 51 to 100%. The developed extraction and LC-MS/MS methods were applied to analyze dairy manure samples subjected to an advanced manure treatment process involving a membrane-based filtration step (reverse osmosis). Monensin and lasalocid were detected at higher concentrations in the suspended solid fractions (4.40-420 ng/g for lasalocid and 85-1950 ng/g for monensin) compared to the liquid fractions (
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Tharwat, Alaa; Moemen, Yasmine S; Hassanien, Aboul Ella
2016-12-09
Measuring toxicity is one of the main steps in drug development. Hence, there is a high demand for computational models to predict the toxicity effects of the potential drugs. In this study, we used a dataset, which consists of four toxicity effects:mutagenic, tumorigenic, irritant and reproductive effects. The proposed model consists of three phases. In the first phase, rough set-based methods are used to select the most discriminative features for reducing the classification time and improving the classification performance. Due to the imbalanced class distribution, in the second phase, different sampling methods such as Random Under-Sampling, Random Over-Sampling and Synthetic Minority Oversampling Technique are used to solve the problem of imbalanced datasets. ITerative Sampling (ITS) method is proposed to avoid the limitations of those methods. ITS method has two steps. The first step (sampling step) iteratively modifies the prior distribution of the minority and majority classes. In the second step, a data cleaning method is used to remove the overlapping that is produced from the first step. In the third phase, Bagging classifier is used to classify an unknown drug into toxic or non-toxic. The experimental results proved that the proposed model performed well in classifying the unknown samples according to all toxic effects in the imbalanced datasets.
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STEPS: Modeling and Simulating Complex Reaction-Diffusion Systems with Python
Wils, Stefan; Schutter, Erik De
2008-01-01
We describe how the use of the Python language improved the user interface of the program STEPS. STEPS is a simulation platform for modeling and stochastic simulation of coupled reaction-diffusion systems with complex 3-dimensional boundary conditions. Setting up such models is a complicated process that consists of many phases. Initial versions of STEPS relied on a static input format that did not cleanly separate these phases, limiting modelers in how they could control the simulation and becoming increasingly complex as new features and new simulation algorithms were added. We solved all of these problems by tightly integrating STEPS with Python, using SWIG to expose our existing simulation code. PMID:19623245
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Capillary-Force-Assisted Clean-Stamp Transfer of Two-Dimensional Materials.
Ma, Xuezhi; Liu, Qiushi; Xu, Da; Zhu, Yangzhi; Kim, Sanggon; Cui, Yongtao; Zhong, Lanlan; Liu, Ming
2017-11-08
A simple and clean method of transferring two-dimensional (2D) materials plays a critical role in the fabrication of 2D electronics, particularly the heterostructure devices based on the artificial vertical stacking of various 2D crystals. Currently, clean transfer techniques rely on sacrificial layers or bulky crystal flakes (e.g., hexagonal boron nitride) to pick up the 2D materials. Here, we develop a capillary-force-assisted clean-stamp technique that uses a thin layer of evaporative liquid (e.g., water) as an instant glue to increase the adhesion energy between 2D crystals and polydimethylsiloxane (PDMS) for the pick-up step. After the liquid evaporates, the adhesion energy decreases, and the 2D crystal can be released. The thin liquid layer is condensed to the PDMS surface from its vapor phase, which ensures the low contamination level on the 2D materials and largely remains their chemical and electrical properties. Using this method, we prepared graphene-based transistors with low charge-neutral concentration (3 × 10 10 cm -2 ) and high carrier mobility (up to 48 820 cm 2 V -1 s -1 at room temperature) and heterostructure optoelectronics with high operation speed. Finally, a capillary-force model is developed to explain the experiment.
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Oellig, Claudia; Schwack, Wolfgang
2012-10-19
Efficient clean-up is indispensable for preventing matrix effects in multi-residue analysis of pesticides in food by liquid and gas chromatography (LC and GC) coupled to mass spectrometry (MS). High-throughput planar solid phase extraction (HTpSPE) was recently introduced as a new clean-up concept in residue analysis of pesticides in fruit and vegetables (C. Oellig, W. Schwack, 2011 [45]). Thin-layer chromatography (TLC) was used to completely separate pesticides from matrix compounds and to focus them into a sharp zone, followed by extraction of the target zone by the TLC-MS interface. As rather challenging matrices, tea samples were chosen in this study. Besides chlorophylls and polyphenols, high amount of caffeine is co-extracted resulting in strong matrix effects both in LC-MS and GC-MS. The former HTpSPE procedure was adapted to initial extracts of green and black tea resulting in colorless extracts nearly free of matrix effects and interferences, as shown for seven chemically representative pesticides (acetamiprid, penconazole, azoxystrobin, chlorpyrifos, pirimicarb, fenarimol, and mepanipyrim). LC-MS/MS calibration curves obtained in the range of 0.002-0.5 mg/kg from matrix-matched standards and solvent standards were nearly identical and demonstrated the effectiveness of clean-up by HTpSPE. Mean recoveries determined by LC-MS/MS against solvent standards at spiking levels of 0.01 and 0.1 mg/kg ranged between 72 and 114% with relative standard deviations (RSDs) of 0.7-4.7% (n=4), while LC-MS measurements of tea samples spiked at 1 mg/kg provided recoveries of 81-104% with RSDs of 1.2-4.9% (n=6). Using LC-MS/MS, the method showed high sensitivity with signal-to-noise ratios>10 for concentrations below 0.002 mg/kg. HTpSPE of one sample was done in a few minutes, while numerous samples were cleaned in parallel at minimal costs with very low sample and solvent consumption. Copyright © 2012 Elsevier B.V. All rights reserved.
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Beltrán, Eduardo; Ibáñez, María; Sancho, Juan Vicente; Hernández, Félix
2014-01-01
Sensitive and reliable analytical methodology has been developed for the measurement of patulin in regulated foodstuffs by using ultra-high-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) with triple quadrupole analyser. Solid samples were extracted with ethyl acetate, while liquid samples were directly injected into the chromatographic system after dilution and filtration without any clean-up step. Chromatographic separation was achieved in less than 4min. Electrospray (ESI) and atmospheric pressure chemical ionisation (APCI) sources were evaluated, in order to assess matrix effects. The use of ESI source caused strong signal suppression in samples; however, matrix effect was negligible using APCI, allowing quantification with calibration standards prepared in solvent. The method was validated in four different apple matrices (juice, fruit, puree and compote) at two concentrations at the low μgkg(-1) level. Average recoveries (n=5) ranged from 71% to 108%, with RSDs lower than 14%. Copyright © 2013 Elsevier Ltd. All rights reserved.
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Cleaning of nanopillar templates for nanoparticle collection using PDMS
NASA Astrophysics Data System (ADS)
Merzsch, S.; Wasisto, H. S.; Waag, A.; Kirsch, I.; Uhde, E.; Salthammer, T.; Peiner, E.
2011-05-01
Nanoparticles are easily attracted by surfaces. This sticking behavior makes it difficult to clean contaminated samples. Some complex approaches have already shown efficiencies in the range of 90%. However, a simple and cost efficient method was still missing. A commonly used silicone for soft lithography, PDMS, is able to mold a given surface. This property was used to cover surface-bonded particles from all other sides. After hardening the PDMS, particles are still embedded. A separation of silicone and sample disjoins also the particles from the surface. After this procedure, samples are clean again. This method was first tested with carbon particles on Si surfaces and Si pillar samples with aspect ratios up to 10. Experiments were done using 2 inch wafers, which, however, is not a size limitation for this method.
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Hop, Cornelis E C A; Cole, Mark J; Davidson, Ralph E; Duignan, David B; Federico, James; Janiszewski, John S; Jenkins, Kelly; Krueger, Suzanne; Lebowitz, Rebecca; Liston, Theodore E; Mitchell, Walter; Snyder, Mark; Steyn, Stefan J; Soglia, John R; Taylor, Christine; Troutman, Matt D; Umland, John; West, Michael; Whalen, Kevin M; Zelesky, Veronica; Zhao, Sabrina X
2008-11-01
Evaluation and optimization of drug metabolism and pharmacokinetic data plays an important role in drug discovery and development and several reliable in vitro ADME models are available. Recently higher throughput in vitro ADME screening facilities have been established in order to be able to evaluate an appreciable fraction of synthesized compounds. The ADME screening process can be dissected in five distinct steps: (1) plate management of compounds in need of in vitro ADME data, (2) optimization of the MS/MS method for the compounds, (3) in vitro ADME experiments and sample clean up, (4) collection and reduction of the raw LC-MS/MS data and (5) archival of the processed ADME data. All steps will be described in detail and the value of the data on drug discovery projects will be discussed as well. Finally, in vitro ADME screening can generate large quantities of data obtained under identical conditions to allow building of reliable in silico models.
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Detection and quantification of ionophore antibiotics in runoff, soil and poultry litter.
Sun, Peizhe; Barmaz, Delphine; Cabrera, Miguel L; Pavlostathis, Spyros G; Huang, Ching-Hua
2013-10-18
Ionophore antibiotics (IPAs) are widely used as coccidiostats in poultry and other livestock industries to promote growth and prevent infections. Because most of the ingested IPAs are excreted in poultry litter, which is primarily applied as grassland fertilizer, a significant amount of IPAs can be released into the litter-soil-water environment. A robust analytical method has been developed to quantify IPAs (monensin (MON), salinomycin (SAL) and narasin (NAR)) in complex environmental compartments including surface runoff, soil and poultry litter, with success to minimize matrix interference. The method for water samples involves solid-phase extraction (SPE) followed by liquid-liquid extraction (LLE) post-clean up steps. The method for solid samples involves bi-solvent LLE. IPAs were detected by HPLC-MS, with optimized parameters to achieve the highest sensitivity. Nigericin (NIG), an IPA not used in livestock industry, is successfully applied and validated as a surrogate standard. The method recoveries were at 92-95% and 81-85% in runoff samples from unfertilized and litter-fertilized fields, respectively. For solids, the method recoveries were at 93-99% in soils, and 79-83% in poultry litter samples. SAL was detected at up to 22mg/kg and MON and NAR at up to 4mg/kg in broiler litter from different farms. Up to 183μg/kg of MON was detected in litter-fertilized soils. All three IPAs were detected in the rainfall runoff from litter-fertilized lands at concentrations up to 9μg/L. Copyright © 2013 Elsevier B.V. All rights reserved.
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Pérez-Rodríguez, Michael; Pellerano, Roberto Gerardo; Pezza, Leonardo; Pezza, Helena Redigolo
2018-05-15
Tetracyclines are widely used for both the treatment and prevention of diseases in animals as well as for the promotion of rapid animal growth and weight gain. This practice may result in trace amounts of these drugs in products of animal origin, such as milk and eggs, posing serious risks to human health. The presence of tetracycline residues in foods can lead to the transmission of antibiotic-resistant pathogenic bacteria through the food chain. In order to ensure food safety and avoid exposure to these substances, national and international regulatory agencies have established tolerance levels for authorized veterinary drugs, including tetracycline antimicrobials. In view of that, numerous sensitive and specific methods have been developed for the quantification of these compounds in different food matrices. One will note, however, that the determination of trace residues in foods such as milk and eggs often requires extensive sample extraction and preparation prior to conducting instrumental analysis. Sample pretreatment is usually the most complicated step in the analytical process and covers both cleaning and pre-concentration. Optimal sample preparation can reduce analysis time and sources of error, enhance sensitivity, apart from enabling unequivocal identification, confirmation and quantification of target analytes. The development and implementation of more environmentally friendly analytical procedures, which involve the use of less hazardous solvents and smaller sample sizes compared to traditional methods, is a rapidly increasing trend in analytical chemistry. This review seeks to provide an updated overview of the main trends in sample preparation for the determination of tetracycline residues in foodstuffs. The applicability of several extraction and clean-up techniques employed in the analysis of foodstuffs, especially milk and egg samples, is also thoroughly discussed. Copyright © 2018 Elsevier B.V. All rights reserved.
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Wang, Ziming; Zhao, Xin; Xu, Xu; Wu, Lijie; Su, Rui; Zhao, Yajing; Jiang, Chengfei; Zhang, Hanqi; Ma, Qiang; Lu, Chunmei; Dong, Deming
2013-01-14
A single-step extraction-cleanup method, including microwave-assisted extraction (MAE) and micro-solid-phase extraction (μ-SPE), was developed for the extraction of ten organophosphorus pesticides in vegetable and fruit samples. Without adding any polar solvent, only one kind of non-polar solvent (hexane) was used as extraction solvent in the whole extraction step. Absorbing microwave μ-SPE device, was prepared by packing activated carbon with microporous polypropylene membrane envelope, and used as not only the sorbent in μ-SPE, but also the microwave absorption medium. Some experimental parameters effecting on extraction efficiency was investigated and optimized. 1.0 g of sample, 8 mL of hexane and three absorbing microwave μ-SPE devices were added in the microwave extraction vessel, the extraction was carried out under 400 W irradiation power at 60°C for 10 min. The extracts obtained by MAE-μ-SPE were directly analyzed by GC-MS without any clean-up process. The recoveries were in the range of 93.5-104.6%, and the relative standard deviations were lower than 8.7%. Copyright © 2012 Elsevier B.V. All rights reserved.
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Kafle, Amol; Klaene, Joshua; Hall, Adam B; Glick, James; Coy, Stephen L; Vouros, Paul
2013-07-15
There is continued interest in exploring new analytical technologies for the detection and quantitation of DNA adducts, biomarkers which provide direct evidence of exposure and genetic damage in cells. With the goal of reducing clean-up steps and improving sample throughput, a Differential Mobility Spectrometry/Mass Spectrometry (DMS/MS) platform has been introduced for adduct analysis. A DMS/MS platform has been utilized for the analysis of dG-ABP, the deoxyguanosine adduct of the bladder carcinogen 4-aminobiphenyl (4-ABP). After optimization of the DMS parameters, each sample was analyzed in just 30 s following a simple protein precipitation step of the digested DNA. A detection limit of one modification in 10^6 nucleosides has been achieved using only 2 µg of DNA. A brief comparison (quantitative and qualitative) with liquid chromatography/mass spectrometry is also presented highlighting the advantages of using the DMS/MS method as a high-throughput platform. The data presented demonstrate the successful application of a DMS/MS/MS platform for the rapid quantitation of DNA adducts using, as a model analyte, the deoxyguanosine adduct of the bladder carcinogen 4-aminobiphenyl. Copyright © 2013 John Wiley & Sons, Ltd.
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Cobb, J; Warwick, P; Carpenter, R C; Morrison, R T
1995-12-01
Strontium-90 may be determined by beta-counting its yttrium-90 daughter following separation by ion-chromatography, using a three column system comprising a chelating concentrator column, a cation-exchange column and an anion-exchange separator column. The column system has previously been applied to the determination of strontium-90 in water and urine samples. The applicability of the system to the analysis of milk is hampered by the large concentrations of calcium present, which significantly reduces the extraction of yttrium-90 by the concentrator column. A maximum of approximately 200 mg of calcium can be present for the successful extraction of yttrium-90, which greatly limits the quantity of milk that can be analysed. The quantity of milk analysed can be increased by the inclusion of a controlled precipitation step prior to the ion-chromatographic separation. The precipitation is carried out on acid digested milk samples by the addition of ammonia solution until the addition of one drop causes a reduction in pH resulting in the precipitation of calcium hydrogenphosphate. Under these conditions, approximately 20% of the calcium present in the original milk sample is precipitated, yttrium-90 is precipitated whereas strontium-90 is not precipitated. Dissolution of the precipitate, followed by separation of yttrium-90 using the ion-chromatography system facilitates the analysis of a litre of milk with recoveries of greater than 80%.
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Materials and manufacturing processes for increased life/reliability. [of turbine wheels
NASA Technical Reports Server (NTRS)
Duttweiler, R. E.
1977-01-01
Improvements in both quality and durability of disk raw material for both military and commercial engines necessitated an entirely new concept in raw material process control which imposes careful selection, screening and sampling of the basic alloy ingredients, followed by careful monitoring of the melting parameters in all phases of the vacuum melting sequence. Special care is taken to preclude solidification conditions that produce adverse levels of segregation. Melt furnaces are routinely cleaned and inspected for contamination. Ingots are also cleaned and inspected before entering the final melt step.
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Shen, Aijin; Wei, Jie; Yan, Jingyu; Jin, Gaowa; Ding, Junjie; Yang, Bingcheng; Guo, Zhimou; Zhang, Feifang; Liang, Xinmiao
2017-03-01
An orthogonal two-dimensional solid-phase extraction strategy was established for the selective enrichment of three aminoglycosides including spectinomycin, streptomycin, and dihydrostreptomycin in milk. A reversed-phase liquid chromatography material (C 18 ) and a weak cation-exchange material (TGA) were integrated in a single solid-phase extraction cartridge. The feasibility of two-dimensional clean-up procedure that experienced two-step adsorption, two-step rinsing, and two-step elution was systematically investigated. Based on the orthogonality of reversed-phase and weak cation-exchange procedures, the two-dimensional solid-phase extraction strategy could minimize the interference from the hydrophobic matrix existing in traditional reversed-phase solid-phase extraction. In addition, high ionic strength in the extracts could be effectively removed before the second dimension of weak cation-exchange solid-phase extraction. Combined with liquid chromatography and tandem mass spectrometry, the optimized procedure was validated according to the European Union Commission directive 2002/657/EC. A good performance was achieved in terms of linearity, recovery, precision, decision limit, and detection capability in milk. Finally, the optimized two-dimensional clean-up procedure incorporated with liquid chromatography and tandem mass spectrometry was successfully applied to the rapid monitoring of aminoglycoside residues in milk. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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From cookbooks to single sentences: The evolution of my labs
NASA Astrophysics Data System (ADS)
Morrison, Andrew
2014-11-01
Like many physics teachers, I love to have my students spend time working in the laboratory. There is often no better way to test an idea about how the physical world works than to actually set up an experiment and see if the idea can be ruled out or not. This process is an authentic representation of the scientific method, which can take a winding and unpredictable path rather than a clean step-by-step recipe that students want to believe science follows.
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40 CFR 281.35 - Release response and corrective action.
Code of Federal Regulations, 2014 CFR
2014-07-01
... soil and ground water, and any nearby surface waters. The extent of soil and ground water contamination... from UST systems are cleaned up through soil and ground water remediation and any other steps, as... § 280.67, the state must notify the affected public of all confirmed releases requiring a plan for soil...
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40 CFR 281.35 - Release response and corrective action.
Code of Federal Regulations, 2010 CFR
2010-07-01
... soil and ground water, and any nearby surface waters. The extent of soil and ground water contamination... from UST systems are cleaned up through soil and ground water remediation and any other steps, as... § 280.67, the state must notify the affected public of all confirmed releases requiring a plan for soil...
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Harvesting "Green-Collar" Jobs
ERIC Educational Resources Information Center
Roach, Ronald
2009-01-01
Emerging in recent years from the need for increased energy efficiency and conservation, greater reduction of greenhouse gas emissions, and stepped-up action to clean the environment, green jobs have arisen as a distinct employment sector within the U.S. and around the world. While social and political activists have taken the lead to make sure…
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40 CFR 281.35 - Release response and corrective action.
Code of Federal Regulations, 2013 CFR
2013-07-01
... soil and ground water, and any nearby surface waters. The extent of soil and ground water contamination... from UST systems are cleaned up through soil and ground water remediation and any other steps, as... § 280.67, the state must notify the affected public of all confirmed releases requiring a plan for soil...
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40 CFR 281.35 - Release response and corrective action.
Code of Federal Regulations, 2011 CFR
2011-07-01
... soil and ground water, and any nearby surface waters. The extent of soil and ground water contamination... from UST systems are cleaned up through soil and ground water remediation and any other steps, as... § 280.67, the state must notify the affected public of all confirmed releases requiring a plan for soil...
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Schrübbers, Lars C; Masís-Mora, Mario; Rojas, Elizabeth Carazo; Valverde, Bernal E; Christensen, Jan H; Cedergreen, Nina
2016-01-01
Glyphosate is a commonly applied herbicide in coffee plantations. Because of its non-selective mode of action it can damage the crop exposed through spray drift. Therefore, it is of interest to study glyphosate fate in coffee plants. The aim of this study was to develop an analytical method for accurate and precise quantification of glyphosate and its main metabolite aminomethylphosphonic acid (AMPA) at trace levels in coffee leaves using liquid chromatography with single-quadrupole mass spectrometry detection. The method is based on a two-step solid phase extraction (SPE) with an intermediate derivatization reaction using 9-fluorenylmethylchloroformate (FMOC). An isotope dilution method was used to account for matrix effects and to enhance the confidence in analyte identification. The limit of quantification (LOQ) for glyphosate and AMPA in coffee leaves was 41 and 111 μg kg(-1) dry weight, respectively. For the method optimization a design of experiments (DOE) approach was used. The sample clean-up procedure can be simplified for the analysis of less challenging matrices, for laboratories having a tandem mass spectrometry detector and for cases in which quantification limits above 0.1 mg kg(-1) are acceptable, which is often the case for glyphosate. The method is robust, possesses high identification confidence, while being suitable for most commercial and academic laboratories. All leaf samples from five coffee fields analyzed (n=21) contained glyphosate, while AMPA was absent. The simplified clean-up procedure was successfully validated for coffee leaves, rice, black beans and river water. Copyright © 2015 Elsevier B.V. All rights reserved.
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Chiap, P; Rbeida, O; Christiaens, B; Hubert, Ph; Lubda, D; Boos, K S; Crommen, J
2002-10-25
A new kind of silica-based restricted-access material (RAM) has been tested in pre-columns for the on-line solid-phase extraction (SPE) of basic drugs from directly injected plasma samples before their quantitative analysis by reversed-phase liquid chromatography (LC), using the column switching technique. The outer surface of the porous RAM particlescontains hydrophilic diol groups while sulphonic acid groups are bound to the internal surface, which gives the sorbent the properties of a strong cation exchanger towards low molecular mass compounds. Macromolecules such as proteins have no access to the internal surface of the pre-column due to their exclusion from the pores and are then flushed directly out. The retention capability of this novel packing material has been tested for some hydrophilic basic drugs, such as atropine, fenoterol, ipratropium, procaine, sotalol and terbutaline, used as model compounds. The influence of the composition of the washing liquid on the retention of the analytes in the pre-column has been investigated. The elution profiles of the different compounds and the plasma matrix as well as the time needed for the transfer of the analytes from the pre-column to the analytical column were determined in order to deduce the most suitable conditions for the clean-up step and develop on-line methods for the LC determination of these compounds in plasma. The cationic exchange sorbent was also compared to another RAM, namely RP-18 ADS (alkyl diol silica) sorbent with respect to retention capability towards basic analytes.
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Kampf, Günter; Degenhardt, Stina; Lackner, Sibylle; Ostermeyer, Christiane
2014-01-01
Background: It has recently been reported that reusable dispensers for surface disinfection tissues may be contaminated, especially with adapted Achromobacter species 3, when products based on surface-active ingredients are used. Fresh solution may quickly become recontaminated if dispensers are not processed adequately. Methods: We evaluated the abilities of six manual and three automatic processes for processing contaminated dispensers to prevent recolonisation of a freshly-prepared disinfectant solution (Mikrobac forte 0.5%). Dispensers were left at room temperature for 28 days. Samples of the disinfectant solution were taken every 7 days and assessed quantitatively for bacterial contamination. Results: All automatic procedures prevented recolonisation of the disinfectant solution when a temperature of 60–70°C was ensured for at least 5 min, with or without the addition of chemical cleaning agents. Manual procedures prevented recontamination of the disinfectant solution when rinsing with hot water or a thorough cleaning step was performed before treating all surfaces with an alcohol-based disinfectant or an oxygen-releaser. Other cleaning and disinfection procedures, including the use of an alcohol-based disinfectant, did not prevent recolonisation. Conclusions: These results indicate that not all processes are effective for processing reusable dispensers for surface-disinfectant tissues, and that a high temperature during the cleaning step or use of a biofilm-active cleaning agent are essential. PMID:24653973
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ASRM process development in aqueous cleaning
NASA Technical Reports Server (NTRS)
Swisher, Bill
1992-01-01
Viewgraphs are included on process development in aqueous cleaning which is taking place at the Aerojet Advanced Solid Rocket Motor (ASRM) Division under a NASA Marshall Space and Flight Center contract for design, development, test, and evaluation of the ASRM including new production facilities. The ASRM will utilize aqueous cleaning in several manufacturing process steps to clean case segments, nozzle metal components, and igniter closures. ASRM manufacturing process development is underway, including agent selection, agent characterization, subscale process optimization, bonding verification, and scale-up validation. Process parameters are currently being tested for optimization utilizing a Taguci Matrix, including agent concentration, cleaning solution temperature, agitation and immersion time, rinse water amount and temperature, and use/non-use of drying air. Based on results of process development testing to date, several observations are offered: aqueous cleaning appears effective for steels and SermeTel-coated metals in ASRM processing; aqueous cleaning agents may stain and/or attack bare aluminum metals to various extents; aqueous cleaning appears unsuitable for thermal sprayed aluminum-coated steel; aqueous cleaning appears to adequately remove a wide range of contaminants from flat metal surfaces, but supplementary assistance may be needed to remove clumps of tenacious contaminants embedded in holes, etc.; and hot rinse water appears to be beneficial to aid in drying of bare steel and retarding oxidation rate.
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Rodríguez-González, N; González-Castro, M J; Beceiro-González, E; Muniategui-Lorenzo, S; Prada-Rodríguez, D
2014-04-01
A method using dual process columns of Matrix Solid Phase Dispersion (MSPD) and Solid Phase Extraction (SPE) has been developed for extracting and cleaning-up of nine triazine herbicides (ametryn, atrazine, cyanazine, prometryn, propazine, simazine, simetryn, terbuthylazine and terbutryn) in seaweed samples. Under optimized conditions, samples were blended with 2g of octasilyl-derivatized silica (C8) and transferred into an SPE cartridge containing ENVI-Carb II/PSA (0.5/0.5 g) as a clean up co-sorbent. Then the dispersed sample was washed with 10 mL of n-hexane and triazines were eluted with 20 mL ethyl acetate and 5 mL acetonitrile. Finally the extract was concentrated to dryness, re-constituted with 1 mL methanol:water (1:1) and injected into the HPLC-DAD system. The linearity of the calibration curves was excellent in matrix matched standards, and yielded the coefficients of determination>0.995 for all the target analytes. The recoveries ranged from 75% to 100% with relative standard deviations lower than 7%. The achieved LOQs (<10 µg kg(-1)) for all triazines under study permits to ensure proper determination at the maximum allowed residue levels set in the European Union Legislation. Samples of three seaweeds were subjected to the procedure proving the suitability of MSPD method for the analysis of triazines in different seaweeds samples. Copyright © 2014 Elsevier B.V. All rights reserved.
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Cundell, A M; Bean, R; Massimore, L; Maier, C
1998-01-01
To determine the relationship between the sampling time of the environmental monitoring, i.e., viable counts, in aseptic filling areas and the microbial count and frequency of alerts for air, surface and personnel microbial monitoring, statistical analyses were conducted on 1) the frequency of alerts versus the time of day for routine environmental sampling conducted in calendar year 1994, and 2) environmental monitoring data collected at 30-minute intervals during routine aseptic filling operations over two separate days in four different clean rooms with multiple shifts and equipment set-ups at a parenteral manufacturing facility. Statistical analyses showed, except for one floor location that had significantly higher number of counts but no alert or action level samplings in the first two hours of operation, there was no relationship between the number of counts and the time of sampling. Further studies over a 30-day period at the floor location showed no relationship between time of sampling and microbial counts. The conclusion reached in the study was that there is no worst case time for environmental monitoring at that facility and that sampling any time during the aseptic filling operation will give a satisfactory measure of the microbial cleanliness in the clean room during the set-up and aseptic filling operation.
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Adapting sensory data for multiple robots performing spill cleanup
DOE Office of Scientific and Technical Information (OSTI.GOV)
Storjohann, K.; Saltzen, E.
1990-09-01
This paper describes a possible method of converting a single performing robot algorithm into a multiple performing robot algorithm without the need to modify previously written codes. The algorithm to be converted involves spill detection and clean up by the HERMIES-III mobile robot. In order to achieve the goal of multiple performing robots with this algorithm, two steps are taken. First, the task is formally divided into two sub-tasks, spill detection and spill clean-up, the former of which is allocated to the added performing robot, HERMIES-IIB. Second, a inverse perspective mapping, is applied to the data acquired by the newmore » performing robot (HERMIES-IIB), allowing the data to be processed by the previously written algorithm without re-writing the code. 6 refs., 4 figs.« less
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Rapid Sample Processing for Detection of Food-Borne Pathogens via Cross-Flow Microfiltration
Li, Xuan; Ximenes, Eduardo; Amalaradjou, Mary Anne Roshni; Vibbert, Hunter B.; Foster, Kirk; Jones, Jim; Liu, Xingya; Bhunia, Arun K.
2013-01-01
This paper reports an approach to enable rapid concentration and recovery of bacterial cells from aqueous chicken homogenates as a preanalytical step of detection. This approach includes biochemical pretreatment and prefiltration of food samples and development of an automated cell concentration instrument based on cross-flow microfiltration. A polysulfone hollow-fiber membrane module having a nominal pore size of 0.2 μm constitutes the core of the cell concentration instrument. The aqueous chicken homogenate samples were circulated within the cross-flow system achieving 500- to 1,000-fold concentration of inoculated Salmonella enterica serovar Enteritidis and naturally occurring microbiota with 70% recovery of viable cells as determined by plate counting and quantitative PCR (qPCR) within 35 to 45 min. These steps enabled 10 CFU/ml microorganisms in chicken homogenates or 102 CFU/g chicken to be quantified. Cleaning and sterilizing the instrument and membrane module by stepwise hydraulic and chemical cleaning (sodium hydroxide and ethanol) enabled reuse of the membrane 15 times before replacement. This approach begins to address the critical need for the food industry for detecting food pathogens within 6 h or less. PMID:24014538
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Cleanups In My Community (CIMC) - Superfund National Priority List (NPL) Sites, National Layer
This data layer provides access to Superfund National Priority List Sites as part of the CIMC web service. Superfund is a program administered by the EPA to locate, investigate, and clean up worst hazardous waste sites throughout the United States. EPA administers the Superfund program in cooperation with individual states and tribal governments. These sites include abandoned warehouses, manufacturing facilities, processing plants, and landfills - the key word here being abandoned.Only NPL sites have been included in Cleanups in My Community thus far. EPA maintains the NPL, which identifies for the States and the public those sites or other releases that appear to warrant remedial (long term) actions. These NPL sites fall into the following categories:Proposed: Sites may be proposed for the NPL and then may be placed on the NPL as final or be removed from the Proposed NPL.Final: Those sites placed on the NPL are called final, and for these sites, a cleanup remedy is selected and implemented. However, it may be several years after construction of the remedy is completed before the hazardous substances are completely cleaned up or controlled in place.Deleted: After the clean up process is complete, and appropriate reviews confirm the area is cleaned up or the hazards are controlled, sites can be deleted from the NPL.For more information on the data provided through this web service, please see the processing steps below, and see more information here: https://www.
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Small Particulate Contamination Survey Of Genesis Flight Sample 61423
NASA Technical Reports Server (NTRS)
Kuhlman, K. R.; Schmeling, M.; Gonzalez, C. P.; Allums, K. K.; Allton, J. H.; Burnett, D. S.
2016-01-01
The Genesis mission collected solar wind and brought it back to Earth in order to provide precise knowledge of solar isotopic and elemental compositions. The ions in the solar wind stop in the collectors at depths on the order of 10 to a few hundred nanometers. This shallow implantation layer is critical for scientific analysis of the composition of the solar wind and must be preserved throughout sample handling, cleaning, processing, distribution, preparation and analysis. We continue to work with the community of scientists analyzing Genesis samples using our unique laboratory facilities -- and, where needed, our unique cleaning techniques -- to significantly enhance the science return from the Genesis mission. This work is motivated by the need to understand the submicron contamination on the collectors in the Genesis payload as recovered from the crash site in the Utah desert, and -- perhaps more importantly -- how to remove it. We continue to evaluate the effectiveness of the wet-chemical "cleaning" steps used by various investigators, to enable them to design improved methods of stripping spacecraft and terrestrial contamination from surfaces while still leaving the solar-wind signal intact.
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Pego, A M F; Roveri, F L; Kuninari, R Y; Leyton, V; Miziara, I D; Yonamine, M
2017-05-01
Hair testing is a recognized approach when it comes to accessing historical drug use. According to the World Drug Report of United Nations Office on Drugs and Crime (UNODC) 2015, Brazil is the largest cocaine (COC) market in South America. New analytical methodologies to detect crack/cocaine analytes in hair samples are highly desirable. Here, a method consisting of a liquid-phase microextraction (LPME) as a clean-up step, followed by gas chromatography-mass spectrometry (GC-MS) analysis has been proposed. The new validated method consisted of a washing step; an overnight incubation with methanol and a quick derivatization with butylchloroformate. Once derivatized, the samples were then submitted to the LPME procedure. Limits of detection (LoD) and quantitation (LoQ) obtained were of 0.1 and 0.5ng/mg for COC 0.4 and 0.5ng/mg for anhydroecgonine methyl ester (AEME); 0.03 and 0.05 for cocaethylene (CE), respectively and 0.05ng/mg for both LoD and LoQ for benzoylecgonine (BZE). All calibration curves were linear over the scope applied, from LoQ up to 20ng/mg, with a r 2 >0.99. Precision and accuracy assays showed acceptable %RSD values, according to international guidelines. Twelve postmortem head hair samples stemming from the Institute of Legal Medicine of Sao Paulo (IML-SP) have been analyzed, from which seven have shown to be positive for COC (0.75->20ng/mg) and BZE (0.1->20ng/mg). Apart from COC's main metabolite, four samples were also positive for CE (0.1-3.9ng/mg) and three samples for AEME (0.5-4.9ng/mg). To conclude, the LPME technique together with GC-MS analysis have shown promising results and were able to meet the demand of the laboratory of analyzing postmortem hair samples to look for all four analytes. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.
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Thormahlen's test; Melanin - urine ... A clean-catch urine sample is needed. ... this substance that it shows up in the urine. ... Normally, melanin is not present in urine. Normal value ranges may ... measurements or test different samples. Talk to your health ...
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Exposure Assessment in a Single-Walled Carbon Nanotube Primary Manufacturer.
Kouassi, Serge; Catto, Cyril; Ostiguy, Claude; L'Espérance, Gilles; Kroeger, Jens; Debia, Maximilien
2017-03-01
This study was aimed at documenting and characterizing occupational exposure to single-walled carbon nanotubes (SWCNTs) generated in a primary manufacturing plant. It also compared various strategies of exposure monitoring. A 6-day measurement protocol was scheduled (D1-D6) including both (i) quasi-personal monitoring with an array of direct reading instruments (DRIs) and (ii) offline electron microscopy analyses of surface and breathing zone filter-based samples. The first step (D1 and D2) consisted of contamination screenings resulting from the various SWCNT production tasks using a multimetric approach. Surface sampling was also carried out to assess workplace cross-contamination. The second step (D3-D6) focused on the exposure monitoring during recovery/cleaning task, by comparing three personal elemental carbon (EC) measurements [respirable EC using a cyclone following the NIOSH 5040 method (REC-CYC), respirable and thoracic EC using parallel particle impactors [REC-PPI and TEC-PPI, respectively)] and gravimetric mass concentration measurements. DustTrak DRX and electrical low-pressure impactor measurements indicated that particles were released during weighing, transferring, and recovery/cleaning tasks of the manufacturing process. Electron microscopy revealed the presence of agglomerated SWCNTs only during the recovery/cleaning task. REC-CYC concentrations remained under the limits of quantification; REC-PPI showed levels up to 58 µg m-3; and TEC-PPI ranged from 40 to 70 µg m-3. Ratios calculated between gravimetric measurements and estimated DustTrak mass concentrations ranged from 2.8 to 4.9. Cross-contamination appeared to be limited since SWCNTs was only found on surface samples collected close to the reactor in the production room. This case study showed that the DustTrak DRX should be the preferred device among DRIs to identify potential exposure to SWCNTs. However, there is a risk of false positive since it is a non-specific instrument; therefore, the actual release of SWCNTs must be confirmed with scanning electron microscopy/transmission electron microscopy analyses. Besides, using EC measurements as a proxy for SWCNT exposure assessments, as suggested by the NIOSH, is still challenging since interferences can occur with other EC sources such as carbon black, which is also present in the workplace. © The Author 2017. Published by Oxford University Press on behalf of the British Occupational Hygiene Society.
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Harvey, David J.; Crispin, Max; Bonomelli, Camille; Scrivens, Jim H.
2016-01-01
Graphical abstract Many samples of complex mixtures of N-glycans released from small amounts of material, such as glycoproteins from viruses, present problems for mass spectrometric analysis because of the presence of contaminating material that is difficult to remove by conventional methods without involving sample loss. This paper describes the use of ion mobility for extraction of glycan profiles from such samples and for obtaining clean CID spectra when targeted m/z values capture additional ions from those of the target compound. N-Glycans were released enzymatically from within SDS-PAGE gels, from the representative glycoprotein, gp120 of the human immunodeficiency virus, and examined by direct infusion electrospray in negative mode followed by ion mobility with a Waters Synapt G2 mass spectrometer. Clean profiles of singly, doubly and triply charged N-glycans were obtained from samples in cases where the raw electrospray spectra displayed only a few glycan ions as the result of low sample concentration or the presence of contamination. Ion mobility also enabled uncontaminated CID spectra to be obtained from glycans when their molecular ions displayed coincidence with ions from fragments or multiply charged ions with similar m/z values. This technique proved to be invaluable for removing extraneous ions from many CID spectra. The presence of such ions often produces spectra that are difficult to interpret. Most CID spectra, even those from abundant glycan constituents, benefited from such clean-up showing that the extra dimension provided by ion mobility was invaluable for studies of this type. PMID:26204966
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Using Image Pro Plus Software to Develop Particle Mapping on Genesis Solar Wind Collector Surfaces
NASA Technical Reports Server (NTRS)
Rodriquez, Melissa C.; Allton, J. H.; Burkett, P. J.
2012-01-01
The continued success of the Genesis mission science team in analyzing solar wind collector array samples is partially based on close collaboration of the JSC curation team with science team members who develop cleaning techniques and those who assess elemental cleanliness at the levels of detection. The goal of this collaboration is to develop a reservoir of solar wind collectors of known cleanliness to be available to investigators. The heart and driving force behind this effort is Genesis mission PI Don Burnett. While JSC contributes characterization, safe clean storage, and benign collector cleaning with ultrapure water (UPW) and UV ozone, Burnett has coordinated more exotic and rigorous cleaning which is contributed by science team members. He also coordinates cleanliness assessment requiring expertise and instruments not available in curation, such as XPS, TRXRF [1,2] and synchrotron TRXRF. JSC participates by optically documenting the particle distributions as cleaning steps progress. Thus, optical document supplements SEM imaging and analysis, and elemental assessment by TRXRF.
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Li, Wen-jing; Chen, Yue; Li, Nai-sheng; Li, Bin; Luo, Wu-gan
2015-03-01
ICP-AES was used to determine the elemental composition of solutions in different conservation steps for understanding the impact of cleaning agents on ceramics from Huaguangjiao I shipwreck. The results showed that high content in solution of Al, Fe, Mg ions, which can be indexes to reflect the damage in conservation of ceramics. According to these indexes, we discovered that agents of strong cleaning ability bring more damage to ceramic samples. Meanwhile, the state of preservation of the ceramics was closely related to the damage in conservation. Ceramics in an excellent state of preservation endure less damage than that in bad state. We also found that each cleaning agent cause certain degree of damage on porcelains, even neutral reagent, like deionized water. Moreover, moderate cleaning reagent, when using a long time, bring the same degree of damage as the strong acid. Therefore, in actual protection procedure, for conservation ceramics safe and effective, damage of each cleaning agents and cumulative damage should be considered.
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1984-09-01
and these accompanied the sample residue through sieving to avoid sample mix- up . B. Field data sheets required logger’s initials on each page to A...ensure data completeness. C. Metal trays were placed to catch residue spillage during residue transfer from sieves to sample bottles. D. Sample bottles...methodologies were comparable for all sample e types and consisted of four sequential components: extraction, clean- up , gas chromatographic (GC) analysis, and
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Hall, Lisa; Farrington, Alison; Mitchell, Brett G; Barnett, Adrian G; Halton, Kate; Allen, Michelle; Page, Katie; Gardner, Anne; Havers, Sally; Bailey, Emily; Dancer, Stephanie J; Riley, Thomas V; Gericke, Christian A; Paterson, David L; Graves, Nicholas
2016-03-24
The Researching Effective Approaches to Cleaning in Hospitals (REACH) study will generate evidence about the effectiveness and cost-effectiveness of a novel cleaning initiative that aims to improve the environmental cleanliness of hospitals. The initiative is an environmental cleaning bundle, with five interdependent, evidence-based components (training, technique, product, audit and communication) implemented with environmental services staff to enhance hospital cleaning practices. The REACH study will use a stepped-wedge randomised controlled design to test the study intervention, an environmental cleaning bundle, in 11 Australian hospitals. All trial hospitals will receive the intervention and act as their own control, with analysis undertaken of the change within each hospital based on data collected in the control and intervention periods. Each site will be randomised to one of the 11 intervention timings with staggered commencement dates in 2016 and an intervention period between 20 and 50 weeks. All sites complete the trial at the same time in 2017. The inclusion criteria allow for a purposive sample of both public and private hospitals that have higher-risk patient populations for healthcare-associated infections (HAIs). The primary outcome (objective one) is the monthly number of Staphylococcus aureus bacteraemias (SABs), Clostridium difficile infections (CDIs) and vancomycin resistant enterococci (VRE) infections, per 10,000 bed days. Secondary outcomes for objective one include the thoroughness of hospital cleaning assessed using fluorescent marker technology, the bio-burden of frequent touch surfaces post cleaning and changes in staff knowledge and attitudes about environmental cleaning. A cost-effectiveness analysis will determine the second key outcome (objective two): the incremental cost-effectiveness ratio from implementation of the cleaning bundle. The study uses the integrated Promoting Action on Research Implementation in Health Services (iPARIHS) framework to support the tailored implementation of the environmental cleaning bundle in each hospital. Evidence from the REACH trial will contribute to future policy and practice guidelines about hospital environmental cleaning. It will be used by healthcare leaders and clinicians to inform decision-making and implementation of best-practice infection prevention strategies to reduce HAIs in hospitals. Australia New Zealand Clinical Trial Registry ACTRN12615000325505.
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Pawar, Ajinkya M; Pawar, Mansing G; Kokate, Sharad R
2014-01-01
The vital steps in any endodontic treatment are thorough mechanical shaping and chemical cleaning followed by obtaining a fluid tight impervious seal by an inert obturating material. For the past two decades, introduction and use of rotary nickel-titanium (Ni-Ti) files have changed our concepts of endodontic treatment from conventional to contemporary. They have reported good success rates, but still have many drawbacks. The Self-Adjusting File (SAF) introduces a new era in endodontics by performing the vital steps of shaping and cleaning simultaneously. The SAF is a hollow file in design that adapts itself three-dimensionally to the root canal and is a single file system, made up of Ni-Ti lattice. The case series presented in the paper report the clinical experience, while treating primary endodontic cases with the SAF system in India.
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Putting Math Into Family Life: What's Possible for Working Parents?
ERIC Educational Resources Information Center
Kliman, Marlene; Mokros, Jan; Parkes, Alana
A set of parent-child math activities designed to help busy, working parents do math with their children as part of everyday situations such as cleaning up and making dinner included basic steps, variations, and information on working with children were developed for families with elementary grades children aged approximately 5 to 11 and…
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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.
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Ziarrusta, Haizea; Val, Nahia; Dominguez, Haizea; Mijangos, Leire; Prieto, Ailette; Usobiaga, Aresatz; Etxebarria, Nestor; Zuloaga, Olatz; Olivares, Maitane
2017-11-01
This work describes the optimization, validation, and application in real samples of accurate and precise analytical methods to determine ten fluoroquinolones (FQs) (norfloxacin, enoxacin, pefloxacin, ofloxacin, levofloxacin, ciprofloxacin, danofloxacin, lomefloxacin, enrofloxacin, and sparfloxacin) in different environmental matrices, such as water (estuarine, seawater, and wastewater treatment plant effluent), fish tissues (muscle and liver), and fish biofluids (plasma and bile). The analysis step performed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was fully optimized to improve the separation and detection steps. The extraction of analytes from fish tissues was accomplished using focused ultrasound solid-liquid extraction using methanol/acetic acid (95:5 v/v) as extractant. The preconcentration and clean-up steps were optimized in terms of extraction efficiency and cleanliness and the best strategy for each matrix was selected: (i) Oasis HLB for seawater and muscle, (ii) liquid-liquid extraction combined with Oasis HLB for the lipid-rich liver, (iii) the combination of Evolute-WAX and Oasis HLB for estuarine water and wastewater treatment plant effluent, and (iv) molecular imprinted polymers for biofluids. The methods afforded satisfactory apparent recoveries (80-126%) and repeatability (RSD < 15%), except for sparfloxacin, which showed a lack of correction with the available isotopically labeled surrogates ([ 2 H 8 ]-ciprofloxacin and [ 2 H 5 ]-enrofloxacin). Ciprofloxacin, norfloxacin, and ofloxacin were detected in both water and fish liver samples from the Biscay Coast at concentrations up to 278 ng/L and 4 ng/g, respectively. To the best of our knowledge, this work is one of the few analyzing up to ten FQs and in so many fish tissues and biofluids. Graphical abstract Determination of fluoroquinolones in different environmental matrices, such as water (estuarine, seawater, and wastewater treatment plant effluent), fish tissues (muscle and liver), and fish biofluids (plasma and bile).
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Microbial diversity in European and South American spacecraft assembly clean rooms
NASA Astrophysics Data System (ADS)
Moissl-Eichinger, Christine; Stieglmeier, Michaela; Schwendner, Petra
Spacecraft assembly clean rooms are unique environments for microbes: Due to low nutri-ent levels, desiccated, clean conditions, constant control of humidity and temperature, these environments are quite inhospitable to microbial life and even considered "extreme". Many procedures keep the contamination as low as possible, but these conditions are also highly se-lective for indigenous microbial communities. For space missions under planetary protection requirements, it is crucial to control the contaminating bioburden as much as possible; but for the development of novel cleaning/sterilization methods it is also important to identify and characterize (understand) the present microbial community of spacecraft clean rooms. In prepa-ration for the recently approved ESA ExoMars mission, two European and one South American spacecraft assembly clean rooms were analyzed with respect to their microbial diversity, using standard procedures, new cultivation approaches and molecular methods, that should shed light onto the presence of planetary protection relevant microorganisms. For this study, the Her-schel Space Observatory (launched in May 2009) and its housing clean rooms in Friedrichshafen (Germany), at ESTEC (The Netherlands) and CSG, Kourou (French Guyana) were sampled during assembly, test and launch operations. Although Herschel does not demand planetary protection requirements, all clean rooms were in a fully operating state during sampling. This gave us the opportunity to sample the microbial diversity under strict particulate and molecular contamination-control. Samples were collected from spacecraft and selected clean room surface areas and were subjected to cultivation assays (32 different media), molecular studies (based on 16S rRNA gene sequence analysis) and quantitative PCR. The results from different strategies will be compared and critically discussed, showing the advantages and limits of the selected methodologies. This talk will sum up the lessons learned from this microbial diversity project.
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Precise Th/U-dating of small and heavily coated samples of deep sea corals
NASA Astrophysics Data System (ADS)
Lomitschka, Michael; Mangini, Augusto
1999-07-01
Marine carbonate skeletons like deep-sea corals are frequently coated with iron and manganese oxides/hydroxides which adsorb additional thorium and uranium out of the sea water. A new cleaning procedure has been developed to reduce this contamination. In this further cleaning step a solution of Na 2EDTA (Na 2H 2T B) and ascorbic acid is used which composition is optimised especially for samples of 20 mg of weight. It was first tested on aliquots of a reef-building coral which had been artificially contaminated with powdered ferromanganese nodule. Applied on heavily contaminated deep-sea corals (scleractinia), it reduced excess 230Th by another order of magnitude in addition to usual cleaning procedures. The measurement of at least three fractions of different contamination, together with an additional standard correction for contaminated carbonates results in Th/U-ages corrected for the authigenic component. A good agreement between Th/U- and 14C-ages can be achieved even for extremely coated corals.
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Piešťanský, Juraj; Maráková, Katarína; Kovaľ, Marián; Havránek, Emil; Mikuš, Peter
2015-12-01
A new multidimensional analytical approach for the ultra-trace determination of target chiral compounds in unpretreated complex real samples was developed in this work. The proposed analytical system provided high orthogonality due to on-line combination of three different methods (separation mechanisms), i.e. (1) isotachophoresis (ITP), (2) chiral capillary zone electrophoresis (chiral CZE), and (3) triple quadrupole mass spectrometry (QqQ MS). The ITP step, performed in a large bore capillary (800 μm), was utilized for the effective sample pretreatment (preconcentration and matrix clean-up) in a large injection volume (1-10 μL) enabling to obtain as low as ca. 80 pg/mL limits of detection for the target enantiomers in urine matrices. In the chiral CZE step, the different chiral selectors (neutral, ionizable, and permanently charged cyclodextrins) and buffer systems were tested in terms of enantioselectivity and influence on the MS detection response. The performance parameters of the optimized ITP - chiral CZE-QqQ MS method were evaluated according to the FDA guidance for bioanalytical method validation. Successful validation and application (enantioselective monitoring of renally eliminated pheniramine and its metabolite in human urine) highlighted great potential of this chiral approach in advanced enantioselective biomedical applications. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Measuring quality indicators in the operating room: cleaning and turnover time.
Jericó, Marli de Carvalho; Perroca, Márcia Galan; da Penha, Vivian Colombo
2011-01-01
This exploratory-descriptive study was carried out in the Surgical Center Unit of a university hospital aiming to measure time spent with concurrent cleaning performed by the cleaning service and turnover time and also investigated potential associations between cleaning time and the surgery's magnitude and specialty, period of the day and the room's size. The sample consisted of 101 surgeries, computing cleaning time and 60 surgeries, computing turnover time. The Kaplan-Meier method was used to analyze time and Pearson's correlation to study potential correlations. The time spent in concurrent cleaning was 7.1 minutes and turnover time was 35.6 minutes. No association between cleaning time and the other variables was found. These findings can support nurses in the efficient use of resources thereby speeding up the work process in the operating room.
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Chuang, Jane C; Emon, Jeanette M Van; Durnford, Joyce; Thomas, Kent
2005-09-15
An enzyme-linked immunosorbent assay (ELISA) method was developed to quantitatively measure 2,4-dichlorophenoxyacetic acid (2,4-D) in human urine. Samples were diluted (1:5) with phosphate-buffered saline containing 0.05% Tween and 0.02% sodium azide, with analysis by a 96-microwell plate immunoassay format. No clean up was required as dilution step minimized sample interferences. Fifty urine samples were received without identifiers from a subset of pesticide applicators and their spouses in an EPA pesticide exposure study (PES) and analyzed by the ELISA method and a conventional gas chromatography/mass spectrometry (GC/MS) procedure. For the GC/MS analysis, urine samples were extracted with acidic dichloromethane (DCM); methylated by diazomethane and fractionated by a Florisil solid phase extraction (SPE) column prior to GC/MS detection. The percent relative standard deviation (%R.S.D.) of the 96-microwell plate triplicate assays ranged from 1.2 to 22% for the urine samples. Day-to-day variation of the assay results was within +/-20%. Quantitative recoveries (>70%) of 2,4-D were obtained for the spiked urine samples by the ELISA method. Quantitative recoveries (>80%) of 2,4-D were also obtained for these samples by the GC/MS procedure. The overall method precision of these samples was within +/-20% for both the ELISA and GC/MS methods. The estimated quantification limit for 2,4-D in urine was 30ng/mL by ELISA and 0.2ng/mL by GC/MS. A higher quantification limit for the ELISA method is partly due to the requirement of a 1:5 dilution to remove the urine sample matrix effect. The GC/MS method can accommodate a 10:1 concentration factor (10mL of urine converted into 1mL organic solvent for analysis) but requires extraction, methylation and clean up on a solid phase column. The immunoassay and GC/MS data were highly correlated, with a correlation coefficient of 0.94 and a slope of 1.00. Favorable results between the two methods were achieved despite the vast differences in sample preparation. Results indicated that the ELISA method could be used as a high throughput, quantitative monitoring tool for human urine samples to identify individuals with exposure to 2,4-D above the typical background levels.
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Vera-Candioti, Luciana; Culzoni, María J; Olivieri, Alejandro C; Goicoechea, Héctor C
2008-11-01
Drug monitoring in serum samples was performed using second-order data generated by CE-DAD, processed with a suitable chemometric strategy. Carbamazepine could be accurately quantitated in the presence of its main metabolite (carbamazepine epoxide), other therapeutic drugs (lamotrigine, phenobarbital, phenytoin, phenylephrine, ibuprofen, acetaminophen, theophylline, caffeine, acetyl salicylic acid), and additional serum endogenous components. The analytical strategy consisted of the following steps: (i) serum sample clean-up to remove matrix interferences, (ii) data pre-processing, in order to reduce the background and to correct for electrophoretic time shifts, and (iii) resolution of fully overlapped CE peaks (corresponding to carbamazepine, its metabolite, lamotrigine and unexpected serum components) by the well-known multivariate curve resolution-alternating least squares algorithm, which extracts quantitative information that can be uniquely ascribed to the analyte of interest. The analyte concentration in serum samples ranged from 2.00 to 8.00 mg/L. Mean recoveries were 102.6% (s=7.7) for binary samples, and 94.8% (s=13.5) for spiked serum samples, while CV (%)=4.0 was computed for five replicate, indicative of the acceptable accuracy and precision of the proposed method.
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Śramska, Paula; Maciejka, Artur; Topolewska, Anna; Stepnowski, Piotr; Haliński, Łukasz P
2017-02-01
Tropane alkaloids are toxic secondary metabolites produced by Solanaceae plants. Among them, plants from Datura genus produce significant amounts of scopolamine and hyoscyamine; the latter undergoes racemization to atropine during isolation. Because of their biological importance, toxic properties and commonly reported food and animal feed contamination by different Datura sp. organs, there is a constant need for reliable methods for the analysis of tropane alkaloids in many matrices. In the current study, three extraction and sample-clean up procedures for the determination of scopolamine and atropine in plant material were compared in terms of their effectiveness and repeatability. Standard liquid-liquid extraction (LLE) and EXtrelut ® NT 3 columns were used for the sample clean-up. Combined ultrasound-assisted extraction and 24h static extraction using ethyl acetate, followed by multiple LLE steps was found the most effective separation method among tested. However, absolute extraction recovery was relatively low and reached 45-67% for atropine and 52-73% for scopolamine, depending on the compound concentration. The same method was also the most effective one for the isolation of target compounds from Datura stramonium leaves. EXtrelut ® columns, on the other hand, displayed relatively low effectiveness in isolating atropine and scopolamine from such a complex matrix and hence could not be recommended. The most effective method was also applied to the extraction of alkaloids from roots and stems of D. stramonium. Quantitative analyses were performed using validated method based on gas chromatography with flame ionization detector (GC-FID). Based on the results, the importance of the proper selection of internal standards in the analysis of tropane alkaloids was stressed out. Copyright © 2016 Elsevier B.V. All rights reserved.
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Interaction of abiotic and microbial processes in hexachloroethane reduction in groundwater
Roberts, A. Lynn; Gschwend, Philip M.
1994-01-01
In order to gain insight into mechanisms of hexachloroethane reduction, hexa- and pentachloroethane transformation rates were measured in anaerobic groundwater samples. For samples spiked with pentachloroethane, disappearance of pentachloroethane was accompanied by tetrachloroethylene production. Transformation rates were similar in unpoisoned and in HgCl2-poisoned samples, and rates were within ±20% of predictions based on measured pH and second-order dehydrochlorination rate constants determined in clean laboratory systems, indicating that the fate of pentachloroethane in this system is dominated by abiotic reactions. No hexachloroethane transformation was observed in HgCl2-poisoned samples, whereas in unpoisoned samples, hexachloroethane disappearance was accompanied by production of tetrachloroethylene as well as traces of pentachloroethane. Although only minor amounts of pentachloroethane accumulated, as much as 30% of the hexachloroethane transformation pathway proceeds via a pentachloroethane intermediate. This suggests that the microbial reduction of hexachloroethane proceeds at least in part through a free-radical mechanism. To the extent that hexachloroethane reduction to tetrachloroethylene occurs through a pentachloroethane intermediate, the first step in the sequence, the microbially-mediated step, is the slow step; the subsequent abiotic dehydrohalogenation step occurs much more rapidly.
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Zhou, Caihong; Tong, Shanshan; Chang, Yunxia; Jia, Qiong; Zhou, Weihong
2012-04-01
Ionic liquid (IL) based dispersive liquid-liquid microextraction (DLLME) with back-extraction coupled with capillary electrophoresis ultraviolet detection was developed to determine four phenolic compounds (bisphenol-A, β-naphthol, α-naphthol, 2, 4-dichlorophenol) in aqueous cosmetics. The developed method was used to preconcentrate and clean up the four phenolic compounds including two steps. The analytes were transferred into room temperature ionic liquid (1-octyl-3-methylimidazolium hexafluorophosphate, [C(8) MIM][PF(6) ]) rich-phase in the first step. In the second step, the analytes were back-extracted into the alkaline aqueous phase. The effects of extraction parameters, such as type and volume of extraction solvent, type and volume of disperser, extraction and centrifugal time, sample pH, salt addition, and concentration and volume of NaOH in back-extraction were investigated. Under the optimal experimental conditions, the preconcentration factors were 60.1 for bisphenol-A, 52.7 for β-naphthol, 49.2 for α-naphthol, and 18.0 for 2, 4-dichlorophenol. The limits of detection for bisphenol-A, β-naphthol, α-naphthol and 2, 4-dichlorophenol were 5, 5, 8, and 100 ng mL(-1), respectively. Four kinds of aqueous cosmetics including toner, soften lotion, make-up remover, and perfume were analyzed and yielded recoveries ranging from 81.6% to 119.4%. The main advantages of the proposed method are quick, easy, cheap, and effective. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Jiang, Yanfeng; Mehedi, Md Al; Fu, Engang; Wang, Yongqiang; Allard, Lawrence F.; Wang, Jian-Ping
2016-01-01
Rare-earth-free magnets are highly demanded by clean and renewable energy industries because of the supply constraints and environmental issues. A promising permanent magnet should possess high remanent magnetic flux density (Br), large coercivity (Hc) and hence large maximum magnetic energy product ((BH)max). Fe16N2 has been emerging as one of promising candidates because of the redundancy of Fe and N on the earth, its large magnetocrystalline anisotropy (Ku > 1.0 × 107 erg/cc), and large saturation magnetization (4πMs > 2.4 T). However, there is no report on the formation of Fe16N2 magnet with high Br and large Hc in bulk format before. In this paper, we successfully synthesize free-standing Fe16N2 foils with a coercivity of up to 1910 Oe and a magnetic energy product of up to 20 MGOe at room temperature. Nitrogen ion implantation is used as an alternative nitriding approach with the benefit of tunable implantation energy and fluence. An integrated synthesis technique is developed, including a direct foil-substrate bonding step, an ion implantation step and a two-step post-annealing process. With the tunable capability of the ion implantation fluence and energy, a microstructure with grain size 25–30 nm is constructed on the FeN foil sample with the implantation fluence of 5 × 1017/cm2. PMID:27145983
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Jiang, Yanfeng; Mehedi, Md Al; Fu, Engang; Wang, Yongqiang; Allard, Lawrence F; Wang, Jian-Ping
2016-05-05
Rare-earth-free magnets are highly demanded by clean and renewable energy industries because of the supply constraints and environmental issues. A promising permanent magnet should possess high remanent magnetic flux density (Br), large coercivity (Hc) and hence large maximum magnetic energy product ((BH)max). Fe16N2 has been emerging as one of promising candidates because of the redundancy of Fe and N on the earth, its large magnetocrystalline anisotropy (Ku > 1.0 × 10(7) erg/cc), and large saturation magnetization (4πMs > 2.4 T). However, there is no report on the formation of Fe16N2 magnet with high Br and large Hc in bulk format before. In this paper, we successfully synthesize free-standing Fe16N2 foils with a coercivity of up to 1910 Oe and a magnetic energy product of up to 20 MGOe at room temperature. Nitrogen ion implantation is used as an alternative nitriding approach with the benefit of tunable implantation energy and fluence. An integrated synthesis technique is developed, including a direct foil-substrate bonding step, an ion implantation step and a two-step post-annealing process. With the tunable capability of the ion implantation fluence and energy, a microstructure with grain size 25-30 nm is constructed on the FeN foil sample with the implantation fluence of 5 × 10(17)/cm(2).
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Clean Up Your Image: A Beginner's Guide to Scanning and Photoshop
ERIC Educational Resources Information Center
Stitzer, Michael S.
2005-01-01
In this article, the author addresses the key steps of scanning and illustrates the process with screen shots taken from a Macintosh G4 Powerbook computer running OSX and Adobe Photoshop 7.0. After reviewing scanning procedures, the author describes how to use Photoshop 7.0 to manipulate a scanned image. This activity gives students a good general…
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Kania-Korwel, Izabela; Zhao, Hongxia; Norstrom, Karin; Li, Xueshu; Hornbuckle, Keri C.; Lehmler, Hans-Joachim
2008-01-01
A pressurized liquid extraction-based method for the simultaneous extraction and in situ clean-up of polychlorinated biphenyls (PCBs), hydroxylated (OH)-PCBs and methylsulfonyl (MeSO2)-PCBs from small (< 0.5 gram) tissue samples was developed and validated. Extraction of a laboratory reference material with hexane:dichloromethane:methanol (48:43:9, v/v) and Florisil as fat retainer allowed an efficient recovery of PCBs (78–112%; RSD: 13–37%), OH-PCBs (46±2%; RSD: 4%) and MeSO2-PCBs (89±21%; RSD: 24%). Comparable results were obtained with an established analysis method for PCBs, OH-PCBs and MeSO2-PCBs. PMID:19019378
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Magnetically suspended stepping motors for clean room and vacuum environments
NASA Technical Reports Server (NTRS)
Higuchi, Toshiro
1994-01-01
To answer the growing needs for super-clean or contact free actuators for uses in clean rooms, vacuum chambers, and space, innovative actuators which combine the functions of stepping motors and magnetic bearings in one body were developed. The rotor of the magnetically suspended stepping motor is suspended like a magnetic bearing and rotated and positioned like a stepping motor. The important trait of the motor is that it is not a simple mixture or combination of a stepping motor and conventional magnetic bearing, but an amalgam of a stepping motor and a magnetic bearing. Owing to optimal design and feed-back control, a toothed stator and rotor are all that are needed structurewise for stable suspension. More than ten types of motors such as linear type, high accuracy rotary type, two-dimensional type, and high vacuum type were built and tested. This paper describes the structure and design of these motors and their performance for such applications as precise positioning rotary table, linear conveyor system, and theta-zeta positioner for clean room and high vacuum use.
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Feddern, Vivian; Aroeira, Carolina Naves; Molognoni, Luciano; Gressler, Vanessa; Daguer, Heitor; Dalla Costa, Osmar Antonio; Castillo, Carmen Josefina Contreras; de Lima, Gustavo Julio Mello Monteiro
2018-05-23
Ractopamine has been allowed by some countries as a repartitioning additive in pig diet, since it promotes protein synthesis and fat lipolysis. Most regulatory agencies only propose the ractopamine assessment in meat, kidney, liver and fat. Aiming at contributing to the scarcity data regarding this analyte in pig lungs, we extended the scope of a LC-MS method to evaluate pig offals. Homogenized tissue samples were extracted by a QuEChERS procedure; following by clean up steps and further tandem mass spectrometry determination. Method performance was evaluated through specificity, recovery, linearity, reproducibility, repeatability, decision limit (CC α ), and detection capability (CC β ), in accordance to the Commission Decision 2002/657/EC. Regression coefficients (R 2 ) between 0.994 and 0.999 were achieved for kidney, liver and lungs. Recoveries ranged from 92.0 to 127%. CC α and CC β values ranged from 3.65 to 4.86 μg kg -1 , and from 6.27 to 7.21 μg kg -1 , respectively. These values were under the maximum residue limits suggested by Codex Alimentarius, which are 90 and 40 μg kg -1 for kidney and liver, respectively. When applied to real samples up to 22.5, 92 and 1003 μg kg -1 of ractopamine residues were detected in pig liver, kidney and lungs, respectively. The results allowed concluding that the proposed analytical method is capable to detect ractopamine residues in all evaluated matrices. Therefore, it can be successfully applied and used as a routine method in laboratories of residue analysis. Copyright © 2018. Published by Elsevier B.V.
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The Relationship of the Silicon Surface Roughness and Gate Oxide Integrity in NH4OH/H2O2 Mixtures
NASA Astrophysics Data System (ADS)
Meuris, M.; Verhaverbeke, S.; Mertens, P. W.; Heyns, M. M.; Hellemans, L.; Bruynseraede, Y.; Philipossian, A.
1992-11-01
In this study some recent findings on the cleaning action of the NH4OH/H2O2 (SC1) step in a pre-gate oxidation cleaning (RCA cleaning) are given. An important parameter in this mixture is the NH4OH/H2O2 ratio. The Fe contamination on the silicon surface after this cleaning step is found to increase upon decreasing the NH4OH/H2O2 ratio. This can be attributed to the incorporation of Fe in the chemical oxide, grown by the hydrogen peroxide. The particle removal efficiency of the cleaning step is found to decrease upon decreasing the NH4OH/H2O2 ratio. On the other hand, using a lower NH4OH concentration results in a less severe silicon surface roughening. It is demonstrated in this study that the NH4OH/H2O2 ratio during the SC1 step of the cleaning is the determining parameter for the breakdown properties of a gate oxide. A (0.25/1/5) NH4OH/H2O2/H2O mixture at 75°C in our experimental conditions is suggested to be the best compromise between particle removal and surface roughness during the SC1 step.
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Ueda, T; Shibata, H; Nakamura, H; Takubo, T; Kubota, Y; Oguma, S; Tani, Y; Masaoka, T; Nagao, T; Takeo, H; Hasegawa, H; Moriyama, Y
1983-01-01
The clinical effectiveness of bioclean rooms was studied in relation to prevention of infection during treatment for induction of remission of acute leukemia. According to the steps in clean patient care, patients were divided into three groups, Group A consisting of 106 patients who were accommodated in laminar air flow (LAF) rooms under strictly clean nursing, Group B consisting of 99 patients who were treated in disinfected rooms with LAF without any clean nursing techniques and Group C consisting of 188 patients who stayed in conventional wards. Since all patients were treated with antileukemic drugs and preventive administration of antimicrobial drugs under the same regimen, any difference between groups should be attributable to LAF or LAF and clean nursing. A marked and stepwise reduction in the incidence of infection between Groups A, B and C was observed. A statistically significant reduction in pneumonia, upper respiratory tract infection, periproctitis and skin abscesses was also observed in Groups A and B. As to the causative organisms, a relative increase in incidence of infections caused by Pseudomonas aeruginosa and Escherichia coli and a decrease in those caused by Proteus and fungi were observed in Groups A and B, as compared with Group C. These data suggest that pneumonia etc. may be exogenous infections and that Proteus and fungi are exogenous organisms, while Pseudomonas aeruginosa and Escherichia coli are endogenous bacteria. These data seem very helpful for setting up several steps in bioclean rooms for effective and economic patient care.
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A Method of Visualizing Three-Dimensional Distribution of Yeast in Bread Dough
NASA Astrophysics Data System (ADS)
Maeda, Tatsurou; Do, Gab-Soo; Sugiyama, Junichi; Oguchi, Kosei; Shiraga, Seizaburou; Ueda, Mitsuyoshi; Takeya, Koji; Endo, Shigeru
A novel technique was developed to monitor the change in three-dimensional (3D) distribution of yeast in frozen bread dough samples in accordance with the progress of mixing process. Application of a surface engineering technology allowed the identification of yeast in bread dough by bonding EGFP (Enhanced Green Fluorescent Protein) to the surface of yeast cells. The fluorescent yeast (a biomarker) was recognized as bright spots at the wavelength of 520 nm. A Micro-Slicer Image Processing System (MSIPS) with a fluorescence microscope was utilized to acquire cross-sectional images of frozen dough samples sliced at intervals of 1 μm. A set of successive two-dimensional images was reconstructed to analyze 3D distribution of yeast. Samples were taken from each of four normal mixing stages (i.e., pick up, clean up, development, and final stages) and also from over mixing stage. In the pick up stage yeast distribution was uneven with local areas of dense yeast. As the mixing progressed from clean up to final stages, the yeast became more evenly distributed throughout the dough sample. However, the uniformity in yeast distribution was lost in the over mixing stage possibly due to the breakdown of gluten structure within the dough sample.
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Anomaly detection for machine learning redshifts applied to SDSS galaxies
NASA Astrophysics Data System (ADS)
Hoyle, Ben; Rau, Markus Michael; Paech, Kerstin; Bonnett, Christopher; Seitz, Stella; Weller, Jochen
2015-10-01
We present an analysis of anomaly detection for machine learning redshift estimation. Anomaly detection allows the removal of poor training examples, which can adversely influence redshift estimates. Anomalous training examples may be photometric galaxies with incorrect spectroscopic redshifts, or galaxies with one or more poorly measured photometric quantity. We select 2.5 million `clean' SDSS DR12 galaxies with reliable spectroscopic redshifts, and 6730 `anomalous' galaxies with spectroscopic redshift measurements which are flagged as unreliable. We contaminate the clean base galaxy sample with galaxies with unreliable redshifts and attempt to recover the contaminating galaxies using the Elliptical Envelope technique. We then train four machine learning architectures for redshift analysis on both the contaminated sample and on the preprocessed `anomaly-removed' sample and measure redshift statistics on a clean validation sample generated without any preprocessing. We find an improvement on all measured statistics of up to 80 per cent when training on the anomaly removed sample as compared with training on the contaminated sample for each of the machine learning routines explored. We further describe a method to estimate the contamination fraction of a base data sample.
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Arias, Jean Lucas de Oliveira; Rombaldi, Caroline; Caldas, Sergiane Souza; Primel, Ednei Gilberto
2014-09-19
The clean-up step is essential to reduce interferences, improve quantification and help to maintain the integrity of the chromatographic system when working with complex matrices. In this study, alternative materials were evaluated as sorbents in the dispersive solid-phase extraction (D-SPE) for the determination and extraction of seventeen pesticides from rice paddy soil samples by the quick, easy, cheap, effective, rugged and safe (QuEChERS) method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Chitin, chitosan, diatomaceous earth and PSA were compared in terms of extraction efficiency and matrix effect. The best results were achieved when chitosan was used. Quantification limits ranged from 0.1 to 100μgkg(-1). Calibration curves showed correlation coefficient values higher than 0.98. Results of accuracy and precision in the spiked soil samples between 60% and 120%, with a relative standard deviation lower than 20%, were reached for 15 out of 17 pesticides. The matrix effect was evaluated and only one compound was influenced by the matrix components, showing medium effect. Results showed that alternative materials are more effective and less expensive than traditional sorbents which have been usually employed, i.e., they may be used in the D-SPE step during the extraction of pesticides from rice paddy soils. Copyright © 2014 Elsevier B.V. All rights reserved.
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Determination of acrylamide in coffee and coffee products by GC-MS using an improved SPE clean-up.
Soares, C; Cunha, S; Fernandes, J
2006-12-01
An improved gas chromatography-mass spectrometry (GC-MS) method to determine acrylamide (AA) in coffee and coffee products was developed. The method was based on two main purification steps: the first with ethanol and Carrez solutions in order to precipitate polysaccharides and proteins, respectively; and the second with a layered solid-phase extraction (SPE) column which proved to be efficient in the elimination of the main chromatographic interferences. The method is applicable to a wide range of coffee products. Twenty-six samples of different coffee products were analysed. The levels of AA were in the range 11.4-36.2 microg l-1 for 'espresso coffee' and 200.8-229.4 microg l-1 for coffee blends with cereals. The results indicate that the presence of cereals significantly increased the levels of AA.
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COMPENDIUM OF METHODS FOR THE DETERMINATION ...
This Second Edition of the Compendium has been prepared to provide regional, state and local environmental regulatory agencies with step-by-step sampling and analysis procedures for the determination of selected toxic organic pollutants in ambient air. It is designed to assist those persons responsible for sampling and analysis of toxic organic pollutants in complying with the requirements of Title III of the Clean Air Act. This revised Compendium presents a set of 17 methods in a standardized format with a variety of applicable sampling methods, as well as several analytical techniques, for specific classes of organic pollutants, as appropriate to the specific pollutant compound, its level, and potential interferences. Consequently, this treatment allows the user flexibility in selecting alternatives to complement his or her background and laboratory capability. Information
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Frégeau, Chantal J; Lett, C Marc; Elliott, Jim; Yensen, Craig; Fourney, Ron M
2008-05-01
An automated process has been developed for the analysis of forensic casework samples using TECAN Genesis RSP 150/8 or Freedom EVO liquid handling workstations equipped exclusively with nondisposable tips. Robot tip cleaning routines have been incorporated strategically within the DNA extraction process as well as at the end of each session. Alternative options were examined for cleaning the tips and different strategies were employed to verify cross-contamination. A 2% sodium hypochlorite wash (1/5th dilution of the 10.8% commercial bleach stock) proved to be the best overall approach for preventing cross-contamination of samples processed using our automated protocol. The bleach wash steps do not adversely impact the short tandem repeat (STR) profiles developed from DNA extracted robotically and allow for major cost savings through the implementation of fixed tips. We have demonstrated that robotic workstations equipped with fixed pipette tips can be used with confidence with properly designed tip washing routines to process casework samples using an adapted magnetic bead extraction protocol.
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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.
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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
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Gilbert-López, Bienvenida; García-Reyes, Juan F; Lozano, Ana; Fernández-Alba, Amadeo R; Molina-Díaz, Antonio
2010-09-24
In this work we have evaluated the performance of two sample preparation methodologies for the large-scale multiresidue analysis of pesticides in olives using liquid chromatography-electrospray tandem mass spectrometry (LC-MS/MS). The tested sample treatment methodologies were: (1) liquid-liquid partitioning with acetonitrile followed by dispersive solid-phase extraction clean-up using GCB, PSA and C18 sorbents (QuEChERS method - modified for fatty vegetables) and (2) matrix solid-phase dispersion (MSPD) using aminopropyl as sorbent material and a final clean-up performed in the elution step using Florisil. An LC-MS/MS method covering 104 multiclass pesticides was developed to examine the performance of these two protocols. The separation of the compounds from the olive extracts was achieved using a short C18 column (50 mm x 4.6 mm i.d.) with 1.8 microm particle size. The identification and confirmation of the compounds was based on retention time matching along with the presence (and ratio) of two typical MRM transitions. Limits of detection obtained were lower than 10 microgkg(-1) for 89% analytes using both sample treatment protocols. Recoveries studies performed on olives samples spiked at two concentration levels (10 and 100 microgkg(-1)) yielded average recoveries in the range 70-120% for most analytes when QuEChERS procedure is employed. When MSPD was the choice for sample extraction, recoveries obtained were in the range 50-70% for most of target compounds. The proposed methods were successfully applied to the analysis of real olives samples, revealing the presence of some of the target species in the microgkg(-1) range. Besides the evaluation of the sample preparation approaches, we also discuss the use of advanced software features associated to MRM method development that overcome several limitations and drawbacks associated to MS/MS methods (time segments boundaries, tedious method development/manual scheduling and acquisition limitations). This software feature recently offered by different vendors is based on an algorithm that associates retention time data for each individual MS/MS transition, so that the number of simultaneously traced transitions throughout the entire chromatographic run (dwell times and sensitivity) is maximized. Copyright 2010 Elsevier B.V. All rights reserved.
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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.
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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.
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Humus-assisted cleaning of heavy metal contaminated soils
NASA Astrophysics Data System (ADS)
Borggaard, Ole K.; Rasmussen, Signe B.
2016-04-01
Contamination of soils with non-degradable heavy metals (HMs) because of human acticities is globally a serious problem threatening human health and ecosystem functioning. To avoid negative effects, HMs must be removed either on-site by plant uptake (phytoremediation) or off-site by extraction (soil washing). In both strategies, HM solubility must be augmented by means of a strong ligand (complexant). Often polycarboxylates such as EDTA and NTA are used but these ligands are toxic, synthetic (non-natural) and may promote HM leaching. Instead naturally occurring soluble humic substances (HS) were tested as means for cleaning HM contaminated soils; HS samples from beech and spruce litter, compost percolate and processed cow slurry were tested. Various long-term HM contaminated soils were extracted with solutions of EDTA, NTA or HS at different pH by single-step and multiple-step extraction mode. The results showed that each of the three complexant types increased HM solubility but the pH-dependent HM extraction efficiency decreased in the order: EDTA ≈ NTA > HS. However, the naturally occurring HS seems suitable for cleaning As, Cd, Cu and Zn contaminated soils both in relation to phytoremediation of moderately contaminated soils and washing of strongly contaminated soils. On the other hand, HS was found unsuited as cleaning agent for Pb polluted calcareous soils. If future field experiments confirm these laboratory results, we have a new cheap and environmentally friendly method for solving a great pollution problem, i.e. cleaning of heavy metal contaminated soils. In addition, humic substances possess additional benefits such as improving soil structure and stimulating microbial activity.
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Going clean: structure and dynamics of peptides in the gas phase and paths to solvation.
Baldauf, Carsten; Rossi, Mariana
2015-12-16
The gas phase is an artificial environment for biomolecules that has gained much attention both experimentally and theoretically due to its unique characteristic of providing a clean room environment for the comparison between theory and experiment. In this review we give an overview mainly on first-principles simulations of isolated peptides and the initial steps of their interactions with ions and solvent molecules: a bottom up approach to the complexity of biological environments. We focus on the accuracy of different methods to explore the conformational space, the connections between theory and experiment regarding collision cross section evaluations and (anharmonic) vibrational spectra, and the challenges faced in this field.
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Vega, Victor A; Young, Michelle; Todd, Sarah
2016-01-01
An extraction for aflatoxin M1 from bovine milk samples is described. The samples were extracted by adding 10 mL acetonitrile to 10 g of sample. The extract was salted out with sodium chloride and magnesium sulfate to separate the water and acetonitrile. The organic layer was dried down and reconstituted in water before being subjected to an immunoaffinity column for cleanup. Once the analyte was isolated, quantitation was obtained by LC with fluorescence detection. LC/fluorescence parameters were optimized with an Agilent Poroshell 120 C18 LC column resulting in a 4 min run time. To test the procedure's robustness, three different kinds of matrixes were fortified at three different levels each. Whole milk, reduced fat milk, and skim milk samples were fortified at approximately 0.25, 0.5, and 1.0 μg/kg. Recoveries from all samples ranged from 70 to 100%. Confirmation was accomplished by injecting the samples in an ion trap mass spectrometer. The method presented here entails an extraction step followed by an immunoaffinity column clean-up that leads to fast analysis time and consistent recoveries with an uncertainty measurement of 10.5% and method detection limit of less than 0.011 μg/kg.
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Haidar Ahmad, Imad A; Tam, James; Li, Xue; Duffield, William; Tarara, Thomas; Blasko, Andrei
2017-02-05
The parameters affecting the recovery of pharmaceutical residues from the surface of stainless steel coupons for quantitative cleaning verification method development have been studied, including active pharmaceutical ingredient (API) level, spiking procedure, API/excipient ratio, analyst-to-analyst variability, inter-day variability, and cleaning procedure of the coupons. The lack of a well-defined procedure that consistently cleaned coupon surface was identified as the major contributor to low and variable recoveries. Assessment of acid, base, and oxidant washes, as well as the order of treatment, showed that a base-water-acid-water-oxidizer-water wash procedure resulted in consistent, accurate spiked recovery (>90%) and reproducible results (S rel ≤4%). By applying this cleaning procedure to the previously used coupons that failed the cleaning acceptance criteria, multiple analysts were able to obtain consistent recoveries from day-to-day for different APIs, and API/excipient ratios at various spike levels. We successfully applied our approach for cleaning verification of small molecules (MW<1000Da) as well as large biomolecules (MW up to 50,000Da). Method robustness was greatly influenced by the sample preparation procedure, especially for analyses using total organic carbon (TOC) determination. Copyright © 2016 Elsevier B.V. All rights reserved.
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Code of Federal Regulations, 2012 CFR
2012-07-01
... to conveniently divert the SO2 from the sampling manifold to provide clean zero air at the output manifold for zero adjustment. The system may be made up using common laboratory components, or it may be a... Reference Material (SRM). 4.1.6.2Clean zero air, free of contaminants that could cause a detectable response...
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Code of Federal Regulations, 2010 CFR
2010-07-01
... to conveniently divert the SO2 from the sampling manifold to provide clean zero air at the output manifold for zero adjustment. The system may be made up using common laboratory components, or it may be a... Reference Material (SRM). 4.1.6.2Clean zero air, free of contaminants that could cause a detectable response...
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Code of Federal Regulations, 2011 CFR
2011-07-01
... to conveniently divert the SO2 from the sampling manifold to provide clean zero air at the output manifold for zero adjustment. The system may be made up using common laboratory components, or it may be a... Reference Material (SRM). 4.1.6.2Clean zero air, free of contaminants that could cause a detectable response...
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Code of Federal Regulations, 2013 CFR
2013-07-01
... to conveniently divert the SO2 from the sampling manifold to provide clean zero air at the output manifold for zero adjustment. The system may be made up using common laboratory components, or it may be a... Reference Material (SRM). 4.1.6.2Clean zero air, free of contaminants that could cause a detectable response...
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Alternative Fuels Data Center: Phoenix Cleans Up with Natural Gas
Phoenix Cleans Up with Natural Gas to someone by E-mail Share Alternative Fuels Data Center : Phoenix Cleans Up with Natural Gas on Facebook Tweet about Alternative Fuels Data Center: Phoenix Cleans Up with Natural Gas on Twitter Bookmark Alternative Fuels Data Center: Phoenix Cleans Up with Natural
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Parirokh, Masoud; Asgary, Saeed; Eghbal, Mohammad Jafar
2005-08-01
This study was carried out to investigate metallic and non-metallic debris remaining on endodontic files after ultrasonic cleaning and autoclave processing. Forty-eight unused rotary and hand endodontic files, including eight different brands, were tested. Instruments were cleaned with ultrasound, autoclaved and before and after each step were observed by scanning electron microscopy (SEM). Adherent debris was analysed by energy-dispersive X-ray analysis (EDXA). All of the instruments before ultrasound cleaning were contaminated with metallic and non-metallic debris. Although most non-metallic debris was removed by ultrasonic cleaning, most of the metallic debris remained even after the final step of sterilization.
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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.
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Míguez-Framil, Martha; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Pilar; Alvarez-Freire, Iván; Tabernero, María Jesús; Bermejo, Ana María
2010-10-08
A simple and fast sample pre-treatment method based on matrix solid-phase dispersion (MSPD) for isolating cocaine, benzoylecgonine (BZE), codeine, morphine and 6-monoacethylmorphine (6-MAM) from human hair has been developed. The MSPD approach consisted of using alumina (1.80 g) as a dispersing agent and 0.6M hydrochloric acid (4 mL) as an extracting solvent. For a fixed hair sample mass of 0.050 g, the alumina mass to sample mass ratio obtained was 36. A previously conditioned Oasis HLB cartridge (2 mL methanol, plus 2 mL ultrapure water, plus 1 mL of 0.2M/0.2M sodium hydroxide/boric acid buffer solution at pH 9.2) was attached to the end of the MSPD syringe for on column clean-up of the hydrochloric acid extract and for transferring the target compounds to a suitable solvent for gas chromatography (GC) analysis. Therefore, the adsorbed analytes were directly eluted from the Oasis HLB cartridges with 2 mL of 2% acetic acid in methanol before concentration by N(2) stream evaporation and dry extract derivatization with N-methyl-tert-butylsilyltrifluoroacetamide (BSTFA) and chlorotrimethylsilane (TMCS). The optimization/evaluation of all the factors affecting the MSPD and on column clean-up procedures has led to a fast sample treatment, and analytes extraction and pre-concentration can be finished in approximately 30 min. The developed method has been applied to eight hair samples from poli-drug abusers and measured analyte concentrations have been found to be statistically similar (95% confidence interval) to those obtained after a conventional enzymatic hydrolysis method (Pronase E). Copyright © 2010. Published by Elsevier B.V.
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Cantú, Ricardo; Shoemaker, Jody A; Kelty, Catherine A; Wymer, Larry J; Behymer, Thomas D; Dufour, Alfred P; Magnuson, Matthew L
2017-08-22
The use of cyanuric acid as a biomarker for ingestion of swimming pool water may lead to quantitative knowledge of the volume of water ingested during swimming, contributing to a better understanding of disease resulting from ingestion of environmental contaminants. When swimming pool water containing chlorinated cyanurates is inadvertently ingested, cyanuric acid is excreted quantitatively within 24 h as a urinary biomarker of ingestion. Because the volume of water ingested can be quantitatively estimated by calculation from the concentration of cyanuric acid in 24 h urine samples, a procedure for preservation, cleanup, and analysis of cyanuric acid was developed to meet the logistical demands of large scale studies. From a practical stand point, urine collected from swimmers cannot be analyzed immediately, given requirements of sample collection, shipping, handling, etc. Thus, to maintain quality control to allow confidence in the results, it is necessary to preserve the samples in a manner that ensures as quantitative analysis as possible. The preservation and clean-up of cyanuric acid in urine is complicated because typical approaches often are incompatible with the keto-enol tautomerization of cyanuric acid, interfering with cyanuric acid sample preparation, chromatography, and detection. Therefore, this paper presents a novel integration of sample preservation, clean-up, chromatography, and detection to determine cyanuric acid in 24 h urine samples. Fortification of urine with cyanuric acid (0.3-3.0 mg/L) demonstrated accuracy (86-93% recovery) and high reproducibility (RSD < 7%). Holding time studies in unpreserved urine suggested sufficient cyanuric acid stability for sample collection procedures, while longer holding times suggested instability of the unpreserved urine. Preserved urine exhibited a loss of around 0.5% after 22 days at refrigerated storage conditions of 4 °C. Published by Elsevier B.V.
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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.
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Osorio-Tobón, J Felipe; Carvalho, Pedro I N; Barbero, Gerardo Fernández; Nogueira, Gislaine Chrystina; Rostagno, Mauricio Ariel; Meireles, Maria Angela de Almeida
2016-06-01
The recent development of fused-core technology in HPLC columns is enabling faster and highly efficient separations. This technology was evaluated for the development of a fast method for the analysis of main curcuminoids (curcumin, demethoxycurcumin and bisdemethoxycurcumin) present in extracts of turmeric (Curcuma longa L.). A step-by-step strategy was used to optimize temperature (40-55 °C), flow rate (1.0-2.5 mL min(-1)), mobile phase composition and equilibration time (1-5 min). A gradient method was developed using acidified water and acetonitrile combined with high column temperature (55 °C) and flow rate (2.5 mL min(-1)). Optimized conditions provided a method for the separation of these three curcuminoids in approximately 1.3 min with a total analysis time (sample-to-sample) of 7 min, including the clean-up and the re-equilibration of the column. Evaluation of chromatographic performance revealed excellent intraday and interday reproducibility (>99%), resolution (>2.23), selectivity (>1.12), peak symmetry (1.24-1.42) while presenting low limits of detection (<0.40 mg L(-1)) and quantification (<1.34 mg L(-1)). The robustness of the method was calculated according to the concentration/dilution of the sample and the injection volume. Several combinations of methanol and ethanol with water as sample solvents were evaluated and the best chromatographic results and extraction rate were obtained using 100% methanol. Finally, the developed method was validated with different extracts of turmeric rhizome and products that use turmeric in their formulation. Copyright © 2016 Elsevier Ltd. All rights reserved.
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NASA Astrophysics Data System (ADS)
Nichols, Leannah M.
Commercially pure titanium can take up to six months to successfully manufacture a six-inch in diameter ingot in which can be shipped to be melted and shaped into other useful components. The applications to the corrosion-resistant, light weight, strong metal are endless, yet so is the manufacturing processing time. At a cost of around $80 per pound of certain grades of titanium powder, the everyday consumer cannot afford to use titanium in the many ways it is beneficial simply because the number of processing steps it takes to manufacture consumes too much time, energy, and labor. In this research, the steps it takes from the raw powder form to the final part are proposed to be reduced from 4-8 steps to only 2 steps utilizing a new technology that may even improve upon the titanium properties at the same time as it is reducing the number of steps of manufacture. The two-step procedure involves selecting a cylindrical or rectangular die and punch to compress a small amount of commercially pure titanium to a strong-enough compact for transportation to the friction stir welder to be consolidated. Friction stir welding invented in 1991 in the United Kingdom uses a tool, similar to a drill bit, to approach a sample and gradually plunge into the material at a certain rotation rate of between 100 to 2,100 RPM. In the second step, the friction stir welder is used to process the titanium powder held in a tight holder to consolidate into a harder titanium form. The resulting samples are cut to expose the cross section and then grinded, polished, and cleaned to be observed and tested using scanning electron microscopy (SEM), electron dispersive spectroscopy (EDS), and a Vickers microhardness tester. The results were that the thicker the sample, the harder the resulting consolidated sample peaking at 2 to 3 times harder than that of the original commercially pure titanium in solid form at a peak value of 435.9 hardness and overall average of 251.13 hardness. The combined results of the SEM and EDS have shown that the mixing of the sample holder material, titanium, and tool material were not of a large amount and therefore proves the feasibility of this study. This study should be continued to lessen the labor, energy, and cost of the production of titanium to therefore allow titanium to be improved upon and be more efficient for many applications across many industries.
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2-in-1 shampoo technology: state-of-the-art shampoo and conditioner in one.
Rushton, H; Gummer, C L; Flasch, H
1994-01-01
Consumers have expressed a need for cleaning and conditioning in one step. Conventional shampoo technology using anionic surfactants and cationic conditioners results in charge interaction and complexing of the ingredients. Neither shampoo nor conditioners achieves the desired result. The successful solution was to incorporate charge neutral dimethicone conditioning ingredients, suspended as microfine droplets within complex crystal lattices, into anionic surfactant shampoo technology. The same solution has also been applied to amphoteric surfactant systems. This provides complete cleaning, and hair conditioning fully equal to separate conditioners without the problems of sebum interactions and conditioner build-up. This was achieved by keeping the dimethicone in suspension throughout the shampoo process. During rinsing, excess water breaks the crystalline lattice and allows deposition of the dimethicone droplets onto the hair. Full cleaning and conditioning are, therefore, achieved in one application. Dimethicone build-up is not encountered as subsequent washes first remove soil and previously deposited dimethicone. Neither do neutral dimethicones show any reactions with sebum. The development of effective 2-in-1 technology has had a major impact on shampoo technology and consumer habits and practices. This has significantly changed the way consumers care for their hair.
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Unidentified Organic Compounds. For target analytes, standards are purchased, extraction and clean-up procedures are optimized, and mass spectra and retention times for the chromatographic separation are obtained for comparison to the target compounds in environmental sample ... -
Martins, Nuno; Carreiro, Elisabete P; Locati, Abel; Ramalho, João P Prates; Cabrita, Maria João; Burke, Anthony J; Garcia, Raquel
2015-08-28
This work firstly addresses the design and development of molecularly imprinted systems selective for deltamethrin aiming to provide a suitable sorbent for solid phase (SPE) extraction that will be further used for the implementation of an analytical methodology for the trace analysis of the target pesticide in spiked olive oil samples. To achieve this goal, a preliminary evaluation of the molecular recognition and selectivity of the molecularly imprinted polymers has been performed. In order to investigate the complexity of the mechanistic basis for template selective recognition in these polymeric matrices, the use of a quantum chemical approach has been attempted providing new insights about the mechanisms underlying template recognition, and in particular the crucial role of the crosslinker agent and the solvent used. Thus, DFT calculations corroborate the results obtained by experimental molecular recognition assays enabling one to select the most suitable imprinting system for MISPE extraction technique which encompasses acrylamide as functional monomer and ethylene glycol dimethacrylate as crosslinker. Furthermore, an analytical methodology comprising a sample preparation step based on solid phase extraction has been implemented using this "tailor made" imprinting system as sorbent, for the selective isolation/pre-concentration of deltamethrin from olive oil samples. Molecularly imprinted solid phase extraction (MISPE) methodology was successfully applied for the clean-up of spiked olive oil samples, with recovery rates up to 94%. Copyright © 2015 Elsevier B.V. All rights reserved.
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Noser, Jürg; Schneider, Patrick; Rother, Martin; Schmutz, Hansruedi
2011-11-01
An ultra performance liquid chromatography (UPLC)-tandem mass spectrometry (MS/MS) method was developed for the determination of the Alternaria toxins tenuazonic acid, alternariol, alternariol monomethyl ether, altenuene, altertoxin I and tentoxin. Owing to its instability, altenusin could not be determined. The sample preparation includes an acidic acetonitrile/water/methanol extraction, followed by SPE clean-up step, before injection into the UPLC-MS/MS system. The separation was made on an Acquity UPLC column using a water/acetonitrile gradient with ammonium hydrogen carbonate as a modifier. Matrix compounds of real samples led to enhancement as well as suppression of the target compounds, depending on analyte and matrix. The recoveries were between 58 and 109% at a level of 10 μg/kg. Eighty-five tomato products, consisting of peeled and minced tomatoes, soup and sauces, tomato purées and concentrates, ketchup as well as dried and fresh tomatoes, were taken from the Swiss market in 2010. Tenuazonic acid was found most frequently (81 out of 85 samples) and in the highest levels of up to 790 μg/kg. Alternariol and alternariol monomethyl ether were found in lower concentrations, ranging from <1 to 33 μg/kg for alternariol and <5 to 9 μg/kg for alternariol monomethyl ether. Only a few samples were positive for altenuene and tentoxin. Altertoxin I was never detected.
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Natural occurrence of ochratoxin A contamination in commercial black and white pepper products.
Jalili, M; Jinap, S; Radu, S
2010-10-01
The concentration of ochratoxin A (OTA) in 120 commercial pepper (84 pre-packed and 36 bulk samples), which consist of local and imported white and black pepper in powder and seed form in Malaysia were determined. The objective of the study was to investigate and compare OTA concentration in black pepper and white pepper being commercialized in Malaysia. Determination method was based on HPLC with fluorescence detection coupled with immunoaffinity column clean-up step. Mobile phase consisted of acetonitrile-water-acetic acid (49.5:49.5:1.0, v/v/v), and flow rate was 1 ml/min. The LOD was 0.02 ng/g, and the average recovery values of OTA ranged from 79.5 to 92.0% in black pepper and 81.2-90.3% in white pepper. A total of 57 samples (47.5%) were contaminated with OTA ranging from 0.15 to 13.58 ng/g. The results showed that there was a significant difference between type of pepper and brands. OTA concentration in black pepper was significantly higher than white pepper (p < 0.05). The highest concentration of ochratoxin, 13.58 ng/g, was detected in a sample of black pepper seed followed by 12.64 ng/g in a sample of black pepper powder, both were bulk samples purchased from open market.
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Is peracetic acid suitable for the cleaning step of reprocessing flexible endoscopes?
Kampf, Günter; Fliss, Patricia M; Martiny, Heike
2014-09-16
The bioburden (blood, protein, pathogens and biofilm) on flexible endoscopes after use is often high and its removal is essential to allow effective disinfection, especially in the case of peracetic acid-based disinfectants, which are easily inactivated by organic material. Cleaning processes using conventional cleaners remove a variable but often sufficient amount of the bioburden. Some formulations based on peracetic acid are recommended by manufacturers for the cleaning step. We performed a systematic literature search and reviewed the available evidence to clarify the suitability of peracetic acid-based formulations for cleaning flexible endoscopes. A total of 243 studies were evaluated. No studies have yet demonstrated that peracetic acid-based cleaners are as effective as conventional cleaners. Some peracetic acid-based formulations have demonstrated some biofilm-cleaning effects and no biofilm-fixation potential, while others have a limited cleaning effect and a clear biofilm-fixation potential. All published data demonstrated a limited blood cleaning effect and a substantial blood and nerve tissue fixation potential of peracetic acid. No evidence-based guidelines on reprocessing flexible endoscopes currently recommend using cleaners containing peracetic acid, but some guidelines clearly recommend not using them because of their fixation potential. Evidence from some outbreaks, especially those involving highly multidrug-resistant gram-negative pathogens, indicated that disinfection using peracetic acid may be insufficient if the preceding cleaning step is not performed adequately. Based on this review we conclude that peracetic acid-based formulations should not be used for cleaning flexible endoscopes.
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Is peracetic acid suitable for the cleaning step of reprocessing flexible endoscopes?
Kampf, Günter; Fliss, Patricia M; Martiny, Heike
2014-01-01
The bioburden (blood, protein, pathogens and biofilm) on flexible endoscopes after use is often high and its removal is essential to allow effective disinfection, especially in the case of peracetic acid-based disinfectants, which are easily inactivated by organic material. Cleaning processes using conventional cleaners remove a variable but often sufficient amount of the bioburden. Some formulations based on peracetic acid are recommended by manufacturers for the cleaning step. We performed a systematic literature search and reviewed the available evidence to clarify the suitability of peracetic acid-based formulations for cleaning flexible endoscopes. A total of 243 studies were evaluated. No studies have yet demonstrated that peracetic acid-based cleaners are as effective as conventional cleaners. Some peracetic acid-based formulations have demonstrated some biofilm-cleaning effects and no biofilm-fixation potential, while others have a limited cleaning effect and a clear biofilm-fixation potential. All published data demonstrated a limited blood cleaning effect and a substantial blood and nerve tissue fixation potential of peracetic acid. No evidence-based guidelines on reprocessing flexible endoscopes currently recommend using cleaners containing peracetic acid, but some guidelines clearly recommend not using them because of their fixation potential. Evidence from some outbreaks, especially those involving highly multidrug-resistant gram-negative pathogens, indicated that disinfection using peracetic acid may be insufficient if the preceding cleaning step is not performed adequately. Based on this review we conclude that peracetic acid-based formulations should not be used for cleaning flexible endoscopes. PMID:25228941
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Evaluation of various cleaning methods to remove bacillus spores from spacecraft hardware materials
NASA Technical Reports Server (NTRS)
Venkateswaran, Kasthuri; Chung, Shirley; Allton, Judith; Kern, Roger
2004-01-01
A detailed study was made of the biological cleaning effectiveness, defined in terms of the ability to remove bacterial spores, of a number of methods used to clean hardware surfaces. Aluminum (Al 6061) and titanium (Ti 6Al-4V) were chosen for the study as they were deemed the two materials most likely to be used in spacecraft extraterrestrial sampler construction. Metal coupons (1 cm x 2.5 cm) were precleaned and inoculated with 5.8 x 10(3) cultivable Bacillus subtilis spores, which are commonly found on spacecraft surfaces and in the assembly environments. The inoculated coupons were subsequently cleaned using: (1) 70% isopropyl alcohol wipe; (2) water wipe; (3) multiple-solvent flight-hardware cleaning procedures used at the Jet Propulsion Laboratory (JPL); (4) Johnson Space Center-developed ultrapure water rinse; and (5) a commercial, semi-aqueous, multiple-solvent (SAMS) cleaning process. The biological cleaning effectiveness was measured by agar plate assay, sterility test (growing in liquid media), and epifluorescent microscopy. None of the cleaning protocols tested completely removed viable spores from the surface of the aluminum. In contrast, titanium was capable of being cleaned to sterility by two methods, the JPL standard and the commercial SAMS cleaning process. Further investigation showed that the passivation step employed in the JPL standard method is an effective surface sterilant on both metals but not compatible with aluminum. It is recommended that titanium (Ti 6Al-4V) be considered superior to aluminum (Al 6061) for use in spacecraft sampling hardware, both for its potential to be cleaned to sterilization and for its ability to withstand the most effective cleaning protocols.
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Evaluation of Various Cleaning Methods to Remove Bacillus Spores from Spacecraft Hardware Materials
NASA Astrophysics Data System (ADS)
Venkateswaran, Kasthuri; Chung, Shirley; Allton, Judith; Kern, Roger
2004-09-01
A detailed study was made of the biological cleaning effectiveness, defined in terms of the ability to remove bacterial spores, of a number of methods used to clean hardware surfaces. Aluminum (Al 6061) and titanium (Ti 6Al-4V) were chosen for the study as they were deemed the two materials most likely to be used in spacecraft extraterrestrial sampler construction. Metal coupons (1 cm × 2.5 cm) were precleaned and inoculated with 5.8 × 103 cultivable Bacillus subtilis spores, which are commonly found on spacecraft surfaces and in the assembly environments. The inoculated coupons were subsequently cleaned using: (1) 70% isopropyl alcohol wipe; (2) water wipe; (3) multiple-solvent flight-hardware cleaning procedures used at the Jet Propulsion Laboratory (JPL); (4) Johnson Space Center-developed ultrapure water rinse; and (5) a commercial, semi-aqueous, multiple-solvent (SAMS) cleaning process. The biological cleaning effectiveness was measured by agar plate assay, sterility test (growing in liquid media), and epifluorescent microscopy. None of the cleaning protocols tested completely removed viable spores from the surface of the aluminum. In contrast, titanium was capable of being cleaned to sterility by two methods, the JPL standard and the commercial SAMS cleaning process. Further investigation showed that the passivation step employed in the JPL standard method is an effective surface sterilant on both metals but not compatible with aluminum. It is recommended that titanium (Ti 6Al-4V) be considered superior to aluminum (Al 6061) for use in spacecraft sampling hardware, both for its potential to be cleaned to sterilization and for its ability to withstand the most effective cleaning protocols.
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Evaluation of various cleaning methods to remove bacillus spores from spacecraft hardware materials.
Venkateswaran, Kasthuri; Chung, Shirley; Allton, Judith; Kern, Roger
2004-01-01
A detailed study was made of the biological cleaning effectiveness, defined in terms of the ability to remove bacterial spores, of a number of methods used to clean hardware surfaces. Aluminum (Al 6061) and titanium (Ti 6Al-4V) were chosen for the study as they were deemed the two materials most likely to be used in spacecraft extraterrestrial sampler construction. Metal coupons (1 cm x 2.5 cm) were precleaned and inoculated with 5.8 x 10(3) cultivable Bacillus subtilis spores, which are commonly found on spacecraft surfaces and in the assembly environments. The inoculated coupons were subsequently cleaned using: (1) 70% isopropyl alcohol wipe; (2) water wipe; (3) multiple-solvent flight-hardware cleaning procedures used at the Jet Propulsion Laboratory (JPL); (4) Johnson Space Center-developed ultrapure water rinse; and (5) a commercial, semi-aqueous, multiple-solvent (SAMS) cleaning process. The biological cleaning effectiveness was measured by agar plate assay, sterility test (growing in liquid media), and epifluorescent microscopy. None of the cleaning protocols tested completely removed viable spores from the surface of the aluminum. In contrast, titanium was capable of being cleaned to sterility by two methods, the JPL standard and the commercial SAMS cleaning process. Further investigation showed that the passivation step employed in the JPL standard method is an effective surface sterilant on both metals but not compatible with aluminum. It is recommended that titanium (Ti 6Al-4V) be considered superior to aluminum (Al 6061) for use in spacecraft sampling hardware, both for its potential to be cleaned to sterilization and for its ability to withstand the most effective cleaning protocols.
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ERIC Educational Resources Information Center
Walker, John
2007-01-01
There is a right way to clean a restroom. If a worker does two things wrong, repeated in 20 restrooms a day, it is fairly certain that restroom users will complain. However, what people see or smell is not the most important issue. The overriding guideline should be to clean for health first, appearance second. Minimizing…
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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.
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ERIC Educational Resources Information Center
Kravitz, Robert
2006-01-01
In the professional cleaning industry, green cleaning has been much discussed in the past few years. Usually, the information pertains to the many reasons why a green cleaning program should be started, the steps involved to get the program off the ground, and the potential benefits. However, although many facility managers and school…
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Ortelli, Didier; Edder, Patrick; Cognard, Emmanuelle; Jan, Philippe
2008-06-09
Cyanobacteria, commonly called "blue-green algae", may accumulate in surface water supplies as "blooms" and may concentrate on the surface as blue-green "scums". Some species of cyanobacteria produce toxins and are of relevance to water supplies and to microalgae dietary supplements. To ensure the safety of drinking water and blue-green algae products, analyses are the only way to determine the presence or absence of toxins. This paper shows the use of ultra performance liquid chromatography (UPLC) coupled to orthogonal acceleration time of flight (TOF) mass spectrometry for the detection and quantitation of microcystins. The method presented is very sensitive, simple, fast, robust and did not require fastidious clean-up step. Limits of detection of 0.1 microg L(-1) in water and 0.1-0.2 microg g(-1) in microalgae samples were achieved. Method performances were satisfactory and appropriate for monitoring of water and dietary supplements. The method was applied in routine to samples taken from Swiss market or buy on internet website. Among 19 samples, six showed the presence of microcystins LR and LA at harmful levels.
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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.
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Daft, J L
1990-01-01
Food samples including fatty, non-fatty, grain-based, and nongrain-based types were fortified with the following five nematocides and fumigants: 1,3-dichloropropene, 2,3-dichloropropene, 1,2-dibromo-3-chloropropane, o-dichlorobenzene, and p-dichlorobenzene. Then, depending on sample consistency and type, the samples were diluted in, or extracted with organic solvent such as isooctane. A few of the high-fat extracts were passed through Florisil to remove excess fat or endogenous interferences. Analysis of the initial or cleaned up extracts was done by gas chromatography (GC) at 90 degrees C. The dichloropropenes were determined on 20% OV-101 columns with electron-capture and Hall electroconductivity detectors. The dichlorobenzenes and 1,2-dibromo-3-chloropropane, which elute beyond 30 min on the above columns, were determined on 5%-loaded columns using the same detectors. All five analytes were recovered from these techniques. Mean analyte recovery following a direct dilution or extraction was 83%, and following the Florisil cleanup step, was 52%. In 1986, a fumigant survey of about 200 foodstuffs by using this overall technique gave no findings of the five compounds studied here.
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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.
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Tölgyesi, Ádám; Barta, Enikő; Simon, Andrea; McDonald, Thomas J; Sharma, Virender K
2017-10-25
Veterinary drugs containing synthetic anabolic steroid and nitroimidazole active agents are not allowed for their applications in livestock of the European Union (EU). This paper presents analyses of twelve selected steroids and six nitroimidazole antibiotics at low levels (1.56μg/L-4.95μg/L and 0.17μg/kg-2.14μg/kg, respectively) in body fluids and egg incurred samples. Analyses involved clean-up procedures, high performance liquid chromatography (HPLC) separation, and tandem mass spectrometric screening and confirmatory methods. Target steroids and nitroimidazoles in samples were cleaned by two independent supported liquid extraction and solid phase extraction procedures. Separation of the selected compounds was conducted on Kinetex XB C-18 HPLC column using gradient elution. The screening methods utilised supported liquid extraction that enabled fast and cost effective clean-up. The confirmatory methods were improved by extending the number of matrices and compounds, and by introducing an isotope dilution mass spectrometry for nitroimidazoles. The new methods were validated according to the recommendation of the European Union Reference Laboratories and the performance characteristics evaluated met fully the criteria. The methods were applied to incurred samples in the proficiency tests. The obtained results of Z-scores demonstrated the applicability of developed protocols of the methods to real samples. The confirmatory methods were applied to the national monitoring program and natural contamination of prednisolone could be detected in urine at low concentration in few samples. Copyright © 2017 Elsevier B.V. All rights reserved.
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Cleaning up the mess: cell corpse clearance in Caenorhabditis elegans.
Pinto, Sérgio Morgado; Hengartner, Michael Otmar
2012-12-01
Genetic and cell biology studies have led to the identification in Caenorhabditis elegans of a set of evolutionary conserved cellular mechanisms responsible for the clearance of apoptotic cells. Based on the phenotype of cell corpse clearance mutants, corpse clearance can be divided into three distinct, but linked steps: corpse recognition, corpse internalization, and corpse degradation. Work in recent years has led to a better understanding of the molecular pathways that mediate each of these steps. Here, we review recent developments in our understanding of in vivo cell corpse clearance in this simple but most elegant model organism. Copyright © 2012 Elsevier Ltd. All rights reserved.
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Focant, Jean-François; Eppe, Gauthier; Massart, Anne-Cécile; Scholl, Georges; Pirard, Catherine; De Pauw, Edwin
2006-10-13
We report on the use of a state-of-the-art method for the measurement of selected polychlorinated dibenzo-p-dioxins, polychlorinated dibenzofurans and polychlorinated biphenyls in human serum specimens. The sample preparation procedure is based on manual small size solid-phase extraction (SPE) followed by automated clean-up and fractionation using multi-sorbent liquid chromatography columns. SPE cartridges and all clean-up columns are disposable. Samples are processed in batches of 20 units, including one blank control (BC) sample and one quality control (QC) sample. The analytical measurement is performed using gas chromatography coupled to isotope dilution high-resolution mass spectrometry. The sample throughput corresponds to one series of 20 samples per day, from sample reception to data quality cross-check and reporting, once the procedure has been started and series of samples keep being produced. Four analysts are required to ensure proper performances of the procedure. The entire procedure has been validated under International Organization for Standardization (ISO) 17025 criteria and further tested over more than 1500 unknown samples during various epidemiological studies. The method is further discussed in terms of reproducibility, efficiency and long-term stability regarding the 35 target analytes. Data related to quality control and limit of quantification (LOQ) calculations are also presented and discussed.
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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.
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NASA Astrophysics Data System (ADS)
Kim, Yong-Hyun; Kim, Ki-Hyun
2015-07-01
The analysis of polycyclic aromatic hydrocarbons (PAH) in ambient air requires the tedious experimental steps of both sampling and pretreatment (e.g., extraction or clean-up). To replace pre-existing conventional methods, a simple, rapid, and novel technique was developed to measure gas-particle fractionation of PAH in ambient air based on ‘sorbent tube-thermal desorption-gas chromatograph-mass spectrometer (ST-TD-GC-MS)’. The separate collection and analysis of ambient PAHs were achieved independently by two serially connected STs. The basic quality assurance confirmed good linearity, precision, and high sensitivity to eliminate the need for complicated pretreatment procedures with the detection limit (16 PAHs: 13.1 ± 7.04 pg). The analysis of real ambient PAH samples showed a clear fractionation between gas (two-three ringed PAHs) and particulate phases (five-six ringed PAHs). In contrast, for intermediate (four ringed) PAHs (fluoranthene, pyrene, benz[a]anthracene, and chrysene), a highly systematic/gradual fractionation was established. It thus suggests a promising role of ST-TD-GC-MS as measurement system in acquiring a reliable database of airborne PAH.
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Determination of N epsilon-(carboxymethyl)lysine in foods and related systems.
Ames, Jennifer M
2008-04-01
The sensitive and specific determination of advanced glycation end products (AGEs) is of considerable interest because these compounds have been associated with pro-oxidative and proinflammatory effects in vivo. AGEs form when carbonyl compounds, such as glucose and its oxidation products, glyoxal and methylglyoxal, react with the epsilon-amino group of lysine and the guanidino group of arginine to give structures including N epsilon-(carboxymethyl)lysine (CML), N epsilon-(carboxyethyl)lysine, and hydroimidazolones. CML is frequently used as a marker for AGEs in general. It exists in both the free or peptide-bound forms. Analysis of CML involves its extraction from the food (including protein hydrolysis to release any peptide-bound adduct) and determination by immunochemical or instrumental means. Various factors must be considered at each step of the analysis. Extraction, hydrolysis, and sample clean-up are all less straight forward for food samples, compared to plasma and tissue. The immunochemical and instrumental methods all have their advantages and disadvantages, and no perfect method exists. Currently, different procedures are being used in different laboratories, and there is an urgent need to compare, improve, and validate methods.
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Liquid-Liquid Extraction of Insecticides from Juice: An Analytical Chemistry Laboratory Experiment
ERIC Educational Resources Information Center
Radford, Samantha A.; Hunter, Ronald E., Jr.; Barr, Dana Boyd; Ryan, P. Barry
2013-01-01
A laboratory experiment was developed to target analytical chemistry students and to teach them about insecticides in food, sample extraction, and cleanup. Micro concentrations (sub-microgram/mL levels) of 12 insecticides spiked into apple juice samples are extracted using liquid-liquid extraction and cleaned up using either a primary-secondary…
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ERIC Educational Resources Information Center
North Carolina State Dept. of Community Colleges, Raleigh.
INSTRUCTIONS FOR CLEANING EVERY PART OF THE HOUSE ARE GIVEN IN OUTLINE FORM WITH PICTURES TO ILLUSTRATE PROCEDURES. FOR EACH JOB A LIST OF SUPPLIES NEEDED, STEP-BY-STEP INSTRUCTIONS, AND SPECIAL TIPS ARE GIVEN. A PLAN FOR KEEPING A CLEAN HOUSE INCLUDES LISTS OF JOBS TO BE DONE DAILY, WEEKLY, AND MONTHLY. THE SECTION ON HOME SAFETY INCLUDES…
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A Miniature Wastewater Cleaning Plant to Demonstrate Primary Treatment in the Classroom
ERIC Educational Resources Information Center
Ne´el, Bastien; Cardoso, Catia; Perret, Didier; Bakker, Eric
2015-01-01
A small-scale wastewater cleaning plant is described that includes the key physical pretreatment steps followed by the chemical treatment of mud by flocculation. Water, clay particles, and riverside deposits mimicked odorless wastewater. After a demonstration of the optimization step, the flocculation process was carried out with iron(III)…
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Ahmed, Trifa M; Lim, Hwanmi; Bergvall, Christoffer; Westerholm, Roger
2013-10-01
A multidimensional, on-line coupled liquid chromatographic/gas chromatographic system was developed for the quantification of polycyclic aromatic hydrocarbons (PAHs). A two-dimensional liquid chromatographic system (2D-liquid chromatography (LC)), with three columns having different selectivities, was connected on-line to a two-dimensional gas chromatographic system (2D-gas chromatography (GC)). Samples were cleaned up by combining normal elution and column back-flush of the LC columns to selectively remove matrix constituents and isolate well-defined, PAH enriched fractions. Using this system, the sequential removal of polar, mono/diaromatic, olefinic and alkane compounds from crude extracts was achieved. The LC/GC coupling was performed using a fused silica transfer line into a programmable temperature vaporizer (PTV) GC injector. Using the PTV in the solvent vent mode, excess solvent was removed and the enriched PAH sample extract was injected into the GC. The 2D-GC setup consisted of two capillary columns with different stationary phase selectivities. Heart-cutting of selected PAH compounds in the first GC column (first dimension) and transfer of these to the second GC column (second dimension) increased the baseline resolutions of closely eluting PAHs. The on-line system was validated using the standard reference materials SRM 1649a (urban dust) and SRM 1975 (diesel particulate extract). The PAH concentrations measured were comparable to the certified values and the fully automated LC/GC system performed the clean-up, separation and detection of PAHs in 16 extracts in less than 24 h. The multidimensional, on-line 2D-LC/2D-GC system eliminated manual handling of the sample extracts and minimised the risk of sample loss and contamination, while increasing accuracy and precision.
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Document image cleanup and binarization
NASA Astrophysics Data System (ADS)
Wu, Victor; Manmatha, Raghaven
1998-04-01
Image binarization is a difficult task for documents with text over textured or shaded backgrounds, poor contrast, and/or considerable noise. Current optical character recognition (OCR) and document analysis technology do not handle such documents well. We have developed a simple yet effective algorithm for document image clean-up and binarization. The algorithm consists of two basic steps. In the first step, the input image is smoothed using a low-pass filter. The smoothing operation enhances the text relative to any background texture. This is because background texture normally has higher frequency than text does. The smoothing operation also removes speckle noise. In the second step, the intensity histogram of the smoothed image is computed and a threshold automatically selected as follows. For black text, the first peak of the histogram corresponds to text. Thresholding the image at the value of the valley between the first and second peaks of the histogram binarizes the image well. In order to reliably identify the valley, the histogram is smoothed by a low-pass filter before the threshold is computed. The algorithm has been applied to some 50 images from a wide variety of source: digitized video frames, photos, newspapers, advertisements in magazines or sales flyers, personal checks, etc. There are 21820 characters and 4406 words in these images. 91 percent of the characters and 86 percent of the words are successfully cleaned up and binarized. A commercial OCR was applied to the binarized text when it consisted of fonts which were OCR recognizable. The recognition rate was 84 percent for the characters and 77 percent for the words.
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NASA Astrophysics Data System (ADS)
Kohlscheen, J.; Emirov, Y. N.; Beerbom, M. M.; Wolan, J. T.; Saddow, S. E.; Chung, G.; MacMillan, M. F.; Schlaf, R.
2003-09-01
The band lineup of p- and n-type 4H-SiC/Al interfaces was determined using x-ray photoemission spectroscopy (XPS). Al was deposited in situ on ex situ cleaned SiC substrates in several steps starting at 1.2 Å up to 238 Å nominal film thickness. Before growth and after each growth step, the sample surface was characterized in situ by XPS. The analysis of the spectral shifts indicated that during the initial deposition stages the Al films react with the ambient surface contamination layer present on the samples after insertion into vacuum. At higher coverage metallic Al clusters are formed. The band lineups were determined from the analysis of the core level peak shifts and the positions of the valence bands maxima (VBM) depending on the Al overlayer thickness. Shifts of the Si 2p and C 1s XPS core levels occurred to higher (lower) binding energy for the p-(n-)type substrates, which was attributed to the occurrence of band bending due to Fermi-level equilibration at the interface. The hole injection barrier at the p-type interface was determined to be 1.83±0.1 eV, while the n-type interface revealed an electron injection barrier of 0.98±0.1 eV. Due to the weak features in the SiC valence bands measured by XPS, the VBM positions were determined using the Si 2p peak positions. This procedure required the determination of the Si 2p-to-VBM binding energy difference (99.34 eV), which was obtained from additional measurements.
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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).
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Dawidowicz, Andrzej L; Czapczyńska, Natalia B; Wianowska, Dorota
2013-02-01
Sea Sand Disruption Method (SSDM) is a simple and cheap sample-preparation procedure allowing the reduction of organic solvent consumption, exclusion of sample component degradation, improvement of extraction efficiency and selectivity, and elimination of additional sample clean-up and pre-concentration step before chromatographic analysis. This article deals with the possibility of SSDM application for the differentiation of essential-oils components occurring in the Scots pine (Pinus sylvestris L.) and cypress (Cupressus sempervirens L.) needles from Madrid (Spain), Laganas (Zakhyntos, Greece), Cala Morell (Menorca, Spain), Lublin (Poland), Helsinki (Finland), and Oradea (Romania). The SSDM results are related to the analogous - obtained applying two other sample preparation methods - steam distillation and Pressurized Liquid Extraction (PLE). The results presented established that the total amount and the composition of essential-oil components revealed by SSDM are equivalent or higher than those obtained by one of the most effective extraction technique, PLE. Moreover, SSDM seems to provide the most representative profile of all essential-oil components as no heat is applied. Thus, this environmentally friendly method is suggested to be used as the main extraction procedure for the differentiation of essential-oil components in conifers for scientific and industrial purposes. Copyright © 2013 Verlag Helvetica Chimica Acta AG, Zürich.
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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.
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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.
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Improved interface and electrical properties of atomic layer deposited Al2O3/4H-SiC
NASA Astrophysics Data System (ADS)
Suvanam, Sethu Saveda; Usman, Muhammed; Martin, David; Yazdi, Milad. G.; Linnarsson, Margareta; Tempez, Agnès; Götelid, Mats; Hallén, Anders
2018-03-01
In this paper we demonstrate a process optimization of atomic layer deposited Al2O3 on 4H-SiC resulting in an improved interface and electrical properties. For this purpose the samples have been treated with two pre deposition surface cleaning processes, namely CP1 and CP2. The former is a typical surface cleaning procedure used in SiC processing while the latter have an additional weak RCA1 cleaning step. In addition to the cleaning and deposition, the effects of post dielectric annealing (PDA) at various temperatures in N2O ambient have been investigated. Analyses by scanning electron microscopy show the presence of structural defects on the Al2O3 surface after annealing at 500 and 800 °C. These defects disappear after annealing at 1100 °C, possibly due to densification of the Al2O3 film. Interface analyses have been performed using X-ray photoelectron spectroscopy (XPS) and time-of-flight medium energy ion scattering (ToF MEIS). Both these measurements show the formation of an interfacial SiOx (0 < x < 2) layer for both the CP1 and CP2, displaying an increased thickness for higher temperatures. Furthermore, the quality of the sub-oxide interfacial layer was found to depend on the pre deposition cleaning. In conclusion, an improved interface with better electrical properties is shown for the CP2 sample annealed at 1100 °C, resulting in lower oxide charges, strongly reduced flatband voltage and leakage current, as well as higher breakdown voltage.
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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.
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Alternative Fuels Data Center: Virginia Cleans up With Natural Gas Refuse
Trucks Virginia Cleans up With Natural Gas Refuse Trucks to someone by E-mail Share Alternative Fuels Data Center: Virginia Cleans up With Natural Gas Refuse Trucks on Facebook Tweet about Alternative Fuels Data Center: Virginia Cleans up With Natural Gas Refuse Trucks on Twitter Bookmark Alternative
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ERIC Educational Resources Information Center
Hugo, John C.
1992-01-01
Presents an activity in which students investigate the formation of solid ammonium chloride aerosol particles to help students better understand the concept of acid rain. Provides activity objectives, procedures, sample data, clean-up instructions, and questions and answers to help interpret the data. (MDH)
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DEMONSTRATION OF AUTONOMOUS AIR MONITORING THROUGH ROBOTICS
Hazardous and/or tedious functions are often performed by on-site workers during investigation, mitigation and clean-up of hazardous substances. These functions include site surveys, sampling and analysis, excavation, and treatment and preparation of wastes for shipment to chemic...
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NASA Astrophysics Data System (ADS)
Lucas, G.; Lénárt, C.; Solymosi, J.
2015-08-01
This paper introduces research done on the automatic preparation of remediation plans and navigation data for the precise guidance of heavy machinery in clean-up work after an industrial disaster. The input test data consists of a pollution extent shapefile derived from the processing of hyperspectral aerial survey data from the Kolontár red mud disaster. Three algorithms were developed and the respective scripts were written in Python. The first model aims at drawing a parcel clean-up plan. The model tests four different parcel orientations (0, 90, 45 and 135 degree) and keeps the plan where clean-up parcels are less numerous considering it is an optimal spatial configuration. The second model drifts the clean-up parcel of a work plan both vertically and horizontally following a grid pattern with sampling distance of a fifth of a parcel width and keep the most optimal drifted version; here also with the belief to reduce the final number of parcel features. The last model aims at drawing a navigation line in the middle of each clean-up parcel. The models work efficiently and achieve automatic optimized plan generation (parcels and navigation lines). Applying the first model we demonstrated that depending on the size and geometry of the features of the contaminated area layer, the number of clean-up parcels generated by the model varies in a range of 4% to 38% from plan to plan. Such a significant variation with the resulting feature numbers shows that the optimal orientation identification can result in saving work, time and money in remediation. The various tests demonstrated that the model gains efficiency when 1/ the individual features of contaminated area present a significant orientation with their geometry (features are long), 2/ the size of pollution extent features becomes closer to the size of the parcels (scale effect). The second model shows only 1% difference with the variation of feature number; so this last is less interesting for planning optimization applications. Last model rather simply fulfils the task it was designed for by drawing navigation lines.
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Dey, Tania; Naughton, Daragh
2017-05-01
Glass surface cleaning is the very first step in advanced coating deposition and it also finds use in conserving museum objects. However, most of the wet chemical methods of glass cleaning use toxic and corrosive chemicals like concentrated sulfuric acid (H 2 SO 4 ), piranha (a mixture of concentrated sulfuric acid and 30% hydrogen peroxide), and hydrogen fluoride (HF). On the other hand, most of the dry cleaning techniques like UV-ozone, plasma, and laser treatment require costly instruments. In this report, five eco-friendly wet chemical methods of glass cleaning were evaluated in terms of contact angle (measured by optical tensiometer), nano-scale surface roughness (measured by atomic force microscopy or AFM), and elemental composition (measured by energy dispersive x-ray spectroscopy or SEM-EDX). These glass cleaning methods are devoid of harsh chemicals and costly equipment, hence can be applied in situ in close proximity with plantation such as greenhouse or upon subtle objects such as museum artifacts. Out of these five methods, three methods are based on the chemical principle of chelation. It was found that the citric acid cleaning method gave the greatest change in contact angle within the hydrophilic regime (14.25° for new glass) indicating effective cleansing and the least surface roughness (0.178 nm for new glass) indicating no corrosive effect. One of the glass sample showed unique features which were traced backed to the history of the glass usage.
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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.
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Vicario, Ana; Aragón, Leslie; Wang, Chien C; Bertolino, Franco; Gomez, María R
2018-02-05
In this work, a novel molecularly imprinted polymer (MIP) proposed as solid phase extraction sorbent was developed for the determination of propylparaben (PP) in diverse cosmetic samples. The use of parabens (PAs) is authorized by regulatory agencies as microbiological preservative; however, recently several studies claim that large-scale use of these preservatives can be a potential health risk and harmful to the environment. Diverse factors that influence on polymer synthesis were studied, including template, functional monomer, porogen and crosslinker used. Morphological characterization of the MIP was performed using SEM and BET analysis. Parameters affecting the molecularly imprinted solid phase extraction (MISPE) and elution efficiency of PP were evaluated. After sample clean-up, the analyte was analyzed by high performance liquid chromatography (HPLC). The whole procedure was validated, showing satisfactory analytical parameters. After applying the MISPE methodology, the extraction recoveries were always better than 86.15%; the obtained precision expressed as RSD% was always lower than 2.19 for the corrected peak areas. Good linear relationship was obtained within the range 8-500ngmL -1 of PP, r 2 =0.99985. Lower limits of detection and quantification after MISPE procedure of 2.4 and 8ngmL -1 , respectively were reached, in comparison with previously reported methodologies. The development of MISPE-HPLC methodology provided a simple an economic way for accomplishing a clean-up/preconcentration step and the subsequent determination of PP in a complex matrix. The performance of the proposed method was compared against C-18 and silica solid phase extraction (SPE) cartridges. The recovery factors obtained after applying extraction methods were 96.6, 64.8 and 0.79 for MISPE, C18-SPE and silica-SPE procedures, respectively. The proposed methodology improves the retention capability of SPE material plus robustness and possibility of reutilization, enabling it to be used for PP routine monitoring in diverse personal care products (PCP) and environmental samples. Copyright © 2017 Elsevier B.V. All rights reserved.
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Bugovsky, Stefan; Winkler, Wolfgang; Balika, Werner; Koranda, Manfred; Allmaier, Günter
2016-07-15
The ideal MALDI/LDI mass spectrometry sample target for an axial TOF instrument possesses a variety of properties. Primarily, it should be chemically inert to the sample, i.e. analyte, matrix and solvents, highly planar across the whole target, without any previous chemical contact and provide a uniform surface to facilitate reproducible measurements without artifacts from previous sample or matrix compounds. This can be hard to achieve with a metal target, which has to be extensively cleaned every time after use. Any cleaning step may leave residues behind, may change the surface properties due to the type of cleaning method used or even cause microscopic scratches over time hence altering matrix crystallization behavior. Alternatively, use of disposable targets avoids these problems. As each possesses the same surface they therefore have the potential to replace the conventional full metal targets so commonly employed. Furthermore, low cost single-use targets with high planarity promise an easier compliance with GLP guidelines as they alleviate the problem of low reproducibility due to inconsistent sample/matrix crystallization and changes to the target surface properties. In our tests, polymeric metal nano-coated targets were compared to a stainless steel reference. The polymeric metal nano-coated targets exhibited all the performance characteristics for a MALDI MS sample support, and even surpassed the - in our lab commonly used - reference in some aspects like limit of detection. The target exhibits all necessary features such as electrical conductivity, vacuum, laser and solvent compatibility. Copyright © 2016 Elsevier Inc. All rights reserved.
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Developing an Approach to Harvesting, Cleaning, and Analyzing Data from Twitter Using R
ERIC Educational Resources Information Center
Hill, Stephen; Scott, Rebecca
2017-01-01
Using data from social media can be of great value to businesses and other interested parties. However, harvesting data from social media networks such as Twitter, cleaning the data, and analyzing the data can be difficult. In this article, a step-by-step approach to obtaining data via the Twitter application program interface (API) is described.…
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NASA Astrophysics Data System (ADS)
Stadler, Philipp; Farnleitner, Andreas H.; Zessner, Matthias
2016-04-01
This presentation describes in-depth how a low cost micro-computer was used for substantial improvement of established measuring systems due to the construction and implementation of a purposeful complementary device for on-site sample pretreatment. A fully automated on-site device was developed and field-tested, that enables water sampling with simultaneous filtration as well as effective cleaning procedure of the devicés components. The described auto-sampler is controlled by a low-cost one-board computer and designed for sample pre-treatment, with minimal sample alteration, to meet requirements of on-site measurement devices that cannot handle coarse suspended solids within the measurement procedure or -cycle. The automated sample pretreatment was tested for over one year for rapid and on-site enzymatic activity (beta-D-glucuronidase, GLUC) determination in sediment laden stream water. The formerly used proprietary sampling set-up was assumed to lead to a significant damping of the measurement signal due to its susceptibility to clogging, debris- and bio film accumulation. Results show that the installation of the developed apparatus considerably enhanced error-free running time of connected measurement devices and increased the measurement accuracy to an up-to-now unmatched quality.
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Beloglazova, N V; Goryacheva, I Yu; Rusanova, T Yu; Yurasov, N A; Galve, R; Marco, M-P; De Saeger, S
2010-07-05
A new rapid method which allows simultaneous one step detection of two analytes of different nature (2,4,6,-trichlorophenol (TCP) and ochratoxin A (OTA)) in red wine was developed. It was based on a column test with three separate immunolayers: two test layers and one control layer. Each layer consisted of sepharose gel with immobilized anti-OTA (OTA test layer), anti-TCP (TCP test layer) or anti-HRP (control layer) antibodies. Analytes bind to the antibodies in the corresponding test layer while sample flows through the column. Then a mixture of OTA-HRP and TCP-HRP in appropriate dilutions was used, followed by the application of chromogenic substrate. Colour development of the test layer occurred when the corresponding analyte was absent in the sample. HRP-conjugates bound to anti-HRP antibody in the control layer independently of presence or absence of analytes and a blue colour developed in the control layer. Cut-off values for both analytes were 2 microg L(-1). The described method was applied to the simultaneous detection of TCP and OTA in wine samples. To screen the analytes in red wine samples, clean-up columns were used for sample pre-treatment in combination with the test column. Results were confirmed by chromatographic methods. Copyright 2010 Elsevier B.V. All rights reserved.
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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.
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DOE Office of Scientific and Technical Information (OSTI.GOV)
Wang, Hao; Guo, Zhiguang, E-mail: zguo@licp.cas.cn; State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000
Self-cleaning properties inspired by the structures and functions of some creatures are of great interest since the late 20th century. In this paper, TiO{sub 2} coatings with hierarchical rutile TiO{sub 2} flowers on fluorine-doped tin oxide substrate are fabricated through a simple one-step hydrothermal method. The flower-like coatings exhibit superhydrophilicity in air and superoleophobicity underwater with a contact angle as high as 157°, presenting good underwater self-cleaning performance. In addition, when contaminated by oleic acid, the as-prepared TiO{sub 2} coatings also exhibit excellent photocatalytic capability under ultraviolet irradiation, which demonstrated self-cleaning properties in a different way. This self-cleaning film providesmore » a good strategy for some industrial and ocean applications.« less
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Process for producing a high emittance coating and resulting article
NASA Technical Reports Server (NTRS)
Le, Huong G. (Inventor); O'Brien, Dudley L. (Inventor)
1993-01-01
Process for anodizing aluminum or its alloys to obtain a surface particularly having high infrared emittance by anodizing an aluminum or aluminum alloy substrate surface in an aqueous sulfuric acid solution at elevated temperature and by a step-wise current density procedure, followed by sealing the resulting anodized surface. In a preferred embodiment the aluminum or aluminum alloy substrate is first alkaline cleaned and then chemically brightened in an acid bath The resulting cleaned substrate is anodized in a 15% by weight sulfuric acid bath maintained at a temperature of 30.degree. C. Anodizing is carried out by a step-wise current density procedure at 19 amperes per square ft. (ASF) for 20 minutes, 15 ASF for 20 minutes and 10 ASF for 20 minutes. After anodizing the sample is sealed by immersion in water at 200.degree. F. and then air dried. The resulting coating has a high infrared emissivity of about 0.92 and a solar absorptivity of about 0.2, for a 5657 aluminum alloy, and a relatively thick anodic coating of about 1 mil.
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NASA Astrophysics Data System (ADS)
Xu, Jun; Klimchitskaya, G. L.; Mostepanenko, V. M.; Mohideen, U.
2018-03-01
It is well known that residual electrostatic forces create significant difficulties in precise measurements of the Casimir force and the wide use of Casimir-operated microdevices. We experimentally demonstrate that, with the help of Ar-ion cleaning of the surfaces, it is possible to make electrostatic effects negligibly small compared to the Casimir interaction. Our experimental setup consists of a dynamic atomic force microscope supplemented with an Ar-ion gun and argon reservoir. The residual potential difference between the Au-coated surfaces of a sphere and those of a plate was measured both before and after in situ Ar-ion cleaning. It is shown that this cleaning decreases the magnitude of the residual potential by up to an order of magnitude and makes it almost independent of the separation. The gradient of the Casimir force was measured using ordinary samples subjected to Ar-ion cleaning. The obtained results are shown to be in good agreement both with previous precision measurements using specially selected samples and with theoretical predictions of the Lifshitz theory. The conclusion is made that the suggested method of in situ Ar-ion cleaning is effective in reducing the electrostatic effects and therefore is a great resource for experiments on measuring the Casimir interaction and for Casimir-operated microdevices.
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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.
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Janiszewska-Olszowska, Joanna; Tandecka, Katarzyna; Szatkiewicz, Tomasz; Stępień, Piotr; Sporniak-Tutak, Katarzyna; Grocholewicz, Katarzyna
2015-11-18
The present study aimed at 3D analysis of adhesive remnants and enamel loss following the debonding of orthodontic molar tubes and orthodontic clean-up to assess the effectiveness and safety of One-Step Finisher and Polisher and Adhesive Residue Remover in comparison to tungsten carbide bur. Thirty human molars were bonded with chemical-cure orthodontic adhesive (Unite, 3M, USA), stored 24 h in 0.9 % saline solution, debonded and cleaned using three methods (Three groups of ten): tungsten carbide bur (Dentaurum, Pforzheim, Germany), one-step finisher and polisher (One gloss, Shofu Dental, Kyoto, Japan) and Adhesive Residue Remover (Dentaurum, Pforzheim, Germany). Direct 3D scanning in blue-light technology to the nearest 2 μm was performed before etching and after adhesive removal. Adhesive remnant height and volume as well as enamel loss depth and volume were calculated. An index of effectiveness and safety was proposed and calculated for every tool; adhesive remnant volume and duplicated enamel lost volume were divided by a sum of multiplicands. Comparisons using parametric ANOVA or nonparametric ANOVA rank Kruskal-Wallis tests were used to compare between tools for adhesive remnant height and volume, enamel loss depth and volume as well as for the proposed index. No statistically significant differences in the volume (p = 0.35) or mean height (p = 0.24) of adhesive remnants were found (ANOVA rank Kruskal-Wallis test) between the groups of teeth cleaned using different tools. Mean volume of enamel loss was 2.159 mm(3) for tungsten carbide bur, 1.366 mm(3) for Shofu One Gloss and 0.659 mm(3) for Adhesive Residue Remover - (F = 2.816, p = 0.0078). A comparison of the proposed new index between tools revealed highly statistically significant differences (p = 0.0081), supporting the best value for Adhesive Residue Remover and the worst - for tungsten carbide bur. The evaluated tools were all characterized by similar effectiveness. The most destructive tool with regards to enamel was the tungsten carbide bur, and the least was Adhesive Residue Removal.
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Comparison of extraction techniques of robenidine from poultry feed samples.
Wilga, Joanna; Wasik, Agata Kot-; Namieśnik, Jacek
2007-10-31
In this paper, effectiveness of six different commonly applied extraction techniques for the determination of robenidine in poultry feed has been compared. The sample preparation techniques included shaking, Soxhlet, Soxtec, ultrasonically assisted extraction, microwave - assisted extraction and accelerated solvent extraction. Comparison of these techniques was done with respect to the recovery extraction, temperature and time, reproducibility and solvent consumption. Every single extract was subjected to clean - up using aluminium oxide column (Pasteur pipette filled with 1g of aluminium oxide), from which robenidine was eluted with 10ml of methanol. The eluate from the clean-up column was collected in a volumetric flask, and finally it was analysed by HPLC-DAD-MS. In general, all extraction techniques were capable of isolating of robenidine from poultry feed, but the recovery obtained using modern extraction techniques was higher than that obtained using conventional techniques. In particular, accelerated solvent extraction was more superior to other techniques, which highlights the advantages of this sample preparation technique. However, in routine analysis, shaking and ultrasonically assisted extraction is still the preferred method for the solution of robenidine and other coccidiostatics.
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Vidal, Juan C; Bonel, Laura; Ezquerra, Alba; Duato, Patricia; Castillo, Juan R
2012-06-01
We report a direct competitive immunosensor for the rapid determination of ochratoxin A (OTA) in wine samples. Magnetic beads (1 ± 0.5 μm diameter) covered with streptavidin were functionalized with a monoclonal antibody against OTA, and then left to incubate in a solution of tracer (ochratoxin conjugated to the enzyme peroxidase) and a range of OTA concentrations (10(-4) to 1,000 ng mL(-1)). After washing and separation steps helped with a magnetic field, a volume of the dispersion was put on screen-printed electrodes under a magnet, and after adding the substrate the p-benzoquinone generated enzymatically was detected by differential-pulse voltammetry. Wine samples (2 mL) were easily prepared simply by adjusting to pH = 7.5 with diluted NaOH and by adding polyvinylpyrrolidone for complexing polyphenols, without any other clean-up or preconcentration steps. The limit of detection for detecting OTA in wines was of 0.11 ± 0.01 ng L(-1), well below the permitted content of the mycotoxin by the European Union (<2 ng mL(-1)). Spiked wines were subjected to immunosensor calibrations to study the matrix effects. OTA concentrations measured with the immunosensor were compared with those obtained by high-performance liquid chromatography coupled to fluorescence detection (AOAC official method 2001.01). The OTA levels from two red wines of "Campo de Borja", Spain, ranged from about 0.027 to 0.033 ng mL(-1) of OTA.
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Batista, Alex D; Chocholouš, Petr; Satínský, Dalibor; Solich, Petr; Rocha, Fábio R P
2015-02-01
On-line sample pretreatment (clean-up and analyte preconcentration) is for the first time coupled to sequential injection chromatography. The approach combines anion-exchange solid-phase extraction and the highly effective pentafluorophenylpropyl (F5) fused-core particle column for separation of eight sulfonamide antibiotics with similar structures (sulfathiazole, sulfanilamide, sulfacetamide, sulfadiazine, sulfamerazine, sulfadimidine, sulfamethoxazole and sulfadimethoxine). The stationary phase was selected after a critical comparison of the performance achieved by three fused-core reversed phase columns (Ascentis(®) Express RP-Amide, Phenyl-Hexyl, and F5) and two monolithic columns (Chromolith(®) High Resolution RP-18 and CN). Acetonitrile and acetate buffer pH 5.0 at 0.60 mL min(-1) were used as mobile phase to perform the separations before spectrophotometric detection. The first mobile phase was successfully used as eluent from SPE column ensuring transfer of a narrow zone to the chromatographic column. Enrichment factors up to 39.2 were achieved with a 500 µL sample volume. The developed procedure showed analysis time <10.5 min, resolutions >1.83 with peak symmetry ≤1.52, LODs between 4.9 and 27 µg L(-1), linear response ranges from 30.0 to 1000.0 µg L(-1) (r(2)>0.996) and RSDs of peak heights <2.9% (n=6) at a 100 µg L(-1) level and enabled the screening control of freshwater samples contaminated at the 100 µg L(-1) level. The proposed approach expanded the analytical potentiality of SIC and avoided the time-consuming batch sample pretreatment step, thus minimizing risks of sample contamination and analyte losses. Copyright © 2014 Elsevier B.V. All rights reserved.
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Cao, Jiliang; Kong, Weijun; Zhou, Shujun; Yin, Lihui; Wan, Li; Yang, Meihua
2013-04-01
A simple, reliable, and low-cost method based on molecularly imprinted polymer as a selective sorbent of SPE was proposed for the determination of ochratoxin A (OTA) in beer, red wine, and grape juice by HPLC coupled with fluorescence detection (HPLC-FLD). Samples were diluted with water and cleaned up with an AFFINIMIP® SPE OTA column. After washing and eluting, the analyte was analyzed by HPLC-FLD. Under the optimized conditions, LOD and LOQ for OTA were 0.025 and 0.08 ng/mL, respectively. The recoveries of OTA from beer, red wine, and grape spiked at 0.1, 2, and 5 ng/mL ranged from 91.6 to 101.7%. Furthermore, after a simple regenerated procedure, the molecularly imprinted polymer based SPE column could be reused at least 14 times to achieve more than 80% recoveries of OTA in real samples. The developed method was applied to the detection of 30 beer, red wine, and grape juice samples and only four samples were contaminated by OTA with levels below the legal limits. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Londoño-Restrepo, S M; Jeronimo-Cruz, R; Rubio-Rosas, E; Rodriguez-García, M E
2018-05-02
This paper focus on physicochemical changes in bio-hydroxyapatite (BIO-HAp) from bovine femur obtained by calcination at high temperatures: 520-620 (each 20 °C) at 7.4 °C/min and from 700 to 1100 °C (each 100 °C) at three heating rates: 7.4, 9.9, and 11.1 °C/min. BIO-HAp samples were obtained using a multi-step process: cleaning, milling, hydrothermal process, calcination in an air atmosphere, and cooling in furnace air. Inductively Couple Plasma (ICP) showed that the presence of Mg, K, S, Ba, Zn, and Na, is not affected by the annealing temperature and heating rate. While Scanning Electron Microscopy (SEM) images showed the continuous growth of the HAp crystals during the calcination process due to the coalescence phenomenon, and the Full Width at the Half Maximum for the X-ray patterns for temperatures up to 700 is affected by the annealing temperature and the heating rate. Through X-ray diffraction, thermal, and calorimetric analysis (TGA-DSC), a partial dehydroxylation of hydroxyapatite was found in samples calcined up to 900 °C for the three heating rates. Also, Ca/P molar ratio decreased for samples calcined up to 900 °C as a result of the dehydroxylation process. NaCaPO 4 , CaCO 3 , Ca 3 (PO 4 ) 2 , MgO, and Ca(H 2 PO 4 ) 2 are some phases identified by X-ray diffraction; some of them are part of the bone and others were formed during the calcination process as a function of annealing temperature and heating rate, as it is the case for MgO.
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Lozano, Ana; Rajski, Łukasz; Belmonte-Valles, Noelia; Uclés, Ana; Uclés, Samanta; Mezcua, Milagros; Fernández-Alba, Amadeo R
2012-12-14
This paper presents the validation of a modified QuEChERS method in four matrices - green tea, red tea, black tea and chamomile. The experiments were carried out using blank samples spiked with a solution of 86 pesticides (insecticides, fungicides and herbicides) at four levels - 10, 25, 50 and 100 μg/kg. The samples were extracted according to the citrate QuEChERS protocol; however, to reduce the amount of coextracted matrix compounds, calcium chloride was employed instead of magnesium sulphate in the clean-up step. The samples were analysed by LC-MS/MS and GC-MS/MS. Included in the scope of validation were: recovery, linearity, matrix effects, limits of detection and quantitation as well as intra-day and inter-day precision. The validated method was used in a real sample survey carried out on 75 samples purchased in ten different countries. In all matrices, recoveries of the majority of compounds were in the 70-120% range and were characterised by precision lower than 20%. In 85% of pesticide/matrix combinations the analytes can be detected quantitatively by the proposed method at the European Union Maximum Residue Level. The analysis of the real samples revealed that large number of teas and chamomiles sold in the European Union contain pesticides whose usage is not approved and also pesticides in concentrations above the EU MRLs. Copyright © 2012 Elsevier B.V. All rights reserved.
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Process Research ON Semix Silicon Materials (PROSSM)
NASA Astrophysics Data System (ADS)
Wohlgemuth, J. H.; Warfield, D. B.
1982-02-01
A cost effective process sequence was identified, equipment was designed to implement a 6.6 MW per year automated production line, and a cost analysis projected a $0.56 per watt cell add-on cost for this line. Four process steps were developed for this program: glass beads back clean-up, hot spray antireflective coating, wave soldering of fronts, and ion milling for edging. While spray dopants were advertised as an off the shelf developed product, they were unreliable with shorter than advertised shelf life.
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Process Research ON Semix Silicon Materials (PROSSM)
NASA Technical Reports Server (NTRS)
Wohlgemuth, J. H.; Warfield, D. B.
1982-01-01
A cost effective process sequence was identified, equipment was designed to implement a 6.6 MW per year automated production line, and a cost analysis projected a $0.56 per watt cell add-on cost for this line. Four process steps were developed for this program: glass beads back clean-up, hot spray antireflective coating, wave soldering of fronts, and ion milling for edging. While spray dopants were advertised as an off the shelf developed product, they were unreliable with shorter than advertised shelf life.
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How to save the national priorities list from the D.C. Circuit -- and itself
DOE Office of Scientific and Technical Information (OSTI.GOV)
Applegate, J.S.
1993-12-31
This article considers the National Priorities List (NPL) and its fate at the hands of the U.S. Court of Appeals for the District of Columbia Circuit. This author describes how the statutory structure of CERCLA, its bureaucratic implementation, and its juducual mistreatment have combined to focus enormous resources on the decisionmaking steps along the way, instead of the actual clean-up. This has contributed to the embarrassingly unproductive system whose reauthorization is now before Congress. 123 refs.
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MINERALOGICAL PRESERVATION OF SOLID SAMPLES COLLECTED FROM ANOXIC SUBSURFACE ENVIRONMENTS
Remedial technologies utilized at hazardous waste sites for the treatment of metal and metalloid contaminants often take advantage of reduction-oxidation (redox) processes to reach ground water clean up goals. This is because redox reactions, in many cases, govern the biogeochem...
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NASA Astrophysics Data System (ADS)
Kowalski, Julia; Francke, Gero; Feldmann, Marco; Espe, Clemens; Heinen, Dirk; Digel, Ilya; Clemens, Joachim; Schüller, Kai; Mikucki, Jill; Tulaczyk, Slawek M.; Pettit, Erin; Berry Lyons, W.; Dachwald, Bernd
2017-04-01
There is significant interest in sampling subglacial environments for geochemical and microbiological studies, yet those environments are typically difficult to access. Existing ice-drilling technologies make it cumbersome to maintain microbiologically clean access for sample acquisition and environmental stewardship of potentially fragile subglacial aquatic ecosystems. With the "IceMole", a minimally invasive, maneuverable subsurface ice probe, we have developed a clean glacial exploration technology for in-situ analysis and sampling of glacial ice and sub- and englacial materials. Its design is based on combining melting and mechanical stabilization, using an ice screw at the tip of the melting head to maintain firm contact between the melting head and the ice. The IceMole can change its melting direction by differential heating of the melting head and optional side wall heaters. Downward, horizontal and upward melting, as well as curve driving and penetration of particulate-ladden layers has already been demonstrated in several field tests. This maneuverability of the IceMole also necessitates a sophisticated on-board navigation system, capable of autonomous operations. Therefore, between 2012 and 2014, a more advanced probe was developed as part of the "Enceladus Explorer" (EnEx) project. The EnEx-IceMole offers systems for accurate positioning, based on in-ice attitude determination, acoustic positioning, ultrasonic obstacle and target detection, which is all integrated through a high-level sensor fusion algorithm. In December 2014, the EnEx-IceMole was used for clean access into a unique subglacial aquatic environment at Blood Falls, Antarctica, where an englacial brine sample was successfully obtained after about 17 meters of oblique melting. Particular attention was paid to clean protocols for sampling for geochemical and microbiological analysis. In this contribution, we will describe the general technological approach of the IceMole and report on the results of its deployment at Blood Falls. In contrast to conventional melting-probe applications, which can only melt vertically, the IceMole realized an oblique melting path to penetrate the englacial conduit. Experimental and numerical results on melting at oblique angles are rare. Besides reporting on the IceMole technology and the field deployment itself, we will compare and discuss the observed melting behavior with re-analysis results in the context of a recently developed numerical model. Finally, we will present our first steps in utilizing the model to infer on the ambient cryo-environment.
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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.
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Repetitive cleaning of a stainless steel first mirror using radio frequency plasma
NASA Astrophysics Data System (ADS)
Peng, Jiao; Yan, Rong; Ding, Rui; Chen, Junling; Zhu, Dahuan; Zhang, Zengming
2017-10-01
First mirrors (FMs) are crucial components of optical diagnostic systems in present-day tokamaks and future fusion reactors. Their lifetimes should be extremely limited due to their proximity to burning plasma, greatly influencing the safe operation of corresponding diagnostics. Repetitive cleaning is expected to provide a solution to the frequent replacement of contaminated FMs, thus prolonging their lifetimes. Three repetitive cleaning cycles using radio frequency plasma were applied to stainless steel (SS) FM samples, to evaluate the change of the mirrors’ optical properties and morphology during each cycle. Amorphous carbon films were deposited on mirror surfaces under identical conditions in three cycles. In three cycles with identical cleaning parameters, the total reflectivity was restored at up to 95%. Nevertheless, with successive cleaning cycles, the FM surfaces gradually appeared to roughen due to damage to the grain boundaries. Correspondingly, the diffuse reflectivity increased from a few percent to 20% and 27% after the second and third cycles. After optimizing the cleaning parameters of the second and third cycles, the roughness showed a significant decrease, and simultaneously the increase of diffuse reflectivity was remarkably improved.
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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
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Rogers, Heather D; Desciak, Edward B; Marcus, Rebecca P; Wang, Shuang; MacKay-Wiggan, Julian; Eliezri, Yehuda D
2010-11-01
Mohs micrographic surgery (MMS) has a low rate of surgical site infection (SSI) without the use of prophylactic antibiotics. In the studies to date, there has been variation in the steps taken by each surgeon to prevent SSIs but in all cases sterile technique was used during wound reconstruction. We sought to evaluate the rate of SSIs among patients undergoing MMS with the use of clean surgical technique for all steps of MMS including wound reconstruction in the absence of prophylactic antibiotics. We prospectively evaluated 1000 patients undergoing MMS using clean surgical technique for SSIs. Clean surgical technique includes the use of clean surgical gloves and towels and a single pack of sterile instruments for all steps including wound reconstruction. There were 11 SSIs among 1000 patients with 1204 tumors, with an overall rate of infection of 0.91% (95% confidence interval 0.38%-1.45%). Three of the 11 infections were complications of hematomas. Four of the 11 infections occurred in flap closures, which had the highest rate of SSIs of 2.67% (4/150). The study was a prospective, single-institution uncontrolled study. To our knowledge, this is the first study to examine the rate of SSIs with the use of clean surgical technique, in the absence of antibiotic prophylaxis, for all steps of MMS including wound reconstruction. Our rate of SSIs of 0.91% is exceedingly low, underscoring the overall safety of MMS and its performance in the outpatient setting without the use of antibiotic prophylaxis or sterile technique. Copyright © 2010 American Academy of Dermatology, Inc. Published by Mosby, Inc. All rights reserved.
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Improving Malaysian cocoa quality through the use of dehumidified air under mild drying conditions.
Hii, Ching L; Law, Chung L; Cloke, Michael; Sharif, Suzannah
2011-01-30
Various studies have been conducted in the past to improve the quality of Malaysian cocoa beans. However, the processing methods still remain crude and lack technological advancement. In terms of drying, no previous study has attempted to apply advanced drying technology to improve bean quality. This paper presents the first attempt to improve the quality of cocoa beans through heat pump drying using constant air (28.6 and 40.4 °C) and stepwise (step-up 30.7-43.6-56.9 °C and step-down 54.9-43.9 °C) drying profiles. Comparison was made against hot air drying at 55.9 °C. Product quality assessment showed significant improvement in the quality of Malaysian cocoa beans. Quality was found to be better in terms of lower acidity (higher pH) and higher degree of browning (cut test) for cocoa beans dried using the step-up profile. All heat pump-dried samples showed flavour quality comparable to that of Ghanaian and better than that of Malaysian and Indonesian commercial samples. Step-up-dried samples showed the best flavour profile with high level of cocoa flavour, low in sourness and not excessive in bitterness and astringency. Dried cocoa samples from the step-up drying profile showed the best overall quality as compared with commercial samples from Malaysia, Indonesia and Ghana. The improvement of Malaysian cocoa bean quality is thus achievable through heat pump drying. 2010 Society of Chemical Industry.
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Ramírez-Silva, Ivonne; Jiménez-Aguilar, Alejandra; Valenzuela-Bravo, Danae; Martinez-Tapia, Brenda; Rodríguez-Ramírez, Sonia; Gaona-Pineda, Elsa Berenice; Angulo-Estrada, Salomón; Shamah-Levy, Teresa
2016-01-01
To describe the methodology used to clean up and estimate dietary intake (DI) data from the Semi-Quantitative Food Frequency Questionnaire (SFFQ) of the Mexican National Health and Nutrition Survey 2012. DI was collected through a shortterm SFFQ regarding 140 foods (from October 2011 to May 2012). Energy and nutrient intake was calculated according to a nutrient database constructed specifically for the SFFQ. A total of 133 nutrients including energy and fiber were generated from SFFQ data. Between 4.8 and 9.6% of the survey sample was excluded as a result of the cleaning process.Valid DI data were obtained regarding energy and nutrients consumed by 1 212 pre-school children, 1 323 school children, 1 961 adolescents, 2 027 adults and 526 older adults. We documented the methodology used to clean up and estimate DI from the SFFQ used in national dietary assessments in Mexico.
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Mouse Cleaning Apparatus and Method
NASA Technical Reports Server (NTRS)
Williams, Glenn L. (Inventor)
2005-01-01
The method of using the mouse pad cleaning apparatus is disclosed and claimed. The method comprises the steps of uncovering the mouse cleaning surface, applying the mouse and ball of the mouse to the cleaning surface, moving the mouse in a rotational pattern on the mouse cleaning surface, removing the mouse form the mouse cleaning surface, washing the cleaning surface, and covering the mouse cleaning surface. A mouse pad cleaning apparatus comprising a plurality of substrates, each said substrate having adhesive thereon, said plurality of substrates residing in and affixed to a receptacle. A single substrate having adhesive, which may be washable or non-washable, thereon may be employed. The washable adhesive may be an organopolysiloxane or gelatinous elastomer.
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ERIC Educational Resources Information Center
Ellis, Tom
2000-01-01
Examines tested techniques that can keep a school's carpeting in good condition. Cleaning with hot water extraction, removing spills and spots, handling emergency cleanups, and cleaning soft surface flooring are addressed. (GR)
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Tewfik, Ihab
2008-01-01
2-Alkylcyclobutanones (cyclobutanones) are accepted as chemical markers for irradiated foods containing lipid. However, current extraction procedures (Soxhlet-florisil chromatography) for the isolation of these markers involve a long and tedious clean-up regime prior to gas chromatography-mass spectrophotometry identification. This paper outlines an alternative isolation and clean-up method for the extraction of cyclobutanones in irradiated Camembert cheese. The newly developed direct solvent extraction method enables the efficient screening of large numbers of food samples and is not as resource intensive as the BS EN 1785:1997 method. Direct solvent extraction appears to be a simple, robust method and has the added advantage of a considerably shorter extraction time for the analysis of foods containing lipid.
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Occurrence of Ochratoxin A in Grape Juice of Iran
Yusefi, Jamal; Valaee, Mehran; Nazari, Firouzeh; Maleki, Javad; Mottaghianpour, Ehsan; Khosrokhavar, Roya; Hosseini, Mir-Jamal
2018-01-01
Ochratoxin A (OTA) is one of the most important mycotoxins that contaminate a broad range of agricultural and food products. In this study, the occurrence of OTA in available brands of grape juice in Iran purchased from retail outlets or producer were determined for the first time using high-performance liquid chromatography (HPLC) with immunoaffinity columns(IAC) as the clean-up step. The average recoveries for OTA in grape juice ranged from 54.2 to 86.6% with the coefficient of variation lower than 17.3% in lowest spiked level (0.5 µg/L). The estimated LOD and LOQ of OTA were 0.04 µg/L and 0.125 µg/L, respectively. In our study, 70 samples of grape juice evaluated for OTA content. The results showed that in 39 out of 70 samples (55.7%) OTA levels were above the LOQ with the maximum level of 2.6 µg/L and the mean contamination was 0.5 µg/L. Although the mean contamination of OTA in analyzing samples was lower than the MRL set by EU, the high incidence of contamination in these products is worried. Considering the importance of OTA in public health, control of pre- and post-harvest, storage and grape juice manufacturing process, such as HACCP, GAP, and GMP recommended preventive measures are required. PMID:29755546
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Zhang, Zhiwen; Li, Xiaowei; Ding, Shuangyang; Jiang, Haiyang; Shen, Jianzhong; Xia, Xi
2016-08-01
A multiresidue method for the efficient identification and quantification of 38 compounds from 3 different classes of antibiotics (tetracyclines, sulfonamides, and quinolones) in animal tissues has been developed. The method optimization involved the selection of extraction solutions, comparison of different solid-phase extraction cartridges and different mobile phases. As a result, the samples were extracted with Mcllvaine and phosphate buffers, followed by clean-up step based on solid-phase extraction with Oasis HLB cartridge. All compounds were determined by ultra-high performance liquid chromatography-tandem mass spectrometry, in one single injection with a chromatographic run time of only 9min. The method efficiency was evaluated in 5 tissues including muscle, liver, and kidney, and the mean recoveries ranged from 54% to 102%, with inter-day relative standard deviation lower than 14%. The limits of quantification were between 0.5 and 10μg/kg, which were satisfactory to support future surveillance monitoring. The developed method was applied to the analysis of swine liver and chicken samples from local markets, and sulfamethazine was the most commonly detected compound in the animal samples, with the highest residue level of 998μg/kg. Copyright © 2016 Elsevier Ltd. All rights reserved.
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Hunting for Dark Matter in Spheroidal Galaxies
NASA Astrophysics Data System (ADS)
Steele, Rebecca; Holwerda, Benne; Kielkopf, John F.
2018-06-01
Searches for blended spectra have been highly successful in identifying strongly lensing galaxies: these spectra show a low-redshift passive galaxy with much stronger emission lines from the source being lensed. We have recently identified 112 strong lensing candidates in the Galaxy and Mass Assembly Survey (GAMA). The improved sensitivity and redshift determination makes this a very clean sample of two-galaxy spectra, spanning both lower-mass galaxy strong lenses as well as a higher redshiftregime (z > 0.4). As a first step of a PhD project, we will vet the 112 candidate strong gravitational lenses using the new Kilo Degree Survey (KiDS), which is both deeper and sharper than existing Sloan images. Once confirmed, these lower mass gravitational lenses can be targeted with the soon-to-launch James Webb Space Telescope or the Hubble Space Telescope for follow-up observations. Models of the gravitational lenses give us direct measures of the dark matter content of these low-mass galaxies, thought to be dominated by dark matter.
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Sub-nanometer Resolution Imaging with Amplitude-modulation Atomic Force Microscopy in Liquid
Farokh Payam, Amir; Piantanida, Luca; Cafolla, Clodomiro; Voïtchovsky, Kislon
2016-01-01
Atomic force microscopy (AFM) has become a well-established technique for nanoscale imaging of samples in air and in liquid. Recent studies have shown that when operated in amplitude-modulation (tapping) mode, atomic or molecular-level resolution images can be achieved over a wide range of soft and hard samples in liquid. In these situations, small oscillation amplitudes (SAM-AFM) enhance the resolution by exploiting the solvated liquid at the surface of the sample. Although the technique has been successfully applied across fields as diverse as materials science, biology and biophysics and surface chemistry, obtaining high-resolution images in liquid can still remain challenging for novice users. This is partly due to the large number of variables to control and optimize such as the choice of cantilever, the sample preparation, and the correct manipulation of the imaging parameters. Here, we present a protocol for achieving high-resolution images of hard and soft samples in fluid using SAM-AFM on a commercial instrument. Our goal is to provide a step-by-step practical guide to achieving high-resolution images, including the cleaning and preparation of the apparatus and the sample, the choice of cantilever and optimization of the imaging parameters. For each step, we explain the scientific rationale behind our choices to facilitate the adaptation of the methodology to every user's specific system. PMID:28060262
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Reichel, W.L.; Kolbe, E.J.; Stafford, C.J.
1981-01-01
A procedure is described for determining fenvalerate and permethrin residues in grasshoppers and duck tissues. Samples are Soxhlet-extracted with hexane and cleaned up by gel permeation chromatography with an in-line alumina column. Samples are analyzed by gas-liquid chromatography with electron capture detection, and confirmed by gas-liquid chromatography-mass spectrometry. The average recovery from fortified tissues was 97%.
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Treatment of surfaces with low-energy electrons
NASA Astrophysics Data System (ADS)
Frank, L.; Mikmeková, E.; Lejeune, M.
2017-06-01
Electron-beam-induced deposition of various materials from suitable precursors has represented an established branch of nanotechnology for more than a decade. A specific alternative is carbon deposition on the basis of hydrocarbons as precursors that has been applied to grow various nanostructures including masks for subsequent technological steps. Our area of study was unintentional electron-beam-induced carbon deposition from spontaneously adsorbed hydrocarbon molecules. This process traditionally constitutes a challenge for scanning electron microscopy practice preventing one from performing any true surface studies outside an ultrahigh vacuum and without in-situ cleaning of samples, and also jeopardising other electron-optical devices such as electron beam lithographs. Here we show that when reducing the energy of irradiating electrons sufficiently, the e-beam-induced deposition can be converted to e-beam-induced release causing desorption of hydrocarbons and ultimate cleaning of surfaces in both an ultrahigh and a standard high vacuum. Using series of experiments with graphene samples, we demonstrate fundamental features of e-beam-induced desorption and present results of checks for possible radiation damage using Raman spectroscopy that led to optimisation of the electron energy for damage-free cleaning. The method of preventing carbon contamination described here paves the way for greatly enhanced surface sensitivity of imaging and substantially reduced demands on vacuum systems for nanotechnological applications.
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Luque-Muñoz, A; Vílchez, J L; Zafra-Gómez, A
2017-07-21
An analytical method for the analysis of 16 pharmaceuticals and personal care products in compost from sewage sludge is successfully validated. Ultrasound assisted extraction with a mixture of acetonitrile:ethyl acetate (1:1, v/v) containing 10% (v/v) of acetic acid was carried out. Two cycles of extraction of 10min were applied. A clean-up of the extracts using salt-assisted liquid-liquid extraction (SALLE) was also included. Experimental design was used for the optimization of the main parameters involved in the extraction and cleaned-up steps. The chromatographic separation was carried out by ultrahigh performance liquid chromatography using a mobile phase gradient mixture of a 13mM buffer ammonium formate solution (pH 9.25) (solvent A) and methanol (solvent B). An ACQUITY UPLC ® BEH C18 column (1.7μm; 2.1×50mm) column was used. Analytes were separated in less than 11min. The compounds were detected and quantified using single reaction monitoring electrospray tandem mass spectrometry. The limits of detection calculated ranged from 0.5 to 4ngg -1 d.w., and the limits of quantification from 2 to 13ngg -1 d.w. Recoveries from 93% to 111%, with relative standar deviations lower than 11% in all cases, were obtained. The method was applied to natural compost samples. High concentrations of some analytes were found. Ketoprofen (510ngg -1 d.w.), methylparaben (240ngg -1 d.w.), diclofenac (175ngg -1 d.w.) and flufenamic acid (128ngg -1 d.w.) were the most abundant. Copyright © 2017 Elsevier B.V. All rights reserved.
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Cleaning a semipermeable membrane in a papermaking machine
Beck, David A.
2004-01-06
A method of cleaning a semipermeable membrane, the semipermeable membrane being configured for carrying a fiber web, includes the steps of providing a cleaning fluid and applying the cleaning fluid on the semipermeable membrane. Further, an air press configured for carrying the semipermeable membrane therethrough is provided, and the air press has pressurized air therein. The semipermeable membrane is conveyed through the air press and is subjected to the pressurized air within the air press. The pressurized air thereby flushes the cleaning fluid through the semipermeable membrane.
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Bixler, Gregory D; Bhushan, Bharat
2014-01-07
In search of new solutions to complex challenges, researchers are turning to living nature for inspiration. For example, special surface characteristics of rice leaves and butterfly wings combine the shark skin (anisotropic flow leading to low drag) and lotus leaf (superhydrophobic and self-cleaning) effects, producing the so-called rice and butterfly wing effect. In this paper, we study four microstructured surfaces inspired by rice leaves and fabricated with photolithography techniques. We also present a method of creating such surfaces using a hot embossing procedure for scaled-up manufacturing. Fluid drag, self-cleaning, contact angle, and contact angle hysteresis data are presented to understand the role of sample geometrical dimensions. Conceptual modeling provides design guidance when developing novel low drag, self-cleaning, and potentially antifouling surfaces for medical, marine, and industrial applications.
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NASA Astrophysics Data System (ADS)
Bixler, Gregory D.; Bhushan, Bharat
2013-12-01
In search of new solutions to complex challenges, researchers are turning to living nature for inspiration. For example, special surface characteristics of rice leaves and butterfly wings combine the shark skin (anisotropic flow leading to low drag) and lotus leaf (superhydrophobic and self-cleaning) effects, producing the so-called rice and butterfly wing effect. In this paper, we study four microstructured surfaces inspired by rice leaves and fabricated with photolithography techniques. We also present a method of creating such surfaces using a hot embossing procedure for scaled-up manufacturing. Fluid drag, self-cleaning, contact angle, and contact angle hysteresis data are presented to understand the role of sample geometrical dimensions. Conceptual modeling provides design guidance when developing novel low drag, self-cleaning, and potentially antifouling surfaces for medical, marine, and industrial applications.
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Deme, Pragney; Azmeera, Tirupathi; Prabhavathi Devi, B L A; Jonnalagadda, Padmaja R; Prasad, R B N; Vijaya Sarathi, U V R
2014-01-01
An improved sample preparation using dispersive solid-phase extraction clean-up was proposed for the trace level determination of 35 multiclass pesticide residues (organochlorine, organophosphorus and synthetic pyrethroids) in edible oils. Quantification of the analytes was carried out by gas chromatography-mass spectrometry in negative chemical ionisation mode (GC-NCI-MS/MS). The limit of detection and limit of quantification of residues were in the range of 0.01-1ng/g and 0.05-2ng/g, respectively. The analytes showed recoveries between 62% and 110%, and the matrix effect was observed to be less than 25% for most of the pesticides. Crude edible oil samples showed endosulfan isomers, p,p'-DDD, α-cypermethrin, chlorpyrifos, and diazinon residues in the range of 0.56-2.14ng/g. However, no pesticide residues in the detection range of the method were observed in refined oils. Copyright © 2013 Elsevier Ltd. All rights reserved.
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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.
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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.
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Analytical strategies for organic food packaging contaminants.
Sanchis, Yovana; Yusà, Vicent; Coscollà, Clara
2017-03-24
In this review, we present current approaches in the analysis of food-packaging contaminants. Gas and liquid chromatography coupled to mass spectrometry detection have been widely used in the analysis of some relevant families of these compounds such as primary aromatic amines, bisphenol A, bisphenol A diglycidyl ether and related compounds, UV-ink photoinitiators, perfluorinated compounds, phthalates and non-intentionally added substances. Main applications for sample treatment and different types of food-contact material migration studies have been also discussed. Pressurized Liquid Extraction, Solid-Phase Microextraction, Focused Ultrasound Solid-Liquid Extraction and Quechers have been mainly used in the extraction of food contact material (FCM) contaminants, due to the trend of minimising solvent consumption, automatization of sample preparation and integration of extraction and clean-up steps. Recent advances in analytical methodologies have allowed unequivocal identification and confirmation of these contaminants using Liquid Chromatography coupled to High Resolution Mass Spectrometry (LC-HRMS) through mass accuracy and isotopic pattern applying. LC-HRMS has been used in the target analysis of primary aromatic amines in different plastic materials, but few studies have been carried out applying this technique in post-target and non-target analysis of FCM contaminants. Copyright © 2017 Elsevier B.V. All rights reserved.
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Clean Money, Clean Elections Act of 2009
Rep. Tierney, John F. [D-MA-6
2009-04-22
House - 04/23/2009 Referred to the Subcommittee on Communications, Technology, and the Internet. (All Actions) Tracker: This bill has the status IntroducedHere are the steps for Status of Legislation:
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NASA Astrophysics Data System (ADS)
Wang, Chenxi; Xu, Jikai; Zeng, Xiaorun; Tian, Yanhong; Wang, Chunqing; Suga, Tadatomo
2018-02-01
We demonstrate a facile bonding process for combining silicon and quartz glass wafers by a two-step wet chemical surface cleaning. After a post-annealing at 200 °C, strong bonding interfaces with no defects or microcracks were obtained. On the basis of the detailed surface and bonding interface characterizations, the bonding mechanism was explored and discussed. The amino groups terminated on the cleaned surfaces might contribute to the bonding strength enhancement during the annealing. This cost-effective bonding process has great potentials for silicon- and glass-based heterogeneous integrations without requiring a vacuum system.
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Liu, Chang; Gómez-Ríos, Germán Augusto; Schneider, Bradley B; Le Blanc, J C Yves; Reyes-Garcés, Nathaly; Arnold, Don W; Covey, Thomas R; Pawliszyn, Janusz
2017-10-23
Mass spectrometry (MS) based quantitative approaches typically require a thorough sample clean-up and a decent chromatographic step in order to achieve needed figures of merit. However, in most cases, such processes are not optimal for urgent assessments and high-throughput determinations. The direct coupling of solid phase microextraction (SPME) to MS has shown great potential to shorten the total sample analysis time of complex matrices, as well as to diminish potential matrix effects and instrument contamination. In this study, we demonstrate the use of the open-port probe (OPP) as a direct and robust sampling interface to couple biocompatible-SPME (Bio-SPME) fibres to MS for the rapid quantitation of opioid isomers (i.e. codeine and hydrocodone) in human plasma. In place of chromatography, a differential mobility spectrometry (DMS) device was implemented to provide the essential selectivity required to quantify these constitutional isomers. Taking advantage of the simplified sample preparation process based on Bio-SPME and the fast separation with DMS-MS coupling via OPP, a high-throughput assay (10-15 s per sample) with limits of detection in the sub-ng/mL range was developed. Succinctly, we demonstrated that by tuning adequate ion mobility separation conditions, SPME-OPP-MS can be employed to quantify non-resolved compounds or those otherwise hindered by co-extracted isobaric interferences without further need of coupling to other separation platforms. Copyright © 2017 Elsevier B.V. All rights reserved.
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Potential sources of microbial contamination in unpasteurized apple cider.
Garcia, Luis; Henderson, John; Fabri, Martha; Oke, Moustapha
2006-01-01
A study was conducted to identify possible sources of microbial contamination and to assess the effect of good cleaning and sanitation practices on the microbial quality and safety of unpasteurized apple cider. Raw unwashed apples, washed apples, cleaning water, fresh cider, and finished cider samples were collected from five Ontario producers over 4 months and microbiologically tested. Total coliforms were found in 31, 71 and 38% of the unwashed apple, water, and washed apple samples, respectively. Escherichia coli was found in 40% of the water samples from one producer alone. The washing step was identified as a potential source of contamination, possibly due to water in the dump tanks seldom being refreshed, and because scrubbers, spray nozzles, and conveyors were not properly cleaned and sanitized. Higher total coliform counts (P < 0.0001) and prevalence (P < 0.0001) in fresh cider compared with those in unwashed apples and washed apples indicated considerable microbial buildup along the process, possibly explained by the lack of appropriate equipment sanitation procedures. Results showed that producers who had better sanitary practices in place had lower (P < 0.001) total coliform prevalence than the rest of the producers. Overall results show that good sanitation procedures are associated with improved microbial quality of fresh cider in terms of total coliforms and that operators who pasteurize and/or UV treat their product should still be required to have a sound good manufacturing practices program in place to prevent recontamination. Cryptosporidium parvum, an important pathogen for this industry, was found in different sample types, including washed apples, water, and fresh and finished cider.
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DOE Office of Scientific and Technical Information (OSTI.GOV)
Barth, Michael; Datta, Suman, E-mail: sdatta@engr.psu.edu; Bruce Rayner, G.
2014-12-01
We investigate in-situ cleaning of GaSb surfaces and its effect on the electrical performance of p-type GaSb metal-oxide-semiconductor capacitor (MOSCAP) using a remote hydrogen plasma. Ultrathin HfO{sub 2} films grown by atomic layer deposition were used as a high permittivity gate dielectric. Compared to conventional ex-situ chemical cleaning methods, the in-situ GaSb surface treatment resulted in a drastic improvement in the impedance characteristics of the MOSCAPs, directly evidencing a much lower interface trap density and enhanced Fermi level movement efficiency. We demonstrate that by using a combination of ex-situ and in-situ surface cleaning steps, aggressively scaled HfO{sub 2}/p-GaSb MOSCAP structuresmore » with a low equivalent oxide thickness of 0.8 nm and efficient gate modulation of the surface potential are achieved, allowing to push the Fermi level far away from the valence band edge high up into the band gap of GaSb.« less
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Bi, Xiaodong; Liu, Zhen
2014-12-16
Enzyme activity assay is an important method in clinical diagnostics. However, conventional enzyme activity assay suffers from apparent interference from the sample matrix. Herein, we present a new format of enzyme activity assay that can effectively eliminate the effects of the sample matrix. The key is a 96-well microplate modified with molecularly imprinted polymer (MIP) prepared according to a newly proposed method called boronate affinity-based oriented surface imprinting. Alkaline phosphatase (ALP), a glycoprotein enzyme that has been routinely used as an indicator for several diseases in clinical tests, was taken as a representative target enzyme. The prepared MIP exhibited strong affinity toward the template enzyme (with a dissociation constant of 10(-10) M) as well as superb tolerance for interference. Thus, the enzyme molecules in a complicated sample matrix could be specifically captured and cleaned up for enzyme activity assay, which eliminated the interference from the sample matrix. On the other hand, because the boronate affinity MIP could well retain the enzymatic activity of glycoprotein enzymes, the enzyme captured by the MIP was directly used for activity assay. Thus, additional assay time and possible enzyme or activity loss due to an enzyme release step required by other methods were avoided. Assay of ALP in human serum was successfully demonstrated, suggesting a promising prospect of the proposed method in real-world applications.
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Cedeño, M
1995-01-01
Tequila is obtained from the distillation of fermented juice of agave plant, Agave tequilana, to which up to 49% (w/v) of an adjunct sugar, mainly from cane or corn, could be added. Agave plants require from 8 to 12 years to mature and during all this time cleaning, pest control, and slacken of land are required to produce an initial raw material with the appropriate chemical composition for tequila production. Production process comprises four steps: cooking to hydrolyze inulin into fructose, milling to extract the sugars, fermentation with a strain of Saccharomyces cerevisiae to convert the sugars into ethanol and organoleptic compounds, and, finally, a two-step distillation process. Maturation, if needed, is carried out in white oak barrels to obtain rested or aged tequila in 2 or 12 months, respectively.
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High temperature thermocouple development program, part A and part B
NASA Technical Reports Server (NTRS)
Toenshoff, D. A.; Zysk, E. D.; Fleischner, P. L.
1972-01-01
The problem of extending the useful life of thermocouples intended for in-core and out-of-core thermionic applications in a vacuum environment at temperatures up to 2273 K for periods of time up to 10,000 hours was investigated. Many factors that may influence this useful life were examined, and a basic probe design was developed. With a few modifications, twenty-three thermocouple assemblies were fabricated. Generally the finished thermocouple consisted of solid doped W-3% Re and W-25% Re wires and high purity and high density BeO insulators, and was sheathed in a high purity tantalum tube. In a few probes, stranded thermocouple wires were substituted; commercial grade BeO was used; and in two cases, CVD W-22% Re tubing was used. Each of the components was made of the highest purity materials available; was subjected to special cleaning steps, and was assembled in a class 10,000 clean room. Pertinent physical and chemical properties were determined on each of the components. Special processing techniques were used in the fabrication of the high purity (99.95%), high density (over 95% of theoretical) BeO.
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Fontana, Ariel R; Lana, Nerina B; Martinez, Luis D; Altamirano, Jorgelina C
2010-06-30
Ultrasound-assisted leaching-dispersive solid-phase extraction followed by dispersive liquid-liquid microextraction (USAL-DSPE-DLLME) technique has been developed as a new analytical approach for extracting, cleaning up and preconcentrating polybrominated diphenyl ethers (PBDEs) from sediment samples prior gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis. In the first place, PBDEs were leached from sediment samples by using acetone. This extract was cleaned-up by DSPE using activated silica gel as sorbent material. After clean-up, PBDEs were preconcentrated by using DLLME technique. Thus, 1 mL acetone extract (disperser solvent) and 60 microL carbon tetrachloride (extraction solvent) were added to 5 mL ultrapure water and a DLLME technique was applied. Several variables that govern the proposed technique were studied and optimized. Under optimum conditions, the method detection limits (MDLs) of PBDEs calculated as three times the signal-to-noise ratio (S/N) were within the range 0.02-0.06 ng g(-1). The relative standard deviations (RSDs) for five replicates were <9.8%. The calibration graphs were linear within the concentration range of 0.07-1000 ng g(-1) for BDE-47, 0.09-1000 ng g(-1) for BDE-100, 0.10-1000 ng g(-1) for BDE-99 and 0.19-1000 ng g(-1) for BDE-153 and the coefficients of estimation were > or =0.9991. Validation of the methodology was carried out by standard addition method at two concentration levels (0.25 and 1 ng g(-1)) and by comparing with a reference Soxhlet technique. Recovery values were > or =80%, which showed a satisfactory robustness of the analytical methodology for determination of low PBDEs concentration in sediment samples. Copyright 2010 Elsevier B.V. All rights reserved.
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Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C
2016-01-28
Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed. Copyright © 2015 Elsevier B.V. All rights reserved.
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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)
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Łozowicka, Bożena; Mojsak, Patrycja; Kaczyński, Piotr; Konecki, Rafał; Borusiewicz, Andrzej
2017-12-15
The aim of this study was to investigate the dissipation of spirotetramat and its four metabolites (B-enol, B-keto, B-mono and B-glu) in different parts of vegetables belong to the minor crops (Appiacea and Brassicaceae) and soil from cultivation. The challenge of this study was to apply an optimized clean up step in QuEChERS to obtain one universal sorbent for different complex matrices like leaves with high levels of pigments, roots containing acids, sugars, polyphenolls and pigments and soil with organic ingredients. Eight commercial (Florisil, neutral alumina, GCB, PSA, C18, diatomaceous earth, VERDE and ChloroFiltr) and one organic (Chitosan) sorbents were tested. A modified clean up step in QuEChERS methodology was used for analysis. The dissipation of spirotetramat and its metabolites was described according to a first-order (FO) kinetics equation with R 2 between 0.9055 and 0.9838. The results showed that the time after 50% (DT 50 ) of the substance degraded was different for soil, roots and leaves, and amounted to 0.2day, 2.8-2.9days and 2.1-2.4days, respectively. The terminal residues of spiroteramat (expressed as the sum of spirotetramat, B-enol, B-glu, B-keto and B-mono) were much lower than the MRLs. Copyright © 2017 Elsevier B.V. All rights reserved.
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Pasquet, Camille; Vulliet, Emmanuelle
2011-10-15
Among the wide range of substances discharged continuously in the environment, alkylphenols became a major focus of environmental research in the last decades, as it was found that they possess endocrine disrupting properties. Knowledge about the occurrence and levels of alkylphenols in environment is critical for the risk assessment of these compounds on both ecosystem and human health. However, the analysis of traces of alkylphenols in environmental matrices is a very difficult task, and the suitable methods involve generally an extraction followed by an extensive sample clean-up before detection, steps often time-consuming and costly. In order to reduce the analysis time, obtain a high throughput of analysis and thus improve work efficiency, the objective of the present study is to investigate the use of immunochemical technique (ELISA) for the determination of nonylphenol and octylphenol in soils and various kinds of water. To our knowledge, this is the first time that the determination of alkylphenols in soil using immunoassay technique is described. A methodology is developed, based on the combination of a single preparation step and the use of a simply ELISA kit. The performances of the method are compared with LC-MS/MS, considered as reference. The developed procedure offers the sensitivity and selectivity necessary for the detection of the target alkylphenols in the ng/g or ng/L range, and is successfully applied to the analysis of several samples. Results indicate that alkylphenols are quantified with concentrations in the same order than LC-MS/MS, meaning that ELISA may be useful not only in screening the samples and get a positive/negative response, but also it allows a good approximation of the concentrations. Copyright © 2011 Elsevier B.V. All rights reserved.
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IDENTIFICATION OF COMPOUNDS IN SOUTH AFRICAN STREAM SAMPLES USING ION COMPOSITION ELUCIDATION (ICE)
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...
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Analysis of 2H-Evaporator Acid Cleaning Samples
DOE Office of Scientific and Technical Information (OSTI.GOV)
Hay, M.; Diprete, D.; Edwards, T.
The 2H-Evaporator acid cleaning solution samples were analyzed by SRNL to determine a composition for the scale present in the evaporator before recent acid cleaning. Composite samples were formed from the solution samples from the two acid cleaning cycles. The solution composition was converted to a weight percent scale solids basis under an assumed chemical composition. The scale composition produced from the acid cleaning solution samples indicates a concentration of 6.85 wt% uranium. An upper bound, onesided 95% confidence interval on the weight percent uranium value may be given as 6.9 wt% + 1.645 × 0.596 wt% = 7.9 wt%.more » The comparison of the composition from the current acid cleaning solutions with the composition of recent scale samples along with the thermodynamic modeling results provides reasonable assurance that the sample results provide a good representation of the overall scale composition in the evaporator prior to acid cleaning. The small amount of scale solids dissolved in the 1.5 M nitric acid during the evaporator cleaning process likely produced only a small amount of precipitation based on modeling results and the visual appearance of the samples.« less
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Multi-element RIMS Analysis of Genesis Solar Wind Collectors
NASA Astrophysics Data System (ADS)
Veryovkin, I. V.; Tripa, C. E.; Zinovev, A. V.; King, B. V.; Pellin, M. J.; Burnett, D. S.
2009-12-01
The samples of Solar Wind (SW) delivered by the NASA Genesis mission, present significant challenges for surface analytical techniques, in part due to severe terrestrial contamination of the samples on reentry, in part due to the ultra-shallow and diffused ion implants in the SW collector materials. We are performing measurements of metallic elements in the Genesis collectors using Resonance Ionization Mass Spectrometry (RIMS), an ultra-sensitive analytical method capable of detecting SW in samples with lateral dimensions of only a few mm and at concentrations from above one ppm to below one ppt. Since our last report at 2008 AGU Fall Meeting, we have (a) developed and tested new resonance ionization schemes permitting simultaneous measurements of up to three (Ca, Cr, and Mg) elements, and (b) improved reproducibility and accuracy of our RIMS analyses for SW-like samples (i.e. shallow ion implants) by developing and implementing an optimized set of new analytical protocols. This is important since the quality of scientific results from the Genesis mission critically depends on the accuracy of analytical techniques. In this work, we report on simultaneous RIMS measurements of Ca and Cr performed on two silicon SW collector samples, (#60179 and #60476). First, we have conducted test experiments with 3×1013 at/cm2 52Cr and 44Ca implants in silicon to evaluate the accuracy of our quantitative analyses. Implant fluencies were measured by RIMS to be 2.73×1013 and 2.71×1013 at/cm2 for 52Cr and 44Ca, respectively, which corresponds to an accuracy of ≈10%. Using the same implanted wafer as a reference, we conducted RIMS analyses of the Genesis samples: 3 spots on #60179 and 4 spots on #60476. The elemental SW fluencies expected for Cr and Ca are 2.95×1010 and 1.33×1011 at/cm2 , respectively. Our measurements of 52Cr yielded 3.0±0.6×1011 at/cm2 and 5.1±4.1×1010 at/cm2 for #60179 and #60476, respectively. For 40Ca, SW fluencies of 1.39±0.70×1011 at/cm2 in #60179 and 3.6±2.5×1013 at/cm2 in #60476 were measured. Thus, only one element in each sample showed reasonable agreement with the expected values, Ca in #60179 and Cr in #60476. However the cleaning procedures applied to these samples were different: #60179 was only Megasonicated in ultra-pure water, while #60476 was subjected to longer Megasonication and an RCA cleaning procedure involving multiple rinsing steps with acid solutions. It is apparent that the surface contamination and cleaning procedures influenced the results of our measurements. We will present these experimental results and discuss procedures - including improved sample cleaning, dual-beam high resolution sputter depth profiling from front and back sides of the sample, and modeling of near-surface impurity transport - aimed at improving the accuracy of determination of elemental abundances by ion sputtering based analytical methods. This work is supported by NASA through a grant NNH08AH761 and by UChicago Argonne, LLC, under contract No. DE-AC02-06CH11357.
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Perfluoroalkyl and polyfluoroalkyl substances in consumer products.
Kotthoff, Matthias; Müller, Josef; Jürling, Heinrich; Schlummer, Martin; Fiedler, Dominik
2015-10-01
Perfluoroalkyl and polyfluoroalkyl substances (PFAS) are used in a wide range of products of all day life. Due to their toxicological potential, an emerging focus is directed towards their exposure to humans. This study investigated the PFAS load of consumer products in a broad perspective. Perfluoroalkyl sulfonic acids (C4, C6-C8, C10-PFSA), carboxylic acids (C4-C14-PFCA) and fluorotelomer alcohols (4:2, 6:2; 8:2 and 10:2 FTOH) were analysed in 115 random samples of consumer products including textiles (outdoor materials), carpets, cleaning and impregnating agents, leather samples, baking and sandwich papers, paper baking forms and ski waxes. PFCA and PFSA were analysed by HPLC-MS/MS, whereas FTOH were detected by GC/CI-MS. Consumer products such as cleaning agents or some baking and sandwich papers show low or negligible PFSA and PFCA contents. On the other hand, high PFAS levels were identified in ski waxes (up to about 2000 μg/kg PFOA), leather samples (up to about 200 μg/kg PFBA and 120 μg/kg PFBS), outdoor textiles (up to 19 μg/m(2) PFOA) and some other baking papers (up to 15 μg/m(2) PFOA). Moreover, some test samples like carpet and leather samples and outdoor materials exceeded the EU regulatory threshold value for PFOS (1 μg/m(2)). A diverse mixture of PFASs can be found in consumer products for all fields of daily use in varying concentrations. This study proves the importance of screening and monitoring of consumer products for PFAS loads and the necessity for an action to regulate the use of PFASs, especially PFOA, in consumer products.
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The purpose of the SOP is to define the particular steps involved in cleaning the electronic data generated from data entry of the 24 Hour Food Diary. The procedure was developed to use during the Arizona NHEXAS project and the "Border" study. Keywords: data; cleaning; 24 hour ...
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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.
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Phase stability of zirconium oxide films during focused ion beam milling
NASA Astrophysics Data System (ADS)
Baxter, Felicity; Garner, Alistair; Topping, Matthew; Hulme, Helen; Preuss, Michael; Frankel, Philipp
2018-06-01
Focused ion beam (FIB) is a widely used technique for preparation of electron transparent samples and so it is vital to understand the potential for introduction of FIB-induced microstructural artefacts. The bombardment of both Xe+ and Ga+ ions is observed to cause extensive monoclinic to tetragonal phase transformation in ZrO2 corrosion films, however, this effect is diminished with reduced energy and is not observed below 5 KeV. This study emphasises the importance of careful FIB sample preparation with a low energy cleaning step, and also gives insight into the stabilisation mechanism of the tetragonal phase during oxidation.
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Assessing airborne aflatoxin B1 during on-farm grain handling activities.
Selim, M I; Juchems, A M; Popendorf, W
1998-04-01
The presence of aflatoxin in corn and corn dust during relatively normal years and the increased risk of Aspergillus flavus infestation during drought conditions suggest that airborne agricultural exposures should be of considerable concern. Liquid extraction, thin layer chromatography, and high pressure liquid chromatography were used for the analysis of aflatoxin B1 in grain dust and bulk corn samples. A total of 24 samples of airborne dust were collected from 8 farms during harvest, 22 samples from 9 farms during animal feeding, and 14 sets of Andersen samples from 11 farms during bin cleaning. A total of 14 samples of settled dust and 18 samples of bulk corn were also collected and analyzed. The airborne concentration of aflatoxin B1 found in dust collected during harvest and grain unloading ranged from 0.04 to 92 ng/m3. Higher levels of aflatoxin B1 were found in the airborne dust samples collected from enclosed animal feeding buildings (5-421 ng/m3) and during bin cleaning (124-4849 ng/m3). Aflatoxin B1 up to 5100 ng/g were detected in settled dust collected from an enclosed animal feeding building; however, no apparent correlation was found between the airborne concentration of aflatoxin B1 and its concentration in settled dust or bulk corn. The data demonstrate that farmers and farm workers may be exposed to potentially hazardous concentrations of aflatoxin B1, particularly during bin cleaning and animal feeding in enclosed buildings.
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A simple and efficient HPLC method for benznidazole dosage in human breast milk.
Marson, María E; Padró, Juan M; Reta, Mario R; Altcheh, Jaime; García-Bournissen, Facundo; Mastrantonio, Guido
2013-08-01
Due to migration, Chagas disease is a significant public health problem in Latin America, and in other nonendemic regions. The 2 drugs currently available for the treatment, nifurtimox and benznidazole (BNZ), are associated with a high risk of toxicity in therapeutic doses. Excretion of drug into human breast milk is a potential source of unwanted exposure and pharmacologic effects in the nursing infant. However, this phenomenon was not evaluated until now, and measurement techniques for both drugs in milk were not developed. In this work, we described the development of a simple and fast method to quantify BNZ in human milk using a pretreatment that involves acid protein precipitation followed by tandem microfiltration, and reverse phase high-performance liquid chromatography/ultraviolet analysis. It is simple because it takes only 3 steps to obtain a clean extracted solution that is ready to inject into the high-performance liquid chromatography equipment. It is fast because a complete analysis of a sample takes only 36 minutes. Although the human breast milk composition is very variable, and lipids are one of the most difficult compounds to clean up on a milk sample, the procedure has proven to be robust and sensitive with a limit of detection of 0.3 μg/mL and quantization of 0.9 μg/mL. Despite a 70% recovery value, which could be considered a relatively low result, this recovery is reproducible (coefficient of variation <10%) and the analytical response under the linear range is very good (r = 0.9969 adjusted). Real samples of human breast milk from patients in treatment with BNZ were dosed to support the validation process of the method. The method described is fast, specific, accurate, precise, and sufficiently sensitive in the clinical context for the quantification of BNZ in human milk. For all these reasons, it is suitable for clinical risk evaluation studies.
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NASA Astrophysics Data System (ADS)
Bagheri, H.; Aliofkhazraei, M.; Forooshani, H. Mojiri; Rouhaghdam, A. Sabour
2018-04-01
In the present study, two-stage process for the fabrication of superhydrophobic Ni-Cu-TiO2 nanocomposite coatings on the copper substrate has been introduced. Surface modification was performed on the electrodeposited coatings by myristic acid-ethanol solution to achieve superhydrophobicity. Additionally, in order to further study the roughness effect, instead of addition of copper ions in electrodeposition bath, three substrates were roughened by electrochemical etching method. Water repellency properties were studied through measurement of static and dynamic contact angles, and performing bouncing test, self-cleaning and water-jet evaluation. The samples were electrodeposited in various current densities, and the highest corrosion resistance and water repellency properties were obtained for the sample which was electrodeposited in two consecutive steps and modified by a fatty acid called myristic acid (which significantly reduces surface energy of the coating). The highest water contact angle (161°) and the lowest contact angle hysteresis (3°) were obtained for the sample which was coated by 10 mA/cm2 (144 min) and 20 mA/cm2 (18 min), respectively. Since this approach does not require any sophisticated equipment and materials, it shows promising future in the fabrication of superhydrophobic coatings.
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To support risk assessment efforts, a comparative study was designed to provide understanding of the toxicity of different types of fibers encountered in EPA clean-up efforts. Physico-chemical properties, and consequentially toxicity, are likely to be different among various fib...
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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...
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Goscinny, Séverine; Hanot, Vincent; Trabelsi, Hasna; Van Loco, Joris
2014-01-01
2-Methylimidazole, 4-methylimidazole (2-MI and 4-MI), 2-acetyl-4-(1,2,3,4-tetrahydroxybutyl) imidazole (THI) and 5-hydroxymethylfurfural (5-HMF) are neo-formed compounds generated during the manufacture of caramel colours and are transferred to the processed food. These contaminants are known to have a toxicological profile that may pose health risks. Hence, to characterise THI, 2- and 4-MI and 5-HMF levels in liquid foods, an ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and sample preparation was divided into two analytical strategies depending on the concentration range expected in the type of foods targeted. For the determination of the imidazole substitutes (THI, 2- and 4-MI), a sample enrichment and clean-up step by strong cation solid-phase extraction was developed. This method is capable of quantifying over a range of 5 ng ml⁻¹ (LOQ) to 500 ng ml⁻¹ with recoveries of 75.4-112.4% and RSDs of 1.5-15%. For determination of 5-HMF, a standard addition method was applied covering the linear range of 0.25-30 µg ml⁻¹ with RSDs from 2.8% (for intraday precision) to 9.2% (for intermediate precision). The validated analytical methods were applied to 28 liquid food samples purchased from local markets. THI was found only in the beer samples at levels up to 141.2 ng ml⁻¹. For 2-MI, non-quantifiable traces were observed for all samples, while 4-MI was observed in all samples with large concentration variations (from < LOQ to 563.9 ng ml⁻¹). 5-HMF was found at expected concentrations, except for a sherry vinegar sample (113 µg ml⁻¹), which required a high level of dilution before following the standard addition protocol.
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April 2016 Pacific Southwest Newsletter
EPA Pacific Southwest Newsletter for April 2016: University of Arizona Reduces Food Waste, Cleaning Up Underground Fuel Tanks in Fresno, The Argonaut Mine, Ensuring Clean Water in Nevada,Cleaning Up Groundwater in Whittier, California, and more!
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Cleaning and activation of beryllium-copper electron multiplier dynodes.
NASA Technical Reports Server (NTRS)
Pongratz, M. B.
1972-01-01
Description of a cleaning and activation procedure followed in preparing beryllium-copper dynodes for electron multipliers used in sounding-rocket experiments to detect auroral electrons. The initial degreasing step involved a 5-min bath in trichloroethylene in an ultrasonic cleaner. This was followed by an ultrasonic rinse in methanol and by a two-step acid pickling treatment to remove the oxides. Additional rinsing in water and methanol was followed by activation in a stainless-steel RF induction oven.
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Particulate Removal Using a CO2 Composite Spray Cleaning System
NASA Technical Reports Server (NTRS)
Chen, Nicole; Lin, Ying; Jackson, David; Chung, Shirley
2016-01-01
The Planetary Protection surface cleanliness requirements for potential Mars Sample Return hardware that would come in contact with Martian samples may be stricter than previous missions. The Jet Propulsion Laboratory has developed a new technology that will enable us to remove sub-micron size particles from critical hardware surfaces. A hand-held CO2 composite cleaning system was tested to verify its cleaning capabilities. This convenient, portable device can be used in cleanrooms for cleaning after rework or during spacecraft integration and assembly. It is environmentally safe and easy to use. This cleaning concept has the potential to be further developed into a robotic cleaning device on a Mars Lander to be used to clean sample acquisition or sample handling devices in situ. Contaminants of known sizes and concentrations, such as fluorescent microspheres and spores were deposited on common spacecraft material surfaces. The cleaning efficiency results will be presented and discussed.
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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.
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Schulz, H; Albroscheit, G
1988-06-17
Rapid and reliable methods are presented for the characterization of biologically active and/or characteristic constituents in aqueous extracts of Hamamelis virginiana, Matricaria chamomilla, Achillea millefolium, Thymus vulgaris, Althaea officinalis and Cinchonia spp. Prior to high-performance liquid chromatographic (HPLC) separation a clean-up step was performed using a solid-phase extraction system. The purified extracts were analysed by HPLC coupled with a diode-array detector and a fluorescence detector. In some instances, previously unreported components of the aqueous plant extracts were found.
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1986-01-31
and 4% diatomaceous earth (binder). Modified EPA Method 5 Sampling Train F The modified EPA Method 5 sampling train used was similar to the one...the fiber glass filter paper were taken by the Amberlite XAD-2. The XAD-2 is a porous polymer adsorbent used to sample organic vapors in effluents...from different kinds of combustion processes. Although a careful clean-up procedure was taken to wash the adsorbents before using, the polymer may still
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Fontana, Ariel R; Bottini, Rubén
2014-05-16
In this work, a reliable, simple, fast, inexpensive and robust sample preparation approach for the determination of multiclass polyphenols in wine samples is proposed. The polyphenols selected for this work were gallic acid, (+)-catechin, (-)-epicatechin, caffeic acid, syringic acid, coumaric acid, ferulic acid, trans-resveratrol, quercetin and cinnamic acid. The method is based on QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction technique coupled with dispersive solid-phase extraction (d-SPE) clean-up. Under optimized conditions, the analytes were extracted from 5mL wine samples (previously acidified with 1% formic acid) using 2.5mL acetonitrile. For phase separation, 1.5g NaCl and 4g anhydrous MgSO4 were added. Then, a 1mL aliquot of the partitioned supernatant was cleaned-up using d-SPE with a combination of 150mg CaCl2, 50mg primary-secondary amine (PSA) and 50mgC18 as sorbents. A 250μL aliquot of the obtained cleaned extract was concentrated to dryness and taken up with the initial mobile phase previous to liquid chromatography-multi-wavelength detection (LC-MWD). The proposed method provided limits of detection (LODs) ranging from 0.004 to 0.079μgmL(-1) and an inter-day variability below 12% RSD for all analytes in red and white wine samples. Considering external calibration (red wines) and matrix-matched calibration (white wines) as quantification techniques, the overall recoveries (accuracy) of the method ranged between 75.0% and 119.6% for red and white wine samples, respectively. The developed method was applied for the determination of polyphenols in 10 wines produced in Argentina. Nine phenolic compounds were determined, at concentrations above detectable levels in the method. The maximum concentrations corresponded to (-)-epicatechin in white wines, while gallic acid and (+)-catechin were the most abundant in red wines. Copyright © 2014 Elsevier B.V. All rights reserved.
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Testing the cleaning effectiveness of new ecological aqueous dispersions applied on old icons
NASA Astrophysics Data System (ADS)
Vasilache, Viorica; Sandu, Irina Crina Anca; Pruteanu, Silvea; Caldeira, Ana Teresa; Simionescu, Atena Elena; Sandu, Ion
2016-03-01
Adherent deposits are very aggressive towards ancient heritage paintings since they affect the varnish and the painting's layers, sometimes reaching the preparative layers. The biggest problem to the restorer is their removal without affecting the patina, the transparent varnish (well preserved) and fine colour glazes made during painting. Therefore, their removal requires preliminary cleaning tests that allow the optimization of the cleaning system composition that is going to be used. The study was focused on organic natural systems, as colourless supernatants, some of them used during ages, but insufficiently studied. The paper presents an evaluation of the effectiveness of cleaning varnished icons of the nineteenth century, with complex conservation cases using supernatants derived from aqueous dispersions extracted from vegetables and dry indigenous herbal infusions. Best results, after six consecutive cleaning steps, on tempera old icon was obtained for a mixture made of mature white onion juice + extract of Soapwort flowers + corn silk tea + acacia tea. As a best result after just one cleaning step was obtained for a quaternary mixture composed from mature white onion juice + mature carrot juice + corn silk tea + aqueous extract of Soapwort flowers.
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NASA Astrophysics Data System (ADS)
Bobzin, K.; Öte, M.; Wiesner, S.
2017-03-01
The quality of brazed joints is determined by different factors such as the atmosphere and the parameters during brazing as well as the condition of the brazing surfaces. Residues of lubricants used during machining of the components and the subsequent cleaning processes can contaminate the faying surfaces and can hence influence the flow ability of the molten filler metals. Besides their influence on the filler metal flow, the residues can result in the formation of carbonic phases in the joint leading to a possible reduction of the corrosion resistance and the mechanical properties. The first step of the current study with the aim of avoiding these defects is to identify the influence of critical contaminations and cleaning methods on the quality of the brazed joints. In a first step, contaminations on AISI304 and Inconel alloy 625 due to different cooling lubricants and the effect of several cleaning methods, in particular plasma cleaning, have been investigated. Information about the surface energy of contaminated and cleaned surfaces was gained by measuring contact angle of testing fluids. Additionally, the lubricants and the resulting contamination products have been analyzed considering the influence of a heat treatment.
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Azbel, Lyuba; Rozanova, Julia; Michels, Ingo; Altice, Frederick L; Stöver, Heino
2017-07-10
Kyrgyzstan, where HIV is concentrated in prisons and driven by injection drug use, provides a prison-based methadone maintenance therapy program as well as abstinence-oriented therapeutic community based on the 12-step model called the "Clean Zone." We aimed to qualitatively assess how prisoners navigate between these treatment options to understand the persistence of the Clean Zone despite a lack of evidence to support its effectiveness in treating opioid use disorders. We conducted an analysis of policy documents and over 60 h of participant observation in February 2016, which included focus groups with a convenience sample of 20 therapeutic community staff members, 110 prisoners across three male and one female prisons, and qualitative interviews with two former Clean Zone participants. Field notes containing verbatim quotes from participants were analyzed through iterative reading and discussion to understand how participants generally perceive the program, barriers to entry and retention, and implications for future treatment within prisons. Our analyses discerned three themes: pride in the mission of the Clean Zone, idealism regarding addiction treatment outcomes against all odds, and the demonization of methadone. Despite low enrollment and lack of an evidence base, the therapeutic community is buttressed by the strong support of the prison administration and its clients as an "ordered" alternative to what is seen as chaotic life outside of the Clean Zone. The lack of services for Clean Zone patients after release likely contributes to high rates of relapse to drug use. The Clean Zone would benefit from integration of stabilized methadone patients combined with a post-release program.
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Végvári, Akos; Magnusson, Mattias; Wallman, Lars; Ekström, Simon; Bolmsjö, Gunnar; Nilsson, Johan; Miliotis, Tasso; Ostling, Jörgen; Kjellström, Sven; Ottervald, Jan; Franzén, Bo; Hultberg, Hans; Marko-Varga, György; Laurell, Thomas
2008-06-01
As much attention has devoted to the proteome research during the last few years, biomarker discovery has become an increasingly hot area, potentially enabling the development of new assays for diagnosis and prognosis of severe diseases. This is the field of research interest where efforts originating from both academic and industrial groups should jointly work on solutions. In this paper, we would like to demonstrate the fruitful combination of both research domains where the scientific crossroads sprout fresh ideas from the basic research domain and how these are refined and tethered to industrial standards. We will present an approach that is based on novel microfluidic devices, utilizing their benefits in processing small-volume samples. Our biomarker discovery strategy, built around this platform, involves optimized samples processing (based on SPE and sample enrichment) and fast MALDI-MS readout. The identification of novel biomarkers at low-abundance level has been achieved by the utilization of a miniaturized sample handling platform, which offers clean-up and enrichment of proteins in one step. Complete automation has been realized in the form of a unique robotic instrumentation that is able to extract and transfer 96 samples onto standard MALDI target plates with high throughput. The developed platform was operated with a 60 sample turnaround per hour allowing sensitivities in femtomol regions of medium- and low-abundant target proteins from clinical studies on samples of multiple sclerosis and gastroesophageal reflux disease. Several proteins have been identified as new biomarkers from cerebrospinal fluid and esophagus epithelial cells.
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Robst, John; Scheeringa, Michael S.; Cohen, Judith A.; Wang, Wei; Murphy, Tanya K.; Tolin, David F.; Storch, Eric A.
2013-01-01
This pilot study explored the preliminary efficacy, parent acceptability and economic cost of delivering Step One within Stepped Care Trauma-Focused Cognitive Behavioral Therapy (SC-TF-CBT). Nine young children ages 3–6 years and their parents participated in SC-TF-CBT. Eighty-three percent (5/6) of the children who completed Step One treatment and 55.6 % (5/9) of the intent-to-treat sample responded to Step One. One case relapsed at post-assessment. Treatment gains were maintained at 3-month follow-up. Generally, parents found Step One to be acceptable and were satisfied with treatment. At 3-month follow-up, the cost per unit improvement for posttraumatic stress symptoms and severity ranged from $27.65 to $131.33 for the responders and from $36.12 to $208.11 for the intent-to-treat sample. Further research on stepped care for young children is warranted to examine if this approach is more efficient, accessible and cost-effective than traditional therapy. PMID:23584728
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Salloum, Alison; Robst, John; Scheeringa, Michael S; Cohen, Judith A; Wang, Wei; Murphy, Tanya K; Tolin, David F; Storch, Eric A
2014-02-01
This pilot study explored the preliminary efficacy, parent acceptability and economic cost of delivering Step One within Stepped Care Trauma-Focused Cognitive Behavioral Therapy (SC-TF-CBT). Nine young children ages 3-6 years and their parents participated in SC-TF-CBT. Eighty-three percent (5/6) of the children who completed Step One treatment and 55.6 % (5/9) of the intent-to-treat sample responded to Step One. One case relapsed at post-assessment. Treatment gains were maintained at 3-month follow-up. Generally, parents found Step One to be acceptable and were satisfied with treatment. At 3-month follow-up, the cost per unit improvement for posttraumatic stress symptoms and severity ranged from $27.65 to $131.33 for the responders and from $36.12 to $208.11 for the intent-to-treat sample. Further research on stepped care for young children is warranted to examine if this approach is more efficient, accessible and cost-effective than traditional therapy.
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High throughput laser texturing of super-hydrophobic surfaces on steel
NASA Astrophysics Data System (ADS)
Gemini, Laura; Faucon, Marc; Romoli, Luca; Kling, Rainer
2017-03-01
Super-hydrophobic surfaces are nowadays of primary interest in several application fields, as for de-icing devices in the automotive and aerospace industries. In this context, laser surface texturing has widely demonstrated to be an easy one-step method to produce super-hydrophobic surfaces on several materials. In this work, a high average power (up to 40W), high repetition-rate (up to 1MHz), femtosecond infrared laser was employed to produce super-hydrophobic surfaces on 316L steel. The set of process and laser parameters for which the super-hydrophobic behavior is optimized, was obtained by varying the laser energy and repetition rate. The morphology of the textured surfaces was firstly analyzed by SEM and confocal microscope analyses. The contact angle was measured over time in order to investigate the effect of air environment on the hydrophobic properties and define the period of time necessary for the super-hydrophobic properties to stabilize. An investigation on the effect of after-processing cleaning solvents on the CA evolution was carried to assess the influence of the after-processing sample handling on the CA evaluation. Results show that the highest values of contact angle, that is the best hydrophobic behavior, are obtained at high repetition rate and low energy, this way opening up a promising scenario in terms of upscaling for reducing the overall process takt-time.
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Bustamante, Julen; Navarro, Patricia; Arana, Gorka; de Diego, Alberto; Madariaga, Juan Manuel
2013-09-30
A new procedure based on ultrasound assisted dialysis (UAD) for the simultaneous and quantitative extraction of a wide number of persistent organic pollutants (POPs) such as polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) or some other organochlorinated pesticides (OCPs) contained in semi-permeable membrane devices (SPMDs) has been developed. This extraction technique combines the advantages of the organic solvent dialysis (OSD) and the speed of the ultrasound assisted extraction. The extraction was performed in an ultrasound bath for 32 min placing the SPMD in a glass flask covered with 80 mL of hexane. This set-up is able to extract simultaneously up to 8 samples. The proposed method entails good repeatabilities (RSD 2-13%) and recoveries (around 100% for almost every analyte). Limits of detection were at ng SPMD(-1) level and enough for the determination of the target analytes in a slightly polluted aquatic environment, as it was tested by successfully comparing the OSD to the proposed methodology. Therefore, the results obtained show that the UAD can be a good alternative for the extraction of POPs in SPMDs as it requires short extraction times and solvent volumes, and provides a cleaner extract for the subsequent clean-up step. Moreover, it fits better than the OSD to the general requirements of Green Chemistry. Copyright © 2013 Elsevier B.V. All rights reserved.
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Etching of Cr tips for scanning tunneling microscopy of cleavable oxides
DOE Office of Scientific and Technical Information (OSTI.GOV)
Huang, Dennis; Liu, Stephen; Zeljkovic, Ilija
Here, we report a detailed three-step roadmap for the fabrication and characterization of bulk Cr tips for spin-polarized scanning tunneling microscopy. Our strategy uniquely circumvents the need for ultra-high vacuum preparation of clean surfaces or films. First, we demonstrate the role of ex situ electrochemical etch parameters on Cr tip apex geometry, using scanning electron micrographs of over 70 etched tips. Second, we describe the suitability of the in situ cleaved surface of the layered antiferromagnet La 1.4Sr 1.6Mn 2O 7 to evaluate the spin characteristics of the Cr tip, replacing the ultra-high vacuum-prepared test samples that have been usedmore » in prior studies. Third, we outline a statistical algorithm that can effectively delineate closely spaced or irregular cleaved step edges, to maximize the accuracy of step height and spin-polarization measurements.« less
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Etching of Cr tips for scanning tunneling microscopy of cleavable oxides
Huang, Dennis; Liu, Stephen; Zeljkovic, Ilija; ...
2017-02-21
Here, we report a detailed three-step roadmap for the fabrication and characterization of bulk Cr tips for spin-polarized scanning tunneling microscopy. Our strategy uniquely circumvents the need for ultra-high vacuum preparation of clean surfaces or films. First, we demonstrate the role of ex situ electrochemical etch parameters on Cr tip apex geometry, using scanning electron micrographs of over 70 etched tips. Second, we describe the suitability of the in situ cleaved surface of the layered antiferromagnet La 1.4Sr 1.6Mn 2O 7 to evaluate the spin characteristics of the Cr tip, replacing the ultra-high vacuum-prepared test samples that have been usedmore » in prior studies. Third, we outline a statistical algorithm that can effectively delineate closely spaced or irregular cleaved step edges, to maximize the accuracy of step height and spin-polarization measurements.« less
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Tank 12H Acidic Chemical Cleaning Sample Analysis And Material Balance
DOE Office of Scientific and Technical Information (OSTI.GOV)
Martino, C. J.; Reboul, S. H.; Wiersma, B. J.
2013-11-08
A process of Bulk Oxalic Acid (BOA) chemical cleaning was performed for Tank 12H during June and July of 2013 to remove all or a portion of the approximately 4400 gallon sludge heel. Three strikes of oxalic acid (nominally 4 wt% or 2 wt%) were used at 55°C and tank volumes of 96- to 140-thousand gallons. This report details the sample analysis of a scrape sample taken prior to BOA cleaning and dip samples taken during BOA cleaning. It also documents a rudimentary material balance for the Tank 12H cleaning results.
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Fluidized-Bed Cleaning of Silicon Particles
NASA Technical Reports Server (NTRS)
Rohatgi, Naresh K.; Hsu, George C.
1987-01-01
Fluidized-bed chemical cleaning process developed to remove metallic impurities from small silicon particles. Particles (250 micrometer in size) utilized as seed material in silane pyrolysis process for production of 1-mm-size silicon. Product silicon (1 mm in size) used as raw material for fabrication of solar cells and other semiconductor devices. Principal cleaning step is wash in mixture of hydrochloric and nitric acids, leaching out metals and carrying them away as soluble chlorides. Particles fluidized by cleaning solution to assure good mixing and uniform wetting.
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Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M
2015-02-06
A method using direct sample introduction (DSI) coupled to gas chromatography-mass spectrometry (GC-MS) is developed for the determination of six phthalate esters (dimethyl, diethyl, dibutyl, butylbenzyl, diethylhexyl and dioctyl phthalate) in cleaning products. The different variables involved in the DSI step, including venting time and temperature, vaporisation time and temperature, injector heating temperature and gas flow rate and pressure, were evaluated and optimised using Taguchi orthogonal arrays. The proposed method, using calibration against methanolic standards, showed good linearity in the 0.05-15 μg g(-1) range and good repeatability, with RSD values ranging from 3.5% to 5.7%. Quantification limits between 0.010 and 0.041 μg g(-1), depending on the compound, were attained, while recovery assays provided values from 83% to 115%. Twenty-seven cleaning products were analysed using the DSI-GC-MS method, being four phthalates (dimethyl, diethyl, dibutyl and diethylhexyl phthalate) found in fourteen of them at concentration levels in the 0.1-21 μg g(-1) range. Compared with the most common GC injection technique, which uses the split/splitless injector, the proposed DSI procedure provided larger peak areas and lower detection limits, as result of the greater injected volume and reduction in noise. Copyright © 2014 Elsevier B.V. All rights reserved.
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Gross, J M; Nascimento, G G; Araújo, V C; Bönecker, Mjs; Furuse, C
2016-04-01
This study aimed to investigate, in vitro, possible alterations on mini-implants surface after retrieval and if the cleaning process and sterilization can predispose damages. Two commercial mini-implants were tested for deformations after drilling and removing in artificial bone four times. Samples were analyzed by scanning electron microscopy, and surface alterations verified through thread and pitches deformation. To alterations caused by insertion/removal and the cleaning process and sterilization were verified in different procedures: Insertions and sterilization, only insertions, and only sterilization. Photomicrographs were analyzed in order to compare the surface characteristics. Head deformation was verified qualitatively. For a quantitative analysis, distances between threads were measured across the active part of the mini-implants. No deformation was observed in both groups. The cleaning and sterilization processes did not provoke alteration in both groups. Nevertheless, the presence of synthetic bone was noted in some samples. The mean distances between implant threads were similar after all steps in all regions in both groups. The results suggest that the tested mini-implants can be retrieved without damage of its surface after four cycles of insertion, removal, and sterilization. Orthodontic mini-implant, Redrilling, Sterilization. Mini-implants can be retrieved without damage to its surface after four cycles of insertion, removal, and sterilization in the same patient without representing a biological concern.
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40 CFR 35.909 - Step 2+3 grants.
Code of Federal Regulations, 2014 CFR
2014-07-01
... ASSISTANCE Grants for Construction of Treatment Works-Clean Water Act § 35.909 Step 2+3 grants. (a) Authority... design (step 2) and construction (step 3) of a waste water treatment works. (b) Limitations. The Regional... Water and Waste Management finds to have unusually high costs of construction, the Regional...
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40 CFR 35.909 - Step 2+3 grants.
Code of Federal Regulations, 2013 CFR
2013-07-01
... ASSISTANCE Grants for Construction of Treatment Works-Clean Water Act § 35.909 Step 2+3 grants. (a) Authority... design (step 2) and construction (step 3) of a waste water treatment works. (b) Limitations. The Regional... Water and Waste Management finds to have unusually high costs of construction, the Regional...
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40 CFR 35.909 - Step 2+3 grants.
Code of Federal Regulations, 2012 CFR
2012-07-01
... ASSISTANCE Grants for Construction of Treatment Works-Clean Water Act § 35.909 Step 2+3 grants. (a) Authority... design (step 2) and construction (step 3) of a waste water treatment works. (b) Limitations. The Regional... Water and Waste Management finds to have unusually high costs of construction, the Regional...
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40 CFR 35.909 - Step 2+3 grants.
Code of Federal Regulations, 2011 CFR
2011-07-01
... design (step 2) and construction (step 3) of a waste water treatment works. (b) Limitations. The Regional... ASSISTANCE Grants for Construction of Treatment Works-Clean Water Act § 35.909 Step 2+3 grants. (a) Authority... Water and Waste Management finds to have unusually high costs of construction, the Regional...
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Characterization of oily sludge from a Tehran oil refinery.
Heidarzadeh, Nima; Gitipour, Saeid; Abdoli, Mohammad Ali
2010-10-01
In this study, oily sludge samples generated from a Tehran oil refinery (Pond I) were evaluated for their contamination levels and to propose an adequate remediation technique for the wastes. A simple, random, sampling method was used to collect the samples. The samples were analyzed to measure Total petroleum hydrocarbon (TPH), polyaromatic hydrocarbon (PAH) and heavy metal concentrations in the sludge. Statistical analysis showed that seven samples were adequate to assess the sludge with respect to TPH analyses. The mean concentration of TPHs in the samples was 265,600 mg kg⁻¹. A composite sample prepared from a mix of the seven samples was used to determine the sludge's additional characteristics. Composite sample analysis showed that there were no detectable amounts of PAHs in the sludge. In addition, mean concentrations of the selected heavy metals Ni, Pb, Cd and Zn were 2700, 850, 100, 6100 mg kg⁻¹, respectively. To assess the sludge contamination level, the results from the analysis above were compared with soil clean-up levels. Due to a lack of national standards for soil clean-up levels in Iran, sludge pollutant concentrations were compared with standards set in developed countries. According to these standards, the sludge was highly polluted with petroleum hydrocarbons. The results indicated that incineration, biological treatment and solidification/stabilization treatments would be the most appropriate methods for treatment of the sludges. In the case of solidification/stabilization, due to the high organic content of the sludge, it is recommended to use organophilic clays prior to treatment of the wastes.
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Atomic hydrogen cleaning of EUV multilayer optics
NASA Astrophysics Data System (ADS)
Graham, Samuel, Jr.; Steinhaus, Charles A.; Clift, W. Miles; Klebanoff, Leonard E.; Bajt, Sasa
2003-06-01
Recent studies have been conducted to investigate the use of atomic hydrogen as an in-situ contamination removal method for EUV optics. In these experiments, a commercial source was used to produce atomic hydrogen by thermal dissociation of molecular hydrogen using a hot filament. Samples for these experiments consisted of silicon wafers coated with sputtered carbon, Mo/Si optics with EUV-induced carbon, and bare Si-capped and Ru-B4C-capped Mo/Si optics. Samples were exposed to an atomic hydrogen source at a distance of 200 - 500 mm downstream and angles between 0-90° with respect to the source. Carbon removal rates and optic oxidation rates were measured using Auger electron spectroscopy depth profiling. In addition, at-wavelength peak reflectance (13.4 nm) was measured using the EUV reflectometer at the Advanced Light Source. Data from these experiments show carbon removal rates up to 20 Ê/hr for sputtered carbon and 40 Ê/hr for EUV deposited carbon at a distance of 200 mm downstream. The cleaning rate was also observed to be a strong function of distance and angular position. Experiments have also shown that the carbon etch rate can be increased by a factor of 4 by channeling atomic hydrogen through quartz tubes in order to direct the atomic hydrogen to the optic surface. Atomic hydrogen exposures of bare optic samples show a small risk in reflectivity degradation after extended periods. Extended exposures (up to 20 hours) of bare Si-capped Mo/Si optics show a 1.2% loss (absolute) in reflectivity while the Ru-B4C-capped Mo/Si optics show a loss on the order of 0.5%. In order to investigate the source of this reflectivity degradation, optic samples were exposed to atomic deuterium and analyzed using low energy ion scattering direct recoil spectroscopy to determine any reactions of the hydrogen with the multilayer stack. Overall, the results show that the risk of over-etching with atomic hydrogen is much less than previous studies using RF discharge cleaning while providing cleaning rates suitable for EUV lithography operations.
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Atomic hydrogen cleaning of EUV multilayer optics
NASA Astrophysics Data System (ADS)
Graham, Samuel, Jr.; Steinhaus, Charles A.; Clift, W. Miles; Klebanoff, Leonard E.; Bajt, Sasa
2003-06-01
Recent studies have been conducted to investigate the use of atomic hydrogen as an in-situ contamination removal method for EUV optics. In these experiments, a commercial source was used to produce atomic hydrogen by thermal dissociation of molecular hydrogen using a hot filament. Samples for these experiments consisted of silicon wafers coated with sputtered carbon, Mo/Si optics with EUV-induced carbon, and bare Si-capped and Ru-B4C-capped Mo/Si optics. Samples were exposed to an atomic hydrogen source at a distance of 200 - 500 mm downstream and angles between 0-90° with respect to the source. Carbon removal rates and optic oxidation rates were measured using Auger electron spectroscopy depth profiling. In addition, at-wavelength peak reflectance (13.4 nm) was measured using the EUV reflectometer at the Advanced Light Source. Data from these experiments show carbon removal rates up to 20 Å/hr for sputtered carbon and 40 Å/hr for EUV deposited carbon at a distance of 200 mm downstream. The cleaning rate was also observed to be a strong function of distance and angular position. Experiments have also shown that the carbon etch rate can be increased by a factor of 4 by channeling atomic hydrogen through quartz tubes in order to direct the atomic hydrogen to the optic surface. Atomic hydrogen exposures of bare optic samples show a small risk in reflectivity degradation after extended periods. Extended exposures (up to 20 hours) of bare Si-capped Mo/Si optics show a 1.2% loss (absolute) in reflectivity while the Ru-B4C-capped Mo/Si optics show a loss on the order of 0.5%. In order to investigate the source of this reflectivity degradation, optic samples were exposed to atomic deuterium and analyzed using low energy ion scattering direct recoil spectroscopy to determine any reactions of the hydrogen with the multilayer stack. Overall, the results show that the risk of over-etching with atomic hydrogen is much less than previous studies using RF discharge cleaning while providing cleaning rates suitable for EUV lithography operations.
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Abrasive blast cleaning method for the renewal of worn-out acceleration tubes
NASA Astrophysics Data System (ADS)
Bartha, L.; Koltay, E.; Mórik, Gy.
1996-04-01
The degradation of the electrical properties of acceleration tubes emerging with performance time is known to be assigned mainly to impurities and surface breakdown tracks appearing on the inner surface of the insulators. Consequently, a radical treatment for removing the surface layer may result in a renewal of the tube. An abrasive blast cleaning procedure has been used on a set of worn-out acceleration tube units. The cleaned tube exhibited its original electrical characteristics and it has been used for more than 4000 h of operation up to the maximum rated voltage of our 5 MV electrostatic accelerator without any observable degradation. XRF and PIXE analytical measurements performed on used and blast-treated insulators as well as on electrode and pump oil samples reveal the contribution of elementary processes in the acceleration tube to the ageing of the tube and indicate the effectness of the blasting process used for the re-establishment of clean surface conditions.
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Composition, mineral profiles and characterization of the ash component in 12 algae samples
USDA-ARS?s Scientific Manuscript database
Algae have been used as food, feed, fertilizer, and lately as an attractive biomass for renewable energy. Key advantages of algae include prolific growth rates, the ability to grow on lands that are marginal for other agricultural purposes, and the ability to clean up water resources with excess nu...
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Bench-scale supercritical fluid extraction (SFE) studies were performed on soil samples obtained from a Superfund site that is contaminated with high levels of p,p,-DDT, p,p,-DDD, p,p,-DDE, toxaphene and hexachlorocyclohexane. The effectiveness of supercritical fluid extraction ...
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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...
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Cristale, Joyce; Lacorte, Silvia
2013-08-30
This study presents a multiresidue method for simultaneous extraction, clean-up and analysis of priority and emerging flame retardants in sediment, sewage sludge and dust. Studied compounds included eight polybrominated diphenyl ethers congeners, nine new brominated flame retardants and ten organophosphorus flame retardants. The analytical method was based on ultrasound-assisted extraction with ethyl acetate/cyclohexane (5:2, v/v), clean-up with Florisil cartridges and analysis by gas chromatography coupled to tandem mass spectrometry (GC-EI-MS/MS). Method development and validation protocol included spiked samples, certified reference material (for dust), and participation in an interlaboratory calibration. The method proved to be efficient and robust for extraction and determination of three families of flame retardants families in the studied solid matrices. The method was applied to river sediment, sewage sludge and dust samples, and allowed detection of 24 among the 27 studied flame retardants. Organophosphate esters, BDE-209 and decabromodiphenyl ethane were the most ubiquitous contaminants detected. Copyright © 2013 Elsevier B.V. All rights reserved.
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LC-MS/MS determination of tranexamic acid in human plasma after phospholipid clean-up.
Fabresse, Nicolas; Fall, Fanta; Etting, Isabelle; Devillier, Philippe; Alvarez, Jean-Claude; Grassin-Delyle, Stanislas
2017-07-15
Tranexamic acid is a widely used antifibrinolytic drug but its pharmacology and pharmacokinetics remains poorly understood. Owing to the recent knowledge on phospholipid-induced matrix effects during human plasma analysis, our aim was to develop a liquid chromatography-mass spectrometry method for the quantitation of tranexamic acid after efficient sample clean-up. Sample preparation consisted in phospholipid removal and protein precipitation. Hydrophilic interaction liquid chromatography was used and the detection was achieved with multiple reaction monitoring. The method was validated according to the European Medicine Agency guideline in the range 1.0-1000.0μg/mL. The performance of the method was excellent with a precision in the range 1.2-3.0%, an accuracy between 88.4 and 96.6% and a coefficient of variation of the internal standard-normalized matrix factor below 6.7%. This method is suitable for the quantification of tranexamic acid in the wide range of concentrations observed during clinical studies, with all the advantages related to phospholipid removal. Copyright © 2017 Elsevier B.V. All rights reserved.
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Brabcová, Ivana; Hlaváčková, Markéta; Satínský, Dalibor; Solich, Petr
2013-11-15
A simple and automated HPLC column-switching method with rapid sample pretreatment has been developed for quantitative determination of β-carotene in food supplements. Commercially samples of food supplements were dissolved in chloroform with help of saponification with 1M solution of sodium hydroxide in ultrasound bath. A 20-min sample dissolution/extraction step was necessary before chromatography analysis to transfer β-carotene from solid state of food supplements preparations (capsules,tablets) to chloroform solution. Sample volume - 3μL of chloroform phase was directly injected into the HPLC system. Next on-line sample clean-up was achieved on the pretreatment precolumn Chromolith Guard Cartridge RP-18e (Merck), 10×4.6mm, with a washing mobile phase (methanol:water, 92:8, (v/v)) at a flow rate of 1.5mL/min. Valve switch to analytical column was set at 2.5min in a back-flush mode. After column switching to the analytical column Ascentis Express C-18, 30×4.6mm, particle size 2.7μm (Sigma Aldrich), the separation and determination of β-carotene in food supplements was performed using a mobile phase consisting of 100% methanol, column temperature at 60°C and flow rate 1.5mL/min. The detector was set at 450nm. Under the optimum chromatographic conditions standard calibration curve was measured with good linearity - correlation coefficient for β-carotene (r(2)=0.999014; n=6) between the peak areas and concentration of β-carotene 20-200μg/mL. Accuracy of the method defined as a mean recovery was in the range 96.66-102.40%. The intraday method precision was satisfactory at three concentration levels 20, 125 and 200μg/mL and relative standard deviations were in the range 0.90-1.02%. The chromatography method has shown high sample throughput during column-switching pretreatment process and analysis in one step in short time (6min) of the whole chromatographic analysis. Copyright © 2013 Elsevier Ltd. All rights reserved.
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Dimitrakopoulos, Ioannis K; Thomaidis, Nikolaos S; Megoulas, Nikolaos C; Koupparis, Michael A
2010-05-28
This paper presents the application of ion chromatography with electrolytic eluent generation and mobile phase suppression for the direct conductimetric detection of glyphosate and its degradation product aminomethylphosphonic acid (AMPA). The compounds were separated on a Dionex AS18 anion exchange column with a 12-40 mM KOH step gradient from 9 to 9.5 min. The effect of the suppressor current intensity on the electrostatic interaction of these amphoteric compounds with the suppressor cation exchange membranes was evaluated. A suppressor current gradient technique was proposed for the limitation of peak broadening and baseline noise, in order to improve method sensitivity and detectability. It was observed that residual sample carbonates co-eluted with AMPA when a large injection loop was installed for the low level determination of both compounds in natural waters. For this reason, glyphosate was isocratically eluted using 33 mM KOH in order to decrease analysis time within 10 min and a column clean up step using 100 mM KOH was used to ensure retention time reproducibility. The developed method was applied to the analysis of drinking and natural water and it was further successfully applied to orange samples with slight modifications. Instrumental LOD for glyphosate was 0.24 microg/L, while method LOD was 0.54 microg/L for spring waters and 0.01 mg/kg for oranges using a 1000 microL direct loop injection of the sample. Intra-day and inter-day precision (as %RSD) for water samples was 4.6% and 12% at a spiking level of 2 microg/L, and the recovery ranged from 64% to 88% depending on sample conductivity. For orange samples, the inter-day precision was 1.4% at a spiking level of 4.4 mg/kg, while overall recovery was 103%. The developed method is direct, fast, sensitive and relatively inexpensive, and could be used as an ideal fast screening tool for the monitoring of glyphosate residues in water and fruit samples. Copyright 2010 Elsevier B.V. All rights reserved.
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Chemical cleaning/disinfection and ageing of organic UF membranes: a review.
Regula, C; Carretier, E; Wyart, Y; Gésan-Guiziou, G; Vincent, A; Boudot, D; Moulin, P
2014-06-01
Membrane separation processes have become a basic unit operation for process design and product development. These processes are used in a variety of separation and concentration steps, but in all cases, the membranes must be cleaned regularly to remove both organic and inorganic material deposited on the surface and/or into the membrane bulk. Cleaning/disinfection is a vital step in maintaining the permeability and selectivity of the membrane in order to get the plant to its original capacity, to minimize risks of bacteriological contamination, and to make acceptable products. For this purpose, a large number of chemical cleaning/disinfection agents are commercially available. In general, these cleaning/disinfection agents have to improve the membrane flux to a certain extent. However, they can also cause irreversible damages in membrane properties and performances over the long term. Until now, there is considerably less literature dedicated to membrane ageing than to cleaning/disinfection. The knowledge in cleaning/disinfection efficiency has recently been improved. But in order to develop optimized cleaning/disinfection protocols there still remains a challenge to better understand membrane ageing. In order to compensate for the lack of correlated cleaning/disinfection and ageing data from the literature, this paper investigates cleaning/disinfection efficiencies and ageing damages of organic ultrafiltration membranes. The final aim is to provide less detrimental cleaning/disinfection procedures and to propose some guidelines which should have been taken into consideration in term of membrane ageing studies. To carry out this study, this article will detail the background of cleaning/disinfection and aging membrane topics in a first introductive part. In a second part, key factors and endpoints of cleaning/disinfection and aging membranes will be discussed deeply: the membrane role and the cleaning parameters roles, such as water quality, storing conditions, cleaning/disinfection/aging agents/conditions/protocols. The third and last part will be developed the parameters, methods and ways of characterization at our disposal and commonly used to develop and implement membrane cleaning and/or ageing studies. Copyright © 2014 Elsevier Ltd. All rights reserved.
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NASA Astrophysics Data System (ADS)
Ngo, Chi-Vinh; Chun, Doo-Man
2017-07-01
Recently, the fabrication of superhydrophobic metallic surfaces by means of pulsed laser texturing has been developed. After laser texturing, samples are typically chemically coated or aged in ambient air for a relatively long time of several weeks to achieve superhydrophobicity. To accelerate the wettability transition from hydrophilicity to superhydrophobicity without the use of additional chemical treatment, a simple annealing post process has been developed. In the present work, grid patterns were first fabricated on stainless steel by a nanosecond pulsed laser, then an additional low-temperature annealing post process at 100 °C was applied. The effect of 100-500 μm step size of the textured grid upon the wettability transition time was also investigated. The proposed post process reduced the transition time from a couple of months to within several hours. All samples showed superhydrophobicity with contact angles greater than 160° and sliding angles smaller than 10° except samples with 500 μm step size, and could be applied in several potential applications such as self-cleaning and control of water adhesion.
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NASA Astrophysics Data System (ADS)
Blanks, J. K.; Hintz, C. J.; Chandler, G. T.; Shaw, T. J.; McCorkle, D. C.; Bernhard, J. M.
2007-12-01
Mg/Ca and Sr/Ca were analyzed from core-top individual Hoeglundina elegans aragonitic tests collected from three continental slope depths within the South Carolina and Little Bahama Bank continental slope environs (220 m to 1084 m). Our study utilized only individuals that labeled with the vital probe CellTracker Green - unlike bulk core-top material often stained with Rose Bengal, which has known inconsistencies in distinguishing live from dead foraminifera. DSr x 10 values were consistently 1.74 $ pm 0.23 across all sampling depths. The analytical error in DSr values (0.7%) determined by ICP-MS between repeated measurements on individual H. elegans tests across all depths was less than analytical error on repeated measurements from standards. Variation in DSr values was not directly explained by a linear temperature relationship (p=0.0003, R2=0.44) over the temperature range of 4.9-11.4°C with a sensitivity of 59.8 μmol/mol/1°C. The standard error by regressing DSr across temperature yields + 3.4°C, which is nearly 3x greater that reported in previous studies. Sr/Ca was more sensitive for calibrating temperature than Mg/Ca in H. elegans. Observed scatter in DSr was too great across individuals of the same size and of different sizes to resolve ontogenetic effects. However, higher DSr values were associated with smaller individuals and warmer/shallower sampling depths. The highest DSr values were observed at the intermediate sampling depth (~600 m). No significant ontogenetic relationship was found across DSr values in different sized individuals due to tighter overall constrained variance; however lower DSr values were observed from several smaller individuals. Several dead tests of H. elegans showed no significant differences in DSr values compared to live specimens cleaned by standard cleaning methods, unlike higher dead than live DMg values observed for the same individuals. There were no significant deviations in DSr across batches cleaned on separate days, unlike the observed sensitivity of DMg across batches. A subset of samples were reductively cleaned (hydrazine solution); and exhibited DMg values within analytical precision of those observed for non-reductively cleaned samples. Therefore, deviations in DMg values resulting from the removal of the reductive cleaning step did not explain analytical errors greater than published values for Mg/Ca or the high variance across same sized individuals. Variation in DMg values across the same cleaning methods and from dead individuals suggests the need for a careful look into how foraminiferal aragonite should be processed. These findings provide evidence that both Mg and Sr in benthic foraminiferal aragonite reflect factors in addition to temperature and pressure that may interfere with absolute temperature calibrations. Funded by NSF OCE 0351029, OCE 0437366, and OCE-0350794.
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2015-01-01
Combination of two physical phenomena, capillary pressure gradient and wettability gradient, allows a simple two-step fabrication process that yields a reliable hydrophobic self-cleaning condenser surface. The surface is fabricated with specific microscopic topography and further treatment with a chemically inert low-surface-energy material. This process does not require growth of nanofeatures (nanotubes) or hydrophilic–hydrophobic patterning of the surface. Trapezoidal geometry of the microfeatures facilitates droplet transfer from the Wenzel to the Cassie state and reduces droplet critical diameter. The geometry of the micropatterns enhances local coalescence and directional movement for droplets with diameter much smaller than the radial length of the micropatterns. The hydrophobic self-cleaning micropatterned condenser surface prevents liquid film formation and promotes continuous dropwise condensation cycle. Upon dropwise condensation, droplets follow a designed wettability gradient created with micropatterns from the most hydrophobic to the least hydrophobic end of the surface. The surface has higher condensation efficiency, due to its directional self-cleaning property, than a plain hydrophobic surface. We explain the self-actuated droplet collection mechanism on the condenser surface and demonstrate experimentally the creation of an effective wettability gradient over a 6 mm radial distance. In spite of its fabrication simplicity, the fabricated surface demonstrates self-cleaning property, enhanced condensation performance, and reliability over time. Our work enables creation of a hydrophobic condenser surface with the directional self-cleaning property that can be used for collection of biological (chemical, environmental) aerosol samples or for condensation enhancement. PMID:25073014
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Zamuruyev, Konstantin O; Bardaweel, Hamzeh K; Carron, Christopher J; Kenyon, Nicholas J; Brand, Oliver; Delplanque, Jean-Pierre; Davis, Cristina E
2014-08-26
Combination of two physical phenomena, capillary pressure gradient and wettability gradient, allows a simple two-step fabrication process that yields a reliable hydrophobic self-cleaning condenser surface. The surface is fabricated with specific microscopic topography and further treatment with a chemically inert low-surface-energy material. This process does not require growth of nanofeatures (nanotubes) or hydrophilic-hydrophobic patterning of the surface. Trapezoidal geometry of the microfeatures facilitates droplet transfer from the Wenzel to the Cassie state and reduces droplet critical diameter. The geometry of the micropatterns enhances local coalescence and directional movement for droplets with diameter much smaller than the radial length of the micropatterns. The hydrophobic self-cleaning micropatterned condenser surface prevents liquid film formation and promotes continuous dropwise condensation cycle. Upon dropwise condensation, droplets follow a designed wettability gradient created with micropatterns from the most hydrophobic to the least hydrophobic end of the surface. The surface has higher condensation efficiency, due to its directional self-cleaning property, than a plain hydrophobic surface. We explain the self-actuated droplet collection mechanism on the condenser surface and demonstrate experimentally the creation of an effective wettability gradient over a 6 mm radial distance. In spite of its fabrication simplicity, the fabricated surface demonstrates self-cleaning property, enhanced condensation performance, and reliability over time. Our work enables creation of a hydrophobic condenser surface with the directional self-cleaning property that can be used for collection of biological (chemical, environmental) aerosol samples or for condensation enhancement.
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Ettiene, Gretty; Bauza, Roberto; Plata, María R; Contento, Ana M; Ríos, Angel
2012-10-01
A sensitive and reliable method based on MEKC has been developed and validated for trace determination of neonicotinoid insecticides (thiamethoxam, acetamiprid, and imidacloprid) and the metabolite 6-chloronicotinic acid in water and soil matrices. Optimum separation of the neonicotinoid insecticides was obtained on a 58 cm long capillary (75 μm id) using as the running electrolyte 40 mM SDS, 5 mM borate (pH 10.4), and 5% (v/v) methanol at a temperature of 25°C, a voltage of 25 kV and with hydrodynamic injection (10 s). The analysis time was less than 7 min. Prior to MEKC determination, the samples were purified and enriched by carrying out extraction-preconcentration steps. For aqueous samples, off-line SPE with a sorptive material such as Strata-X (polymeric hydrophobic sorbent) and octadecylsilane (C₁₈) was carried out to clean up and preconcentrate the insecticides. However, for soil samples, matrix solid-phase dispersion (MSPD) was applied with C₁₈ used as the dispersant. Good linearity, accuracy, and precision were obtained and the detection limits were in the range between 0.01 and 0.07 μg mL⁻¹ for river water and 0.17 and 0.37 μg g⁻¹ for soil samples. Recovery levels reached greater than 92% for all of the assayed neonicotinoids in river water samples with Strata-X. In soil matrices, the best recoveries (63-99%) were obtained with MSPD. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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NASA Technical Reports Server (NTRS)
Himmel, R. P.
1975-01-01
Various hybrid processing steps, handling procedures, and materials are examined in an attempt to identify sources of contamination and to propose methods for the control of these contaminants. It is found that package sealing, assembly, and rework are especially susceptible to contamination. Moisture and loose particles are identified as the worst contaminants. The points at which contaminants are most likely to enter the hybrid package are also identified, and both general and specific methods for their detection and control are developed. In general, the most effective controls for contaminants are: clean working areas, visual inspection at each step of the process, and effective cleaning at critical process steps. Specific methods suggested include the detection of loose particles by a precap visual inspection, by preseal and post-seal electrical testing, and by a particle impact noise test. Moisture is best controlled by sealing all packages in a clean, dry, inert atmosphere after a thorough bake-out of all parts.
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[Implementation of a rational standard of hygiene for preparation of operating rooms].
Bauer, M; Scheithauer, S; Moerer, O; Pütz, H; Sliwa, B; Schmidt, C E; Russo, S G; Waeschle, R M
2015-10-01
The assurance of high standards of care is a major requirement in German hospitals while cost reduction and efficient use of resources are mandatory. These requirements are particularly evident in the high-risk and cost-intensive operating theatre field with multiple process steps. The cleaning of operating rooms (OR) between surgical procedures is of major relevance for patient safety and requires time and human resources. The hygiene procedure plan for OR cleaning between operations at the university hospital in Göttingen was revised and optimized according to the plan-do-check-act principle due to not clearly defined specifications of responsibilities, use of resources, prolonged process times and increased staff engagement. The current status was evaluated in 2012 as part of the first step "plan". The subsequent step "do" included an expert symposium with external consultants, interdisciplinary consensus conferences with an actualization of the former hygiene procedure plan and the implementation process. All staff members involved were integrated into this management change process. The penetration rate of the training and information measures as well as the acceptance and compliance with the new hygiene procedure plan were reviewed within step "check". The rates of positive swabs and air sampling as well as of postoperative wound infections were analyzed for quality control and no evidence for a reduced effectiveness of the new hygiene plan was found. After the successful implementation of these measures the next improvement cycle ("act") was performed in 2014 which led to a simplification of the hygiene plan by reduction of the number of defined cleaning and disinfection programs for preparation of the OR. The reorganization measures described led to a comprehensive commitment of the hygiene procedure plan by distinct specifications for responsibilities, for the course of action and for the use of resources. Furthermore, a simplification of the plan, a rational staff assignment and reduced process times were accomplished. Finally, potential conflicts due to an insufficient evidence-based knowledge of personnel was reduced. This present project description can be used by other hospitals as a guideline for similar changes in management processes.
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Hawley, Brie; Casey, Megan; Virji, Mohammed Abbas; Cummings, Kristin J.; Johnson, Alyson; Cox-Ganser, Jean
2017-01-01
Cleaning and disinfecting products consisting of a mixture of hydrogen peroxide (HP), peracetic acid (PAA), and acetic acid (AA) are widely used as sporicidal agents in health care, childcare, agricultural, food service, and food production industries. HP and PAA are strong oxidants and their mixture is a recognized asthmagen. However, few exposure assessment studies to date have measured HP, PAA, and AA in a health care setting. In 2015, we performed a health and exposure assessment at a hospital where a new sporicidal product, consisting of HP, PAA, and AA was introduced 16 months prior. We collected 49 full-shift time-weighted average (TWA) air samples and analyzed samples for HP, AA, and PAA content. Study participants were observed while they performed cleaning duties, and duration and frequency of cleaning product use was recorded. Acute upper airway, eye, and lower airway symptoms were recorded in a post-shift survey (n = 50). A subset of 35 cleaning staff also completed an extended questionnaire that assessed symptoms reported by workers as regularly occurring or as having occurred in the previous 12 months. Air samples for HP (range: 5.5 to 511.4 ppb) and AA (range: 6.7 to 530.3 ppb) were all below established US occupational exposure limits (OEL). To date, no full-shift TWA OEL for PAA has been established in the United States, however an OEL of 0.2 ppm has been suggested by several research groups. Air samples for PAA ranged from 1.1 to 48.0 ppb and were well below the suggested OEL of 0.2 ppm. Hospital cleaning staff using a sporicidal product containing HP, PAA, and AA reported work-shift eye (44%), upper airway (58%), and lower airway (34%) symptoms. Acute nasal and eye irritation were significantly positively associated with increased exposure to the mixture of the two oxidants: HP and PAA, as well as the total mixture (TM) of HP, PAA, and AA. Shortness of breath when hurrying on level ground or walking up a slight hill was significantly associated with increased exposure to the oxidant mixture (P = 0.017), as well as the TM (P = 0.026). Our results suggest that exposure to a product containing HP, PAA, and AA contributed to eye and respiratory symptoms reported by hospital cleaning staff at low levels of measured exposure. PMID:29077798
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Matumba, Limbikani; Singano, Lazarus; Pungulani, Lawrent; Mvula, Naomi; Matumba, Annie; Singano, Charles; Matita, Grey
2017-05-01
Aflatoxin contamination and biodeterioration were examined in 302 samples of dry cowpeas and pigeon peas that were randomly purchased from 9 districts of the Southern Region of Malawi during July and November 2015. Further, the impact of flotation/washing on aflatoxin levels on the pulses was elucidated. Aflatoxin analyses involved immunoaffinity column (IAC) clean-up and HPLC quantification with fluorescence detection (FLD) while legume biodeterioration assessments were done by visual inspection. Aflatoxins were frequently detected in cowpea (24%, max., 66 μg/kg) and pigeon pea (22%, max., 80 μg/kg) samples that were collected in the month of July. Lower aflatoxin incidence of 15% in cowpeas (max., 470 μg/kg) and 14% in pigeon peas (max., 377 μg/kg) was recorded in the November collection. Overall, aflatoxin levels were significantly higher in the pulses that were collected in November. However, there were no significant differences in the total aflatoxin (aflatoxin B 1 (AFB 1 ) + AFB 2 + AFG 1 + AFG 2 ) levels between the two types of pulses. Remarkably, in 76.2% of the aflatoxin positive cowpea and in 41.7% of the aflatoxin positive pigeon pea samples, aflatoxin G 1 concentration exceeded aflatoxin B 1. Insect damage percentage averaged at 18.1 ± 18.2% (mean ± SD) in the cowpeas and 16.1 ± 19.4% in pigeon peas. Mean discolouration percentage (number of pulses) of the cowpeas and pigeon peas was found to be at 6.7 ± 4.9 and 8.7 ± 6.2%, respectively. Washing and discarding the buoyant fraction was highly efficient in reducing aflatoxin levels; only 5.2 ± 11.1% of the initial aflatoxin level was found in the cleaned samples. In conclusion, cowpeas and pigeon peas sold on the local market in Malawi may constitute a hazard especially if floatation/washing step is skipped.
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Clean Air Act Amendments of 2010
Sen. Carper, Thomas R. [D-DE
2010-02-04
Senate - 03/04/2010 Committee on Environment and Public Works Senate Subcommittee on Clean Air and Nuclear Safety. Hearings held. With printed Hearing: S.Hrg. 111-1228. (All Actions) Tracker: This bill has the status IntroducedHere are the steps for Status of Legislation:
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Miralles, Pablo; Bellver, Raquel; Chisvert, Alberto; Salvador, Amparo
2016-03-01
Vortex-assisted emulsification semimicroextraction is proposed as a one-step solution-extraction procedure for sample preparation in cosmetic products. The procedure allows rapid preparation based on dispersion of the sample in a mixture of 1 mL of n-hexane and 0.5 mL of ethanol, followed by the addition of 0.5 mL of water and centrifugation to obtain two separated phases. This procedure provides good sample clean-up with minimum dilution and is very useful for the determination of ingredients with restricted concentrations, such as bronopol. The procedure was applied to the determination of bronopol by liquid chromatography with UV detection. The best chromatographic separation was obtained by using a C18 column set at 40 °C and performing a stepwise elution with a mixture of ethanol/aqueous 1 % acetic acid solution as mobile phase pumped at 0.5 mL min(-1). The detection wavelength was set at 250 nm and the total run time required was 12 min. The method was successfully applied to 18 commercial cosmetic samples including creams, shampoos, and bath gels. Good recoveries and repeatability were obtained, with a limit of detection of 0.9 μg mL(-1), which makes the method suitable for the analytical control of cosmetic products. Moreover, it could be considered environmentally friendly, because water, ethanol, and only a low volume of n-hexane are used as solvents.
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Gasperotti, Mattia; Masuero, Domenico; Guella, Graziano; Mattivi, Fulvio; Vrhovsek, Urska
2014-10-01
An increasing number of studies have concerned the profiling of polyphenol microbial metabolites, especially in urine or plasma, but only a few have regarded their accurate quantification. This study reports on a new ultra-performance liquid chromatography tandem mass spectrometry method with electrospray ionisation (UHPLC-ESI-MS/MS) using a simple clean-up step with solid phase extraction (SPE) and validation on different biological matrices. The method was tested with spiked samples of liver, heart, kidneys, brain, blood and urine. The purification procedure, after the evaluation of three different cartridges, makes it possible to obtain cleaner samples and better quantification of putative trace metabolites, especially related to dietary studies, with concentrations below ng/g in tissue and for urine and blood, starting from ng/ml. Limits of detection and linear range were also assessed using mixed polyphenol metabolite standards. Short chromatographic separation was carried out for 23 target compounds related to the polyphenol microbial metabolism, coupled with a triple quadrupole mass spectrometer for their accurate quantification. By analysing different spiked biological samples we were able to test metabolite detection in the matrix and validate the overall recovery of the method, from purification to quantification. The method developed can be successfully applied and is suitable for high-throughput targeted metabolomics analysis related to nutritional intervention, or the study of the metabolic mechanism in response to a polyphenol-rich diet. Copyright © 2014 Elsevier B.V. All rights reserved.
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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.
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NASA Astrophysics Data System (ADS)
Badiei, Hamid R.; McEnaney, Jennifer; Karanassios, Vassili
2012-12-01
A field-deployable electrochemical approach to preconcentration, matrix clean up and selective electrodeposition of Cr(III) and Cr(III) + Cr(VI) in seawater is described. Using portable, battery-operated electrochemical instrumentation, Cr species in seawater were electrodeposited in the field on portable coiled-filament assemblies made from Re. Assemblies with dried residues of Cr(III) or Cr(III) + Cr(VI) on them were transported to the lab for concentration determination by electrothermal, near-torch vaporization (NTV) sample introduction and inductively coupled plasma-atomic emission spectrometry (ICP-AES). Electrodeposition offers selective species deposition, preconcentration and matrix clean up from seawater samples. For selective deposition, free Cr(VI) was electrodeposited at - 0.3 V and Cr(III) + Cr(VI) at - 1.6 V (both vs Ag/AgCl). Interestingly, at 0 V (vs Ag/AgCl) and in the absence of an electrodeposition potential only Cr(VI) was spontaneously and selectively adsorbed on the coil and reasons for this are given. Due to preconcentration afforded by electrodeposition, the detection limits obtained after a 60 s electrodeposition at the voltages stated above using buffered (pH = 4.7) artificial seawater spiked with either Cr(III) or Cr(VI) were 20 pg/mL for Cr(III) and 10 pg/mL for Cr(VI). For comparison, the detection limit for Cr obtained by pipetting directly on the coil 5 μL of diluted standard solution was 500 pg/mL, thus it was concluded that electrodeposition offered 40 to 60 fold improvements. Matrix clean up is required due to the high salt content of seawater and this was addressed by simply rinsing the coil with 18.2 MΩ water without any loss of Cr species. Reasons for this are provided. The method was validated in the lab using buffered artificial seawater and it was used in the field for the first time by sampling seawater, buffering it and immediately electrodepositing Cr species on portable assemblies on-site. Electrodeposition in the field addressed species transformation during sample pre-treatment. Such transformations occur due to sample acidification and may take place during transport and possibly storage prior to analysis. Thus, electrodeposition in the field is more reflective of Cr species concentration at the environmental conditions (e.g., temperature) at the time of sampling. It also opens up the possibility for shipping to the lab portable assemblies with Cr species on them rather than shipping large volumes of sample to the lab, thus also reducing shipping, handling and storage costs.
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Minty, B; Ramsey, E D; Davies, I
2000-12-01
A direct aqueous supercritical fluid extraction (SFE) system was developed which can be directly interfaced to an infrared spectrometer for the determination of oil in water. The technique is designed to provide an environmentally clean, automated alternative to established IR methods for oil in water analysis which require the use of restricted organic solvents. The SFE-FTIR method involves minimum sample handling stages, with on-line analysis of a 500 ml water sample being complete within 15 min. Method accuracy for determining water samples spiked with gasoline, white spirit, kerosene, diesel or engine oil was 81-100% with precision (RSD) ranging from 3 to 17%. An independent evaluation determined a 2 ppm limit of quantification for diesel in industrial effluents. The results of a comparative study involving an established IR method and the SFE-FTIR method indicate that oil levels calculated using an accepted equation which includes coefficients derived from reference hydrocarbon standards may result in significant errors. A new approach permitted the derivation of quantification coefficients for the SFE-FTIR analyses which provided improved results. In situations where the identity of the oil to be analysed is known, a rapid off-line SFE-FTIR system calibration procedure was developed and successfully applied to various oils. An optional in-line silica gel clean-up procedure incorporated within the SFE-FTIR system enables the same water sample to be analysed for total oil content including vegetable oils and selectively for petroleum oil content within a total of 20 min. At the end of an analysis the SFE system is cleaned using an in situ 3 min clean cycle.
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Liu, Ying; Xu, Fengguo; Zhang, Zunjian; Song, Rui; Tian, Yuan
2008-07-01
To quantify naringenin and hesperetin in rat plasma after oral administration of Da-Cheng-Qi decoction, a famous purgative traditional Chinese medicine, a high-performance liquid chromatography-tandem mass spectrometry method was developed and validated. The HPLC separation was carried out on a Zorbax SB-C(18) column using 0.1% formic acid-methanol as mobile phase and estazolam as internal standard after the sample of rat plasma had been cleaned up with one-step protein precipitation using methanol. Atmospheric pressure chemical ionization in the positive ion mode and selected reaction monitoring method was developed to determine the active components. This method was validated in terms of recovery, linearity, accuracy and precision (intra- and inter-batch variation). The recoveries of naringenin and hesperetin were 72.8-76.6 and 75.7-77.2%, respectively. Linearity in rat plasma was observed over the range of 0.5-250 ng/mL (r2 > 0.99) for both naringenin and hesperetin. The accuracy and precision were well within the acceptable range and the relative standard deviation of the measured rat plasma samples was less than 15% (n = 5). The validated method was successfully applied for the evaluation of the pharmacokinetics of naringenin and hesperetin administered to six rats.
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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.
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Demougeot-Renard, Helene; De Fouquet, Chantal
2004-10-01
Assessing the volume of soil requiring remediation and the accuracy of this assessment constitutes an essential step in polluted site management. If this remediation volume is not properly assessed, misclassification may lead both to environmental risks (polluted soils may not be remediated) and financial risks (unexpected discovery of polluted soils may generate additional remediation costs). To minimize such risks, this paper proposes a geostatistical methodology based on stochastic simulations that allows the remediation volume and the uncertainty to be assessed using investigation data. The methodology thoroughly reproduces the conditions in which the soils are classified and extracted at the remediation stage. The validity of the approach is tested by applying it on the data collected during the investigation phase of a former lead smelting works and by comparing the results with the volume that has actually been remediated. This real remediated volume was composed of all the remediation units that were classified as polluted after systematic sampling and analysis during clean-up stage. The volume estimated from the 75 samples collected during site investigation slightly overestimates (5.3% relative error) the remediated volume deduced from 212 remediation units. Furthermore, the real volume falls within the range of uncertainty predicted using the proposed methodology.
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Armentano, Antonio; Summa, Simona; Magro, Sonia Lo; D’Antini, Pasquale; Palermo, Carmen; Muscarella, Marilena
2016-01-01
A C18 column packed with core-shell particles was used for the chromatographic separation of sulphonamides in feed and meat by a conventional high performance liquid chromatography system coupled with a diode array detector. Two analytical methods, already used in our laboratory, have been modified without any changes in the extraction and clean-up steps and in the liquid chromatography instrumentation. Chromatographic conditions applied on a traditional 5-µm column have been optimized on a column packed with 2.6 µm core-shell particles. A binary mobile phase [acetate buffer solution at pH 4.50 and a mixture of methanol acetonitrile 50: 50 (v/v)] was employed in gradient mode at the flow rate of 1.2 mL with an injection volume of 6 µL. These chromatographic conditions allow the separation of 13 sulphonamides with an entire run of 13 minutes. Preliminary studies have been carried out comparing blanks and spiked samples of feed and meat. A good resolution and the absence of interferences were achieved in chromatograms for both matrices. Since no change was made to the sample preparation, the optimized method does not require a complete revalidation and can be used to make routine analysis faster. PMID:28217560
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Hu, Xiaofeng; Hu, Rui; Zhang, Zhaowei; Li, Peiwu; Zhang, Qi; Wang, Min
2016-09-01
A sensitive and specific immunoaffinity column to clean up and isolate multiple mycotoxins was developed along with a rapid one-step sample preparation procedure for ultra-performance liquid chromatography-tandem mass spectrometry analysis. Monoclonal antibodies against aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, zearalenone, ochratoxin A, sterigmatocystin, and T-2 toxin were coupled to microbeads for mycotoxin purification. We optimized a homogenization and extraction procedure as well as column loading and elution conditions to maximize recoveries from complex feed matrices. This method allowed rapid, simple, and simultaneous determination of mycotoxins in feeds with a single chromatographic run. Detection limits for these toxins ranged from 0.006 to 0.12 ng mL(-1), and quantitation limits ranged from 0.06 to 0.75 ng mL(-1). Concentration curves were linear from 0.12 to 40 μg kg(-1) with correlation coefficients of R (2) > 0.99. Intra-assay and inter-assay comparisons indicated excellent repeatability and reproducibility of the multiple immunoaffinity columns. As a proof of principle, 80 feed samples were tested and several contained multiple mycotoxins. This method is sensitive, rapid, and durable enough for multiple mycotoxin determinations that fulfill European Union and Chinese testing criteria.
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Seraglio, Siluana Katia Tischer; Valese, Andressa Camargo; Daguer, Heitor; Bergamo, Greici; Azevedo, Mônia Stremel; Gonzaga, Luciano Valdemiro; Fett, Roseane; Costa, Ana Carolina Oliveira
2016-09-01
A simple, reproducible and sensitive method has been optimized and validated for simultaneous determination of 32 phenolic compounds in bracatinga (Mimosa scabrella Benth.) with the diluted-and-shoot approach, without the need of any additional clean-up steps. It has been based on high performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry and electrospray ionization (HPLC-ESI-MS/MS). The chromatography conditions were optimized, and due to the selectivity provided by MRM monitoring, LC separation required only 9min. The developed method was validated on the basis of Eurachem and European Commission Decision 2002/657/EC guidelines. Mean recoveries ranged from 70.4 to 110%. Intra-day and inter-day precision with RSD (relative standard deviations) from 0.14 to 18.9% and 0.34 to 20.0%, respectively were achieved. Limits of detection (LOD) and quantification (LOQ) ranged from 0.03 to 3.20μgL -1 and 0.20-12.8μgL -1 . Finally, the method was applied to samples and 20 phenolic compounds were quantified in all the samples analyzed, representing a contribution to the characterization and quantification of phenolic compounds from bracatinga (M. scabrella Bentham) honeydew honey. Copyright © 2016 Elsevier Ltd. All rights reserved.
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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.
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Bieri, Stefan; Ilias, Yara; Bicchi, Carlo; Veuthey, Jean-Luc; Christen, Philippe
2006-04-21
An effective combination of focused microwave-assisted extraction (FMAE) with solid-phase microextraction (SPME) prior to gas chromatography (GC) is described for the selective extraction and quantitative analysis of cocaine from coca leaves (Erythroxylum coca). This approach required switching from an organic extraction solvent to an aqueous medium more compatible with SPME liquid sampling. SPME was performed in the direct immersion mode with a universal 100 microm polydimethylsiloxane (PDMS) coated fibre. Parameters influencing this extraction step, such as solution pH, sampling time and temperature are discussed. Furthermore, the overall extraction process takes into account the stability of cocaine in alkaline aqueous solutions at different temperatures. Cocaine degradation rate was determined by capillary electrophoresis using the short end injection procedure. In the selected extraction conditions, less than 5% of cocaine was degraded after 60 min. From a qualitative point of view, a significant gain in selectivity was obtained with the incorporation of SPME in the extraction procedure. As a consequence of SPME clean-up, shorter columns could be used and analysis time was reduced to 6 min compared to 35 min with conventional GC. Quantitative results led to a cocaine content of 0.70 +/- 0.04% in dry leaves (RSD <5%) which agreed with previous investigations.
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Jank, Louise; Martins, Magda Targa; Arsand, Juliana Bazzan; Campos Motta, Tanara Magalhães; Hoff, Rodrigo Barcellos; Barreto, Fabiano; Pizzolato, Tânia Mara
2015-11-01
A fast and simple method for residue analysis of the antibiotics classes of macrolides (erythromycin, azithromycin, tylosin, tilmicosin and spiramycin) and lincosamides (lincomycin and clindamycin) was developed and validated for cattle, swine and chicken muscle and for bovine milk. Sample preparation consists in a liquid-liquid extraction (LLE) with acetonitrile, followed by liquid chromatography-electrospray-tandem mass spectrometry analysis (LC-ESI-MS/MS), without the need of any additional clean-up steps. Chromatographic separation was achieved using a C18 column and a mobile phase composed by acidified acetonitrile and water. The method was fully validated according the criteria of the Commission Decision 2002/657/EC. Validation parameters such as limit of detection, limit of quantification, linearity, accuracy, repeatability, specificity, reproducibility, decision limit (CCα) and detection capability (CCβ) were evaluated. All calculated values met the established criteria. Reproducibility values, expressed as coefficient of variation, were all lower than 19.1%. Recoveries range from 60% to 107%. Limits of detection were from 5 to 25 µg kg(-1).The present method is able to be applied in routine analysis, with adequate time of analysis, low cost and a simple sample preparation protocol. Copyright © 2015. Published by Elsevier B.V.
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National Clean Fleets Partnership (Fact Sheet)
DOE Office of Scientific and Technical Information (OSTI.GOV)
Not Available
2012-01-01
Provides an overview of Clean Cities National Clean Fleets Partnership (NCFP). The NCFP is open to large private-sector companies that have fleet operations in multiple states. Companies that join the partnership receive customized assistance to reduce petroleum use through increased efficiency and use of alternative fuels. This initiative provides fleets with specialized resources, expertise, and support to successfully incorporate alternative fuels and fuel-saving measures into their operations. The National Clean Fleets Partnership builds on the established success of DOE's Clean Cities program, which reduces petroleum consumption at the community level through a nationwide network of coalitions that work with localmore » stakeholders. Developed with input from fleet managers, industry representatives, and Clean Cities coordinators, the National Clean Fleets Partnership goes one step further by working with large private-sector fleets.« less
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Wang, Shu; Liu, Baomin; Yuan, Dongxing; Ma, Jian
2016-12-01
Glyphosate (GLYP) is an important herbicide which is also used as the phosphorus source for marine organisms. The wide applications of GLYP can lead to its accumulation in oceans and coastal waters, thus creating environmental issues. However, there is limited methods for detection of GLYP and its degradation product, aminomethylphosphonic acid (AMPA) in saline samples. Therefore, a simple and fast method for the quantification of GLYP and AMPA in seawater matrix has been developed based on the derivatization with 9-fluorenylmethylchloroformate (FMOC-Cl), separation with high performance liquid chromatography (HPLC) and detection with fluorescence detector (FLD). In order to maximize sensitivity, the derivatization procedure was carefully optimized regarding concentration of FMOC-Cl, volume of borate buffer, pH of borate buffer, mixing and derivatization time. The derivatization reaction could be completed within 30min in seawater samples without any additional clean-up or desalting steps. Under the optimized conditions, the developed HPLC method showed a wide linear response (up to several mg/L, R 2 >0.99). The limits of detection were 0.60μg/L and 0.30μg/L for GLYP and AMPA in seawater matrix, respectively. The relative standard deviation was 14.0% for GLYP (1.00mg/L) and 3.1% for AMPA (100μg/L) in saline samples with three different operators (n=24). This method was applied to determine the concentration of GLYP and AMPA in seawater culture media and the recovery data indicated minimal matrix interference. Due to its simplicity, high reproducibility and successful application in seawater culture media analysis, this method is a potentially useful analytical technique for both marine research and environmental science. Copyright © 2016 Elsevier B.V. All rights reserved.
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Chiesa, L M; Labella, G F; Panseri, S; Pavlovic, R; Bonacci, S; Arioli, F
2016-06-01
Residues of environmental contaminants in food represent a concern in food safety programs. In this study, the distribution of persistent organic pollutants (POPs) were evaluated in 79 tuna samples from FAO areas 51 (Indian Ocean), 71 (Pacific Ocean), 34 (Atlantic Ocean), and 37 (Mediterranean Sea). 6 polychlorinated biphenyls (PCBs), 16 organochlorines (OCs) and 7 polybrominated biphenyl ethers (PBDEs) were selected as representative compounds according to EFSA POPs monitoring guidelines. An analytical method, based on Accelerated Solvent Extraction (ASE), with an "in-line" clean-up step and GC-MS/MS detection, was developed, validated and applied. PCBs were detected in all FAO areas, with a prevalence of 100% for most of them. In the FAO area 37, only, all PBDEs were detected. Only 5 OCs were detected. The results showed that POPs contamination of tuna reflects FAO area contamination; in particular FAO area 37 was the most polluted. Moreover, tuna muscle was an appropriate matrix for monitoring contamination and for obtaining information about food safety. Copyright © 2016 Elsevier Ltd. All rights reserved.
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Naing, Nyi Nyi; Li, Sam Fong Yau; Lee, Hian Kee
2015-12-24
A fast and low-cost sample preparation method of graphene based dispersive solid-phase extraction combined with gas chromatography-mass spectrometric (GC-MS) analysis, was developed. The procedure involves an initial extraction with water-immiscible organic solvent, followed by a rapid clean-up using amine functionalized reduced graphene oxide as sorbent. Simple and fast one-step in situ derivatization using trimethylphenylammonium hydroxide was subsequently applied on acidic pharmaceuticals serving as model analytes, ibuprofen, gemfibrozil, naproxen, ketoprofen and diclofenac, before GC-MS analysis. Extraction parameters affecting the derivatization and extraction efficiency such as volume of derivatization agent, effect of desorption solvent, effect of pH and effect of ionic strength were investigated. Under the optimum conditions, the method demonstrated good limits of detection ranging from 1 to 16ngL(-1), linearity (from 0.01 to 50 and 0.05 to 50μgL(-1), depending on the analytes) and satisfactory repeatability of extractions (relative standard deviations, below 13%, n=3). Copyright © 2015 Elsevier B.V. All rights reserved.
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Aoki, Kimiko; Tanaka, Hiroyuki; Ueki, Makoto
2017-08-01
When the tampering of a urine sample is suspected in doping control, personal identification of the sample needs to be determined by short tandem repeat (STR) analysis using DNA. We established a method for extracting DNA from urine samples stored at -20 °C without using any additives or procedures, which is consistent with how samples are required to be managed for doping control. The method, using the Puregene® Blood Core kit followed by NucleoSpin® gDNA Clean-up or NucleoSpin® gDNA Clean-up XS kit, does not need any special instrument and can provide a purified extract with high-quality DNA from up to 40 mL of urine suitable for STR analysis using an AmpFlSTR® Identifiler® PCR amplification kit. Storing urine at -20 °C is detrimental to the stability of DNA. The DNA concentration of preserved urine could not be predicted by specific gravity or creatinine level at the time of urine collection. The DNA concentration of a purified extract (10 μL) was required to be >0.06 ng/μL to ensure a successful STR analysis. Thus, the required extraction volumes of urine preserved for 3-7 years at -20 °C were estimated to be 30 mL and 20 mL to succeed in at least 86% of men and 91% of women, respectively. Considering the long half-life of DNA during long-term preservation, our extraction method is applicable to urine samples stored even for 10 years, which is currently the storage duration allowed (increased from 8 years) before re-examination in doping control. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.
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Waldner, M H; Halter, R; Sigg, A; Brosch, B; Gehrmann, H J; Keunecke, M
2013-02-01
Traditionally EfW (Energy from Waste) plants apply a reciprocating grate to combust waste fuel. An integrated steam generator recovers the heat of combustion and converts it to steam for use in a steam turbine/generator set. This is followed by an array of flue gas cleaning technologies to meet regulatory limitations. Modern combustion applies a two-step method using primary air to fuel the combustion process on the grate. This generates a complex mixture of pyrolysis gases, combustion gases and unused combustion air. The post-combustion step in the first pass of the boiler above the grate is intended to "clean up" this mixture by oxidizing unburned gases with secondary air. This paper describes modifications to the combustion process to minimize exhaust gas volumes and the generation of noxious gases and thus improving the overall thermal efficiency of the EfW plant. The resulting process can be coupled with an innovative SNCR (Selective Non-Catalytic Reduction) technology to form a clean and efficient solid waste combustion system. Measurements immediately above the grate show that gas compositions along the grate vary from 10% CO, 5% H(2) and 0% O(2) to essentially unused "pure" air, in good agreement with results from a mathematical model. Introducing these diverse gas compositions to the post combustion process will overwhelm its ability to process all these gas fractions in an optimal manner. Inserting an intermediate step aimed at homogenizing the mixture above the grate has shown to significantly improve the quality of combustion, allowing for optimized process parameters. These measures also resulted in reduced formation of NO(x) (nitrogenous oxides) due to a lower oxygen level at which the combustion process was run (2.6 vol% O(2,)(wet) instead of 6.0 vol% O(2,)(wet)). This reduction establishes optimal conditions for the DyNOR™ (Dynamic NO(x) Reduction) NO(x) reduction process. This innovative SNCR technology is adapted to situations typically encountered in solid fuel combustion. DyNOR™ measures temperature in small furnace segments and delivers the reducing reagent to the exact location where it is most effective. The DyNOR™ distributor reacts precisely and dynamically to rapid changes in combustion conditions, resulting in very low NO(x) emissions from the stack. Copyright © 2012 Elsevier Ltd. All rights reserved.
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Recovery, Transportation and Acceptance to the Curation Facility of the Hayabusa Re-Entry Capsule
NASA Technical Reports Server (NTRS)
Abe, M.; Fujimura, A.; Yano, H.; Okamoto, C.; Okada, T.; Yada, T.; Ishibashi, Y.; Shirai, K.; Nakamura, T.; Noguchi, T.;
2011-01-01
The "Hayabusa" re-entry capsule was safely carried into the clean room of Sagamihara Planetary Sample Curation Facility in JAXA on June 18, 2010. After executing computed tomographic (CT) scanning, removal of heat shield, and surface cleaning of sample container, the sample container was enclosed into the clean chamber. After opening the sample container and residual gas sampling in the clean chamber, optical observation, sample recovery, sample separation for initial analysis will be performed. This curation work is continuing for several manths with some selected member of Hayabusa Asteroidal Sample Preliminary Examination Team (HASPET). We report here on the 'Hayabusa' capsule recovery operation, and transportation and acceptance at the curation facility of the Hayabusa re-entry capsule.
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NASA Astrophysics Data System (ADS)
Lägel, B.; Beerbom, M. M.; Doran, B. V.; Lägel, M.; Cascio, A.; Schlaf, R.
2005-07-01
The interface between the luminescent polymer poly [2-methoxy-5-(2'-ethyl-hexyloxy)-1,4-phenylene vinylene] (MEH-PPV) and sputter-cleaned indium tin oxide (ITO) was investigated using photoemission spectroscopy in combination with in situ thin film deposition. MEH-PPV was deposited in high vacuum directly from toluene solution on the ITO substrate using a home-built electrospray thin-film deposition system. The deposition was carried out in multiple steps without breaking the vacuum. In between deposition steps the sample was characterized with x-ray and ultraviolet photoemission spectroscopy. The evaluation of the spectra sequence allowed the determination of the orbital lineup (charge injection barriers) at the interface, as well as the MEH-PPV growth mode at the interface.
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Tebbutt, G. M.
1991-01-01
The performance of agar-contact plates and an alginate-swab method for sampling food surfaces before and after cleaning was compared. Contact plates were more convenient, and were at least as sensitive as the swabbing method. To assess cleaning efficiency repeated sampling was carried out in selected premises, and several cleaning methods were introduced for trial periods. Some surfaces, notably wood and polypropylene, were particularly difficult to clean. For these scrubbing with a nylon brush was the best method. Other surfaces were more easily cleaned, and generally the methods introduced as part of this study were better than the original method used in the premises. Paper proved to be unpopular, and cleaning solutions applied with it did no better than those cleaned with a multiuse cloth kept soaking in a detergent and hypochlorite solution. PMID:1850362
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Social and psychological state of the Chornobyl clean up workers. Risk factors for negative changes.
Buzunov, V O; Loganovsky, K N; Krasnikova, L I; Bomko, M O; Belyaev, Yu M; Yaroshenko, Zh S; Domashevska, T Ye
2016-12-01
It is generally recognized that the Chornobyl nuclear accident caused strong psychosocial stress affecting the entire population of Ukraine, primarily people involved in recovery operations. But what are the reasons? What is the struc ture of stressors? What are their social, medical and biological consequences, what are strategy and preventive meas ures? Issues that require special research and development. To study social and psychological state of the Chornobyl cleanup workers 1986-1987, and to determine regularities of changes and dangerous risk factors. On the basis of Polyclinic of Radiation Registry, NRCRM, we conducted sample epidemiolog ical study of social and psychological state of the Chornobyl clean up workers 1986-1987. We used method of inter viewing based on «questionnaire», specially developed for this purpose. The study was conducted in October 2013 - May 2015. The sample numbered 235 males aged 18-50 at the time of the accident. Their average age was (31.3 ± 5.3) years at the time of the accident and (58.9 ± 5.3) at the time of survey. The results revealed that the Chornobyl nuclear accident and its consequences caused strong social and psychological stress among clean up workers 1986-1987. We have identified a set of factors closely related to the Chornobyl accident, they have caused a sustainable development of mental syndrome - «Anxiety about their own health and the health of family members, especially children». The other set of stressors which are not closely relat ed to the Chornobyl accident but are the result of the social and economic, social and political situation in the coun try. However the former was found to be the cause of such a psychological state as «dissatisfaction with the com pleteness and quality of life». Social and psychological state of the Chornobyl clean up workers 1986-1987 is estimated as «poor» and it integrally can be characterized as a state of chronic psychosocial stress. Mental syndrome «Anxiety about per sonal health and the health of family members» and psychological syndrome «Dissatisfaction with living condi tions» are main consequences of this state. We identified the main stressors closely related to the consequences of the Chornobyl accident as well as those that are not related to the accident but affect profoundly the level of men tal, social and physical well being. Results of the research are of great importance in organization and provision of social, medical and antiradiation protection of population under emergency situations involving radiation exposure. Key words: Chornobyl accident, clean up workers, social and psychological state, risk factors. V. О. Buzunov, K. N. Loganovsky, L. I. Krasnikova, M. O. Bomko, Yu. M. Belyaev, Zh. S. Yaroshenko, T. Ye. Domashevska.
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Low Temperature Hall Measurements of Neutron Irradiated Silicon Carbide
2004-03-01
23 7. Cleaning Supplies in Hood. Samples were...chemicals used in the chemical hood. Figure 7: Cleaning Supplies in Hood. Samples were cleaned prior to contact deposition Additionally, the quartz tube used
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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.
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To support risk assessment efforts, a comparative intratracheal instillation (IT) study is being conducted to provide mechanistic understanding of the toxicity of different types of fibers encountered in EPA clean-up efforts. While other types of asbestos have been shown to cause...
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Federal Register 2010, 2011, 2012, 2013, 2014
2012-11-08
... ENVIRONMENTAL PROTECTION AGENCY [FRL 9750-7; CERCLA-04-2010-3768] Ellis Road/American Electric... conduct sampling, perform a clean-up and compromise cost with over 80 settling parties at the Ellis Road.... Submit your comments by Site name Ellis Road/American Electric Corporation Site by one of the following...
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10 CFR 36.59 - Detection of leaking sources.
Code of Federal Regulations, 2013 CFR
2013-01-01
... alarm set-point to a higher level if necessary to operate the pool water purification system to clean up... certificate from a transferor that leak test has been done within the 6 months before the transfer. Water from... either by using a radiation monitor on a pool water circulating system or by analysis of a sample of pool...
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10 CFR 36.59 - Detection of leaking sources.
Code of Federal Regulations, 2012 CFR
2012-01-01
... alarm set-point to a higher level if necessary to operate the pool water purification system to clean up... certificate from a transferor that leak test has been done within the 6 months before the transfer. Water from... either by using a radiation monitor on a pool water circulating system or by analysis of a sample of pool...
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10 CFR 36.59 - Detection of leaking sources.
Code of Federal Regulations, 2011 CFR
2011-01-01
... alarm set-point to a higher level if necessary to operate the pool water purification system to clean up... certificate from a transferor that leak test has been done within the 6 months before the transfer. Water from... either by using a radiation monitor on a pool water circulating system or by analysis of a sample of pool...
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10 CFR 36.59 - Detection of leaking sources.
Code of Federal Regulations, 2014 CFR
2014-01-01
... alarm set-point to a higher level if necessary to operate the pool water purification system to clean up... certificate from a transferor that leak test has been done within the 6 months before the transfer. Water from... either by using a radiation monitor on a pool water circulating system or by analysis of a sample of pool...
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Cyanuric acide (CA) is widely used as a chlorine stabilizer in outdoor pools. No simple method exists for CA measurement in the urine of exposed swimmers. The high hydrophilicity of CA makes usage of solid phase sorbents to extract it from urine nearly impossible because of samp...
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Clean-up and disposal process of polluted sediments from urban rivers.
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.
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40 CFR 35.909 - Step 2+3 grants.
Code of Federal Regulations, 2010 CFR
2010-07-01
... 40 Protection of Environment 1 2010-07-01 2010-07-01 false Step 2+3 grants. 35.909 Section 35.909... ASSISTANCE Grants for Construction of Treatment Works-Clean Water Act § 35.909 Step 2+3 grants. (a) Authority. The Regional Administrator may award grant assistance for a step 2=3 project for the combination of...
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40 CFR 35.935-4 - Step 2+3 projects.
Code of Federal Regulations, 2010 CFR
2010-07-01
... 40 Protection of Environment 1 2010-07-01 2010-07-01 false Step 2+3 projects. 35.935-4 Section 35... STATE AND LOCAL ASSISTANCE Grants for Construction of Treatment Works-Clean Water Act § 35.935-4 Step 2+3 projects. A grantee which has received step 2=3 grant assistance must make submittals required by...
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Oakley, Jennifer A; Shaw, Kirsty J; Docker, Peter T; Dyer, Charlotte E; Greenman, John; Greenway, Gillian M; Haswell, Stephen J
2009-06-07
A silica monolith used to support both electro-osmotic pumping (EOP) and the extraction/elution of DNA coupled with gel-supported reagents is described. The benefits of the combined EOP extraction/elution system were illustrated by combining DNA extraction and gene amplification using the polymerase chain reaction (PCR) process. All the reagents necessary for both processes were supported within pre-loaded gels that allow the reagents to be stored at 4 degrees C for up to four weeks in the microfluidic device. When carrying out an analysis the crude sample only needed to be hydrodynamically introduced into the device which was connected to an external computer controlled power supply via platinum wire electrodes. DNA was extracted with 65% efficiency after loading lysed cells onto a silica monolith. Ethanol contained within an agarose gel matrix was then used to wash unwanted debris away from the sample by EOP (100 V cm(-1) for 5 min). The retained DNA was subsequently eluted from the monolith by water contained in a second agarose gel, again by EOP using an electric field of 100 V cm(-1) for 5 min, and transferred into the PCR reagent containing gel. The eluted DNA in solution was successfully amplified by PCR, confirming that the concept of a complete self-contained microfluidic device could be realised for DNA sample clean up and amplification, using a simple pumping and on-chip reagent storage methodology.
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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.
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Garcia-Febrero, Raul; Valera, Enrique; Muriano, Alejandro; Pividori, M-Isabel; Sanchez-Baeza, Francisco; Marco, M-Pilar
2013-09-01
An electrochemical magneto immunosensor for the detection of low concentrations of paraquat (PQ) in food samples has been developed and its performance evaluated in a complex sample such as potato extracts. The immunosensor presented uses immunoreagents specifically developed for the recognition of paraquat, a magnetic graphite-epoxy composite (m-GEC) electrode and biofunctionalized magnetic micro-particles (PQ1-BSAMP) that allow reduction of the potential interferences caused by the matrix components. The amperometric signal is provided by an enzymatic probe prepared by covalently linking an enzyme to the specific antibodies (Ab198-cc-HRP). The use of hydroquinone, as mediator, allows recording of the signal at a low potential, which also contributes to reducing the background noise potentially caused by the sample matrix. The immunocomplexes formed on top of the modified MP are easily captured by the m-GEC, which acts simultaneously as transducer. PQ can be detected at concentrations as low as 0.18 ± 0.09 μg L(-1). Combined with an efficient extraction procedure, PQ residues can be directly detected and accurately quantified in potato extracts without additional clean-up or purification steps, with a limit of detection (90% of the maximum signal) of 2.18 ± 2.08 μg kg(-1), far below the maximum residue level (20 μg kg(-1)) established by the EC. The immunosensor presented here is suitable for on-site analysis. Combined with the use of magnetic racks, multiple samples can be run simultaneously in a reasonable time.
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36. HISTORIC PHOTOGRAPH SHOWING BILL KEYS CLEANING UP AFTER THE ...
36. HISTORIC PHOTOGRAPH SHOWING BILL KEYS CLEANING UP AFTER THE MILL RUN (NOTE SCREEN FROM MORTAR SETTING ON TABLE, STAMPS ARE HUNG UP). - Wall Street Gold Mill, Twentynine Palms, San Bernardino County, CA
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Hemmati, Maryam; Rajabi, Maryam; Asghari, Alireza
2017-11-17
In this research work, two consecutive dispersive solid/liquid phase microextractions based on efficient extraction media were developed for the influential and clean pre-concentration of clonazepam and lorazepam from complicated bio-samples. The magnetism nature of the proposed nanoadsorbent proceeded the clean-up step conveniently and swiftly (∼5min), pursued by a further enrichment via a highly effective and rapid emulsification microextraction process (∼4min) based on a deep eutectic solvent (DES). Finally, the instrumental analysis step was practicable via high performance liquid chromatography-ultraviolet detection. The solid phase used was an adequate magnetic nanocomposite termed as polythiophene-sodium dodecyl benzene sulfonate/iron oxide (PTh-DBSNa/Fe 3 O 4 ), easily and cost-effectively prepared by the impressive co-precipitation method followed by the efficient in situ sonochemical oxidative polymerization approach. The identification techniques viz. FESEM, XRD, and EDX certified the supreme physico-chemical properties of this effective nanosorbent. Also the powerful liquid extraction agent, DES, based on bio-degradable choline chloride, possessed a high efficiency, tolerable safety, low cost, and facile and mild synthesis route. The parameters involved in this versatile hyphenated procedure, efficiently evaluated via the central composite design (CCD), showed that the best extraction conditions consisted of an initial pH value of 7.2, 17mg of the PTh-DBSNa/Fe 3 O 4 nanocomposite, 20 air-agitation cycles (first step), 245μL of methanol, 250μL of DES, 440μL of THF, and 8 air-agitation cycles (second step). Under the optimal conditions, the understudied drugs could be accurately determined in the wide linear dynamic ranges (LDRs) of 4.0-3000ngmL -1 and 2.0-2000ngmL -1 for clonazepam and lorazepam, respectively, with low limits of detection (LODs) ranged from 0.7 to 1.0ngmL -1 . The enrichment factor (EF) and percentage extraction recovery (%ER) values were found to be 75 and 57% for clonazepam and 56 and 42% for lorazepam at the spiked level of 75.0ngmL -1 , possessing proper repeatabilities (relative standard deviation values (RSDs) below 5.9%, n=3). These valid analytical features provided quite accurate drug analyses at therapeutically low spans and levels below potentially toxic domains, implying a proper purification/enrichment of the proposed microextraction procedure. Copyright © 2017 Elsevier B.V. All rights reserved.
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Corrosion protection of reusable surgical instruments.
Shah, Sadiq; Bernardo, Mildred
2002-01-01
To understand the corrosion properties of surgical scissors, 416 stainless steel disks and custom electrodes were used as simulated surfaces under various conditions. These simulated surfaces were exposed to tap water and 400-ppm synthetic hard water as Ca2CO3 under different conditions. The samples were evaluated by various techniques for corrosion potential and the impact of environmental conditions on the integrity of the passive film. The electrodes were used to monitor the corrosion behavior by potentiodynamic polarization technique in water both in the presence and absence of a cleaning product. The surface topography of the 416 stainless steel disks was characterized by visual observations and scanning electron microscopy (SEM), and the surface chemistry of the passive film on the surface of the scissors was characterized by x-ray photoelectron spectroscopy (XPS). The results suggest that surgical instruments made from 416 stainless steel are not susceptible to uniform corrosion; however, they do undergo localized corrosion. The use of suitable cleaning products can offer protection against localized corrosion during the cleaning step. More importantly, the use of potentiodynamic polarization techniques allowed for a quick and convenient approach to evaluate the corrosion properties of surgical instruments under a variety of simulated-use environmental conditions.
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Health investigations of depleted-uranium clean-up workers.
Milacic, Snezana
2008-01-01
The soil contaminated by depleted uranium (238U) ammunition during the NATO bombing of Serbia and Montenegro was cleaned-up for four months in 2002. A team of 11 clean-up workers (expert members) were medically examined three times: before decontamination as a preliminary medical check-up, immediately after decontamination, and four years after cleaning up contaminated ground. This short report presents investigations and health risk assessments of clean-up workers in radioactive decontamination operations and an assessment of the environmental health perspectives for citizens living in surrounding areas. The method of initial health disorders was used, analyzing the most sensitive biological materials, such as blood cells or chromosome damage, DNA strand breaks, radio-toxicological examination of urine. The total number of blood cells did not change, but variations of the relative number (percentage) of cells in the leukocyte formula were observed. The total number of DNA alterations was higher immediately after decontamination than before decontamination. Four years after decontamination the number of DNA alterations had decreased. However, the number of damaged cells (lymphocytes containing chromosome lesions) was higher in both medical examinations, immediately after and four years after decontamination. Disease or tumours due to 238U did not develop in the group of depleted uranium clean-up workers during the investigation period of four years. Further monitoring of haematological and chromosomal effects and the health condition of workers is necessary.
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Nanomaterials for the cleaning and pH adjustment of vegetable-tanned leather
NASA Astrophysics Data System (ADS)
Baglioni, Michele; Bartoletti, Angelica; Bozec, Laurent; Chelazzi, David; Giorgi, Rodorico; Odlyha, Marianne; Pianorsi, Diletta; Poggi, Giovanna; Baglioni, Piero
2016-02-01
Leather artifacts in historical collections and archives are often contaminated by physical changes such as soiling, which alter their appearance and readability, and by chemical changes which occur on aging and give rise to excessive proportion of acids that promote hydrolysis of collagen, eventually leading to gelatinization and loss of mechanical properties. However, both cleaning and pH adjustment of vegetable-tanned leather pose a great challenge for conservators, owing to the sensitivity of these materials to the action of solvents, especially water-based formulations and alkaline chemicals. In this study, the cleaning of historical leather samples was optimized by confining an oil-in-water nanostructured fluid in a highly retentive chemical hydrogel, which allows the controlled release of the cleaning fluid on sensitive surfaces. The chemical gel exhibits optimal viscoelasticity, which facilitates its removal after the application without leaving residues on the object. Nanoparticles of calcium hydroxide and lactate, dispersed in 2-propanol, were used to adjust the pH up to the natural value of leather, preventing too high alkalinity which causes swelling of fibers and denaturation of the collagen. The treated samples were characterized using scanning electron microscopy, controlled environment dynamic mechanical analysis, and infrared spectroscopy. The analytical assessment validated the use of tools derived from colloid and materials science for the preservation of collagen-based artifacts.
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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.
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Sydney tar ponds: some problems in quantifying toxic waste.
Furimsky, Edward
2002-12-01
Information on the type and amount of hazardous and toxic waste is required to develop a meaningful strategy and estimate a realistic cost for clean up of the Sydney Tar Pond site which is located on Cape Breton, in the province of Nova Scotia, Canada. The site covers the area of the decommissioned Sysco (Sydney Steel Corporation) plant. The materials of concern include BTEX (benzene, toluene, ethylbenzene, and xylenes), PAH (polycyclic aromatic hydrocarbons), PCB (polychlorinated biphenyl), and particulates laden with toxic metals, such as arsenic, lead, and others. The originally nontoxic materials such as soil, blast furnace slag, and vegetation, as well as surface and ground waters, which were subsequently contaminated, must also be included if they fail tests prescribed by environmental regulations. An extensive sampling program must be undertaken to obtain data for an accurate estimate of the waste to be cleaned and disposed of. Apparently, 700,000 tons of toxic waste, which is believed to be present on the site, may represent only a fraction of the actual amount. The clean-up of the site is only part of the solution. Toxic waste has to be disposed of in accordance with environmental regulations.
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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.
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HPLC, MS, and pharmacokinetics of melphalan, bisantrene and 13-cis retinoic acid.
Davis, T P; Peng, Y M; Goodman, G E; Alberts, D S
1982-11-01
High performance liquid chromatographic procedures are described for melphalan, bisantrene, and 13-cis retinoic acid, three important anticancer drugs in various stages of clinical development. The procedures require a rapid and simple sample clean-up followed by a 10-to 20-min chromatographic separation on a reversed-phase C18 column. Precisions are all less than 8% with recoveries greater than 80%. Mass spectrometry confirmation of each drug from patient sample separations is presented to provide unambiguous identification for valid pharmacokinetic parameter determination.
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Project CLEAN: Safe, Sanitary School Restrooms. Fastback.
ERIC Educational Resources Information Center
Keating, Tom
After introducing the problem of unsafe, dirty public school restrooms, this publication describes Project CLEAN (Citizens, Learners, and Educators Against Neglect), an effort to improve the safety, cleanliness, and hygiene of student restrooms in public schools. The Project builds a five-step, school-by-school communication process that includes:…
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Clean Energy Solutions Center: Assisting Countries with Clean Energy Policy
Energy Solutions Center: Assisting Countries with Clean Energy Policy NREL helps developing countries and adapting to climate change impacts, developing countries are looking for clean energy solutions supports clean energy scale-up in the developing world are knowledge, capacity, and cost. The Clean Energy
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Bremer, Philip J; Fillery, Suzanne; McQuillan, A James
2006-02-15
A laboratory scale, bench top flow system was used to partially reproduce dairy plant conditions under which biofilms form and to quantify the effectiveness of caustic and acid wash steps in reducing the number of viable bacteria attached to stainless steel (SS) surfaces. Once bacteria attached to surfaces, a standard clean-in-place (CIP) regime (water rinse, 1% sodium hydroxide at 65 degrees C for 10 min, water rinse, 1.0% nitric acid at 65 degrees C for 10 min, water rinse) did not reproducibly ensure their removal. Standard CIP effectiveness was compared to alternative cleaning chemicals such as: caustic blends (Alkazolv 48, Ultrazolv 700, Concept C20, and Reflex B165); a caustic additive (Eliminator); acid blends (Nitroplus and Nitrobrite); and sanitizer (Perform). The addition of a caustic additive, Eliminator, enhanced biofilm removal compared to the standard CIP regime and further increases in cleaning efficiency occurred when nitric acid was substituted with Nitroplus. The combination of NaOH plus Eliminator and Nitroplus achieved a 3.8 log reduction in the number of cells recovered from the stainless steel surface. The incorporation of a sanitizer step into the CIP did not appear to enhance biofilm removal. This study has shown that the effectiveness of a "standard" CIP can possibly be enhanced through the testing and use of caustic and acid blends. There are many implications of these findings, including: the development of improved cleaning regimes and improved product quality, plant performance, and economic returns.
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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.
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Focused ion beam assisted three-dimensional rock imaging at submicron scale
DOE Office of Scientific and Technical Information (OSTI.GOV)
Tomutsa, Liviu; Radmilovic, Velimir
2003-05-09
Computation of effective flow properties of fluids in porous media based on three dimensional (3D) pore structure information has become more successful in the last few years, due to both improvements in the input data and the network models. Computed X-ray microtomography has been successful in 3D pore imaging at micron scale, which is adequate for many sandstones. For other rocks of economic interest, such as chalk and diatomite, submicron resolution is needed in order to resolve the 3D-pore structure. To achieve submicron resolution, a new method of sample serial sectioning and imaging using Focused Ion Beam (FIB) technology hasmore » been developed and 3D pore images of the pore system for diatomite and chalk have been obtained. FIB was used in the milling of layers as wide as 50 micrometers and as thin as 100 nanometers by sputtering of atoms from the sample surface. The focused ion beam, consisting of gallium ions (Ga+) accelerated by potentials of up to 30 kV and currents up to 20,000 pA, yields very clean, flat surfaces in which the pore-grain boundaries appear in high contrast. No distortion of the pore boundaries due to the ion milling is apparent. After each milling step, as a new surface is exposed, an image of the surface is generated. Using secondary electrons or ions, resolutions as high as 10 nm can be obtained. Afterwards, the series of 2D images can be stacked in the computer and, using appropriate interpolation and surface rendering algorithms, the 3D pore structure is reconstructed.« less
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Moving zone Marangoni drying of wet objects using naturally evaporated solvent vapor
Britten, Jerald A.
1997-01-01
A surface tension gradient driven flow (a Marangoni flow) is used to remove the thin film of water remaining on the surface of an object following rinsing. The process passively introduces by natural evaporation and diffusion of minute amounts of alcohol (or other suitable material) vapor in the immediate vicinity of a continuously refreshed meniscus of deionized water or another aqueous-based, nonsurfactant rinsing agent. Used in conjunction with cleaning, developing or wet etching application, rinsing coupled with Marangoni drying provides a single-step process for 1) cleaning, developing or etching, 2) rinsing, and 3) drying objects such as flat substrates or coatings on flat substrates without necessarily using heat, forced air flow, contact wiping, centrifugation or large amounts of flammable solvents. This process is useful in one-step cleaning and drying of large flat optical substrates, one-step developing/rinsing and drying or etching/rinsing/drying of large flat patterned substrates and flat panel displays during lithographic processing, and room-temperature rinsing/drying of other large parts, sheets or continuous rolls of material.
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Moving zone Marangoni drying of wet objects using naturally evaporated solvent vapor
Britten, J.A.
1997-08-26
A surface tension gradient driven flow (a Marangoni flow) is used to remove the thin film of water remaining on the surface of an object following rinsing. The process passively introduces by natural evaporation and diffusion of minute amounts of alcohol (or other suitable material) vapor in the immediate vicinity of a continuously refreshed meniscus of deionized water or another aqueous-based, nonsurfactant rinsing agent. Used in conjunction with cleaning, developing or wet etching application, rinsing coupled with Marangoni drying provides a single-step process for (1) cleaning, developing or etching, (2) rinsing, and (3) drying objects such as flat substrates or coatings on flat substrates without necessarily using heat, forced air flow, contact wiping, centrifugation or large amounts of flammable solvents. This process is useful in one-step cleaning and drying of large flat optical substrates, one-step developing/rinsing and drying or etching/rinsing/drying of large flat patterned substrates and flat panel displays during lithographic processing, and room-temperature rinsing/drying of other large parts, sheets or continuous rolls of material. 5 figs.
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Clean then Assemble Versus Assemble then Clean: Several Comparisons
NASA Technical Reports Server (NTRS)
Welker, Roger W.
2004-01-01
Cleanliness of manufactured parts and assemblies is a significant issue in many industries including disk drives, semiconductors, aerospace, and medical devices. Clean manufacturing requires cleanroom floor space and cleaning technology that are both expensive to own and expensive to operate. Strategies to reduce these costs are an important consideration. One strategy shown to be effective at reducing costs is to assemble parts into subassemblies and then clean the subassembly, rather than clean the individual parts first and then assemble them. One advantage is that assembly outside of the cleanroom reduces the amount of cleanroom floor space and its associated operating cost premium. A second advantage is that this strategy reduces the number of individual parts that must be cleaned prior to assembly, reducing the number of cleaning baskets, handling and, possibly, reducing the number of cleaners. The assemble then clean strategy also results in a part that is significantly cleaner because contamination generated during the assembly steps are more effectively removed that normally can be achieved by hand wiping after assembly in the cleanroom.
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30 CFR 90.204 - Approved sampling devices; maintenance and calibration.
Code of Federal Regulations, 2013 CFR
2013-07-01
... performed to assure that the sampling devices are clean and in proper working condition by a person... voltage per cell value; (2) Examination of all components of the cyclone to assure that they are clean and... sampling device to assure that it is clean and free of leaks; and (5) Examination of the clamping and...
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30 CFR 90.204 - Approved sampling devices; maintenance and calibration.
Code of Federal Regulations, 2014 CFR
2014-07-01
... performed to assure that the sampling devices are clean and in proper working condition by a person... voltage per cell value; (2) Examination of all components of the cyclone to assure that they are clean and... sampling device to assure that it is clean and free of leaks; and (5) Examination of the clamping and...
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30 CFR 90.204 - Approved sampling devices; maintenance and calibration.
Code of Federal Regulations, 2012 CFR
2012-07-01
... performed to assure that the sampling devices are clean and in proper working condition by a person... voltage per cell value; (2) Examination of all components of the cyclone to assure that they are clean and... sampling device to assure that it is clean and free of leaks; and (5) Examination of the clamping and...
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Kirschhöfer, Frank; Sahin, Olga; Becker, Gero C; Meffert, Florian; Nusser, Michael; Anderer, Gilbert; Kusche, Stepan; Klaeusli, Thomas; Kruse, Andrea; Brenner-Weiss, Gerald
2016-01-01
Organic micropollutants (MPs), in particular xenobiotics and their transformation products, have been detected in the aquatic environment and the main sources of these MPs are wastewater treatment plants. Therefore, an additional cleaning step is necessary. The use of activated carbon (AC) is one approach to providing this additional cleaning. Industrial AC derived from different carbonaceous materials is predominantly produced in low-income countries by polluting processes. In contrast, AC derived from sewage sludge by hydrothermal carbonization (HTC) is a regional and sustainable alternative, based on waste material. Our experiments demonstrate that the HTC-AC from sewage sludge was able to remove most of the applied MPs. In fact more than 50% of sulfamethoxazole, diclofenac and bezafibrate were removed from artificial water samples. With the same approach carbamazepine was eliminated to nearly 70% and atrazine more than 80%. In addition a pre-treated (phosphorus-reduced) HTC-AC was able to eliminate 80% of carbamazepine and diclofenac. Atrazine, sulfamethoxazole and bezafibrate were removed to more than 90%. Experiments using real wastewater samples with high organic content (11.1 g m(-3)) succeeded in proving the adsorption capability of phosphorus-reduced HTC-AC.
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Schmitt, Cristiane; Pires Maciel, Amanda Luiz; Boszczowski, Icaro; da Silva, Thaís Pereira; Neves, Eliane Aparecida Job; Rossini, Giulio Fabio; Rizek, Camila; Costa, Silvia Figueiredo; Lourenço, Rogério Ferreira; Alfa, Michelle J
2018-05-18
Using adenosine triphosphate (ATP) tests to assess manual cleaning of gastroscopes and to determine the associated workload in a busy endoscopy unit. Patient-used gastroscopes were sampled before and after cleaning to assess ATP levels, bioburden, and protein. Samples were collected by flushing 20 mL of sterile water through the biopsy port to the distal end. Time spent for reprocessing and performing the ATP test was recorded. Twenty-four samples were collected from 10 gastroscopes. After manual cleaning, 14/24 (58.3%) samples had no microbial growth (mean, 21 colony-forming units/cm 2 ), and in 22/24 (91.7%) samples the protein was undetectable (mean, 0.04 µg/cm 2 ). ATP test was above the cutoff (200 relative light units [RLU]) in 17/24 (70.8%) samples (mean, 498 RLU). After the second cleaning, 11/17 (64.7%) gastroscopes still failed the ATP test (mean, 321.2 RLU). The mean time spent to perform manual cleaning and ATP tests was 16 and 8 minutes, respectively. Hence, each test increased the length of time for cleaning plus testing cleanliness by 50%. Further studies regarding the optimal cutoff for ATP tests are needed. ATP tests for cleaning monitoring are easy to perform and provide immediate feedback to the team. However, the increased workload needs to be considered. Copyright © 2018 Association for Professionals in Infection Control and Epidemiology, Inc. Published by Elsevier Inc. All rights reserved.
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Biernat, John L.
2002-11-05
This invention generally relates to the remote removal of pelletized samples from cylindrical containment capsules. V-blocks are used to receive the samples and provide guidance to push out rods. Stainless steel liners fit into the v-channels on the v-blocks which permits them to be remotely removed and replaced or cleaned to prevent cross contamination between capsules and samples. A capsule holder securely holds the capsule while allowing manual up/down and in/out movement to align each sample hole with the v-blocks. Both end sections contain identical v-blocks; one that guides the drive out screw and rods or manual push out rods and the other to receive the samples as they are driven out of the capsule.
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Design and research of built-in sample cell with multiple optical reflections
NASA Astrophysics Data System (ADS)
Liu, Jianhui; Wang, Shuyao; Lv, Jinwei; Liu, Shuyang; Zhou, Tao; Jia, Xiaodong
2017-10-01
In the field of trace gas measurement, with the characteristics of high sensitivity, high selectivity and rapid detection, tunable diode laser absorption spectroscopy (TDLAS) is widely used in industrial process and trace gas pollution monitoring. Herriott cell is a common form of multiple reflections of the sample cell, the structure of the Herriott cell is relatively simple, which be used to application of trace gas absorption spectroscopy. In the pragmatic situation, the gas components are complicated, and the continuous testing process for a long time can lead to different degree of pollution and corrosion for the reflector in the sample cell. If the mirror is not cleaned up in time, it will have a great influence on the detection accuracy. In order to solve this problem in the process of harsh environment detection, this paper presents a design of the built-in sample cell to avoid the contact of gas and the mirror, thereby effectively reducing corrosion pollution. If there is optical pollution, direct replacement of the built-in optical sample cell can easily to be disassembled, and cleaned. The advantage of this design is long optical path, high precision, cost savings and so on.
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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.
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RFI to CMS: An Approach to Regulatory Acceptance of Site Remediation Technologies
NASA Technical Reports Server (NTRS)
Rowland, Martin A.
2001-01-01
Lockheed Martin made a smooth transition from RCRA Facility Investigation (RFI) at the National Aeronautics and Space Administrations'(NASA) Michoud Assembly Facility (MA-F) to its Corrective Measures Study (CMS) phase within the RCRA Corrective Action Process. We located trichloroethylene (TCE) contamination that resulted from the manufacture of the Apollo Program Saturn V rocket and the Space Shuttle External Tank, began the cleanup, and identified appropriate technologies for final remedies. This was accomplished by establishing a close working relationship with the state environmental regulatory agency through each step of the process, and resulted in receiving approvals for each of those steps. The agency has designated Lockheed Martin's management of the TCE-contamination at the MAF site as a model for other manufacturing sites in a similar situation. In February 1984, the Louisiana Department of Environmental Quality (LDEQ) issued a compliance order to begin the clean up of groundwater contaminated with TCE. In April 1984 Lockheed Martin began operating a groundwater recovery well to capture the TCE plume. The well not only removes contaminants, but also sustains an inward groundwater hydraulic gradient so that the potential offsite migration of the TCE plume is greatly diminished. This effort was successful, and for the agency to give orders and for a regulated industry to follow them is standard procedure, but this is a passive approach to solving environmental problems. The goal of the company thereafter was to take a leadership, proactive role and guide the MAF contamination clean up to its best conclusion at minimum time and lowest cost to NASA. To accomplish this goal, we have established a positive working relationship with LDEQ, involving them interactively in the implementation of advanced remedial activities at MAF as outlined in the following paragraphs.
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ERIC Educational Resources Information Center
van Rooy, Wilhelmina
2017-01-01
Clean Up Australia Day is the country's largest community-based environmental annual event when participants work in teams to remove rubbish from their local environment. This article describes an interpretive study in which a sample of preservice primary teachers' (n = 30) responses to questions about their involvement in the event were evaluated…
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Bar-Yosef, Omer; Rotman, Yaron; Nelken, Israel
2002-10-01
The responses of neurons to natural sounds and simplified natural sounds were recorded in the primary auditory cortex (AI) of halothane-anesthetized cats. Bird chirps were used as the base natural stimuli. They were first presented within the original acoustic context (at least 250 msec of sounds before and after each chirp). The first simplification step consisted of extracting a short segment containing just the chirp from the longer segment. For the second step, the chirp was cleaned of its accompanying background noise. Finally, each chirp was replaced by an artificial version that had approximately the same frequency trajectory but with constant amplitude. Neurons had a wide range of different response patterns to these stimuli, and many neurons had late response components in addition, or instead of, their onset responses. In general, every simplification step had a substantial influence on the responses. Neither the extracted chirp nor the clean chirp evoked a similar response to the chirp presented within its acoustic context. The extracted chirp evoked different responses than its clean version. The artificial chirps evoked stronger responses with a shorter latency than the corresponding clean chirp because of envelope differences. These results illustrate the sensitivity of neurons in AI to small perturbations of their acoustic input. In particular, they pose a challenge to models based on linear summation of energy within a spectrotemporal receptive field.
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Two-Step Plasma Process for Cleaning Indium Bonding Bumps
NASA Technical Reports Server (NTRS)
Greer, Harold F.; Vasquez, Richard P.; Jones, Todd J.; Hoenk, Michael E.; Dickie, Matthew R.; Nikzad, Shouleh
2009-01-01
A two-step plasma process has been developed as a means of removing surface oxide layers from indium bumps used in flip-chip hybridization (bump bonding) of integrated circuits. The two-step plasma process makes it possible to remove surface indium oxide, without incurring the adverse effects of the acid etching process.
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Guzmán-Vázquez de Prada, A; Loaiza, Oscar A; Serra, B; Morales, D; Martínez-Ruiz, P; Reviejo, A J; Pingarrón, J M
2007-05-01
A molecularly imprinted polymer was developed and used for solid-phase extraction (MISPE) of the antihelmintic fenbendazole in beef liver samples. Detection of the analyte was accomplished using square wave voltammetry (SWV) at a cylindrical carbon fibre microelectrode (CFME). A mixture of MeOH/HAc (9:1) was employed both as eluent in the MISPE system and as working medium for electrochemical detection of fenbendazole. The limit of detection was 1.9x10(-7) mol L-1 (57 microg L-1), which was appropriate for the determination of fenbendazole at the maximum residue level permitted by the European Commission (500 microg kg-1 in liver). Given that the SW voltammetric analysis could not be directly performed in the sample extract as a consequence of interference from some sample components, a sample clean-up with a MIP for selectively retaining fenbendazole was performed. The MIP was synthesized using a 1:8:22 template/methacrylic acid/ethylene glycol dimethacrylate ratio. A Britton-Robinson Buffer of pH 9.0 was selected for retaining fenbendazole in the MIP cartridges, and an eluent volume of 5.0 mL at a flow rate of 2.0 mL min-1 was chosen in the elution step. Cross-reactivity with the MIP was observed for other benzimidazoles. The synthesized MIP exhibited a good selectivity for benzimidazoles with respect to other veterinary drugs. The applicability of the MISPE-SWV method was tested with beef liver samples, spiked with fenbendazole at 5,000 and 500 microg kg-1. Results obtained for ten different liver samples yielded mean recoveries of (95+/-12)% and (96+/-11)% for the upper and lower concentration level, respectively.
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Quantification of penicillin G during labor and delivery by capillary electrophoresis.
Thomas, Andrea; Ukpoma, Omon K; Inman, Jennifer A; Kaul, Anil K; Beeson, James H; Roberts, Kenneth P
2008-04-24
In this study, a capillary electrophoresis (CE) method was developed as a means to measure levels of penicillin G (PCN G) in Group B Streptococcus (GBS) positive pregnant women during labor and delivery. Volunteers for this developmental study were administered five million units of PCN G at the onset of labor. Urine, blood, and amniotic fluid samples were collected during labor and post delivery. Samples were semi-purified by solid-phase extraction (SPE) using Waters tC18 SepPak 3cc cartridges with a sodium phosphate/methanol step gradient for elution. Capillary electrophoresis or reversed-phase high-performance liquid chromatography (RP-HPLC) with diode-array absorbance detection were used to separate the samples in less than 30 min. Quantification was accomplished by establishing a calibration curve with a linear dynamic range. The tC18 SPE methodology provided substantial sample clean-up with high recovery yields of PCN G ( approximately 90%). It was found that SPE was critical for maintaining the integrity of the separation column when using RP-HPLC, but was not necessary for sample analysis by CE where no stationary phase is present. Quantification results ranged from millimolar concentrations of PCN G in maternal urine to micromolar concentrations in amniotic fluid. Serum and cord blood levels of PCN G were below quantification limits, which is likely due to the prolonged delay in sample collection after antibiotic administration. These results show that CE can serve as a simple and effective means to characterize the pharmacokinetic distribution of PCN G from mother to unborn fetus during labor and delivery. It is anticipated that similar methodologies have the potential to provide a quick, simple, and cost-effective means of monitoring the clinical efficacy of PCN G and other drugs during pregnancy.
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Hawley, Brie; Casey, Megan; Virji, Mohammed Abbas; Cummings, Kristin J; Johnson, Alyson; Cox-Ganser, Jean
2017-12-15
Cleaning and disinfecting products consisting of a mixture of hydrogen peroxide (HP), peracetic acid (PAA), and acetic acid (AA) are widely used as sporicidal agents in health care, childcare, agricultural, food service, and food production industries. HP and PAA are strong oxidants and their mixture is a recognized asthmagen. However, few exposure assessment studies to date have measured HP, PAA, and AA in a health care setting. In 2015, we performed a health and exposure assessment at a hospital where a new sporicidal product, consisting of HP, PAA, and AA was introduced 16 months prior. We collected 49 full-shift time-weighted average (TWA) air samples and analyzed samples for HP, AA, and PAA content. Study participants were observed while they performed cleaning duties, and duration and frequency of cleaning product use was recorded. Acute upper airway, eye, and lower airway symptoms were recorded in a post-shift survey (n = 50). A subset of 35 cleaning staff also completed an extended questionnaire that assessed symptoms reported by workers as regularly occurring or as having occurred in the previous 12 months. Air samples for HP (range: 5.5 to 511.4 ppb) and AA (range: 6.7 to 530.3 ppb) were all below established US occupational exposure limits (OEL). To date, no full-shift TWA OEL for PAA has been established in the United States, however an OEL of 0.2 ppm has been suggested by several research groups. Air samples for PAA ranged from 1.1 to 48.0 ppb and were well below the suggested OEL of 0.2 ppm. Hospital cleaning staff using a sporicidal product containing HP, PAA, and AA reported work-shift eye (44%), upper airway (58%), and lower airway (34%) symptoms. Acute nasal and eye irritation were significantly positively associated with increased exposure to the mixture of the two oxidants: HP and PAA, as well as the total mixture (TM)of HP, PAA, and AA. Shortness of breath when hurrying on level ground or walking up a slight hill was significantly associated with increased exposure to the oxidant mixture (P = 0.017), as well as the TM (P = 0.026). Our results suggest that exposure to a product containing HP, PAA, and AA contributed to eye and respiratory symptoms reported by hospital cleaning staff at low levels of measured exposure. Published by Oxford University Press on behalf of the British Occupational Hygiene Society 2017.
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Clean fuel for demanding environmental markets
DOE Office of Scientific and Technical Information (OSTI.GOV)
Josewicz, W.; Natschke, D.E.
1995-12-31
Acurex Environmental Corporation is bringing Clean Fuel to the environmentally demand Krakow market, through the cooperative agreement with the U.S. Department of Energy. Clean fuel is a proprietary clean burning coal-based energy source intended for use in stoves and hand stoked boilers. Clean Fuel is a home heating fuel that is similar in form and function to raw coal, but is more environmentally friendly and lower in cost. The heating value of Clean Fuel is 24,45 kJ/kg. Extensive sets of confirmation runs were conducted in the Academy of Mining and Metallurgy in the Krakow laboratories. It demonstrated up to 54more » percent reduction of particulate matter emission, up to 35 percent reduction of total hydrocarbon emissions. Most importantly, polycyclic aromatic hydrocarbons (toxic and carcinogens compounds) emissions were reduced by up to 85 percent, depending on species measured. The above comparison was made against premium chunk coal that is currently available in Krakow for approximately $83 to 93/ton. Clean Fuel will be made available in Krakow at a price approximately 10 percent lower than that of the premium chunk coal.« less
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De Kesel, Pieter M M; Lambert, Willy E; Stove, Christophe P
2015-11-01
Caffeine is the probe drug of choice to assess the phenotype of the drug metabolizing enzyme CYP1A2. Typically, molar concentration ratios of paraxanthine, caffeine's major metabolite, to its precursor are determined in plasma following administration of a caffeine test dose. The aim of this study was to develop and validate an LC-MS/MS method for the determination of caffeine and paraxanthine in hair. The different steps of a hair extraction procedure were thoroughly optimized. Following a three-step decontamination procedure, caffeine and paraxanthine were extracted from 20 mg of ground hair using a solution of protease type VIII in Tris buffer (pH 7.5). Resulting hair extracts were cleaned up on Strata-X™ SPE cartridges. All samples were analyzed on a Waters Acquity UPLC® system coupled to an AB SCIEX API 4000™ triple quadrupole mass spectrometer. The final method was fully validated based on international guidelines. Linear calibration lines for caffeine and paraxanthine ranged from 20 to 500 pg/mg. Precision (%RSD) and accuracy (%bias) were below 12% and 7%, respectively. The isotopically labeled internal standards compensated for the ion suppression observed for both compounds. Relative matrix effects were below 15%RSD. The recovery of the sample preparation procedure was high (>85%) and reproducible. Caffeine and paraxanthine were stable in hair for at least 644 days. The effect of the hair decontamination procedure was evaluated as well. Finally, the applicability of the developed procedure was demonstrated by determining caffeine and paraxanthine concentrations in hair samples of ten healthy volunteers. The optimized and validated method for determination of caffeine and paraxanthine in hair proved to be reliable and may serve to evaluate the potential of hair analysis for CYP1A2 phenotyping. Copyright © 2015 Elsevier B.V. All rights reserved.
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Round, Adam; Felisaz, Franck; Fodinger, Lukas; Gobbo, Alexandre; Huet, Julien; Villard, Cyril; Blanchet, Clement E.; Pernot, Petra; McSweeney, Sean; Roessle, Manfred; Svergun, Dmitri I.; Cipriani, Florent
2015-01-01
Small-angle X-ray scattering (SAXS) of macromolecules in solution is in increasing demand by an ever more diverse research community, both academic and industrial. To better serve user needs, and to allow automated and high-throughput operation, a sample changer (BioSAXS Sample Changer) that is able to perform unattended measurements of up to several hundred samples per day has been developed. The Sample Changer is able to handle and expose sample volumes of down to 5 µl with a measurement/cleaning cycle of under 1 min. The samples are stored in standard 96-well plates and the data are collected in a vacuum-mounted capillary with automated positioning of the solution in the X-ray beam. Fast and efficient capillary cleaning avoids cross-contamination and ensures reproducibility of the measurements. Independent temperature control for the well storage and for the measurement capillary allows the samples to be kept cool while still collecting data at physiological temperatures. The Sample Changer has been installed at three major third-generation synchrotrons: on the BM29 beamline at the European Synchrotron Radiation Facility (ESRF), the P12 beamline at the PETRA-III synchrotron (EMBL@PETRA-III) and the I22/B21 beamlines at Diamond Light Source, with the latter being the first commercial unit supplied by Bruker ASC. PMID:25615861
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Rapid separation and purification of uranium and plutonium from dilute-matrix samples
Armstrong, Christopher R.; Ticknor, Brian W.; Hall, Gregory; ...
2014-03-11
This work presents a streamlined separation and purification approach for trace uranium and plutonium from dilute (carrier-free) matrices. The method, effective for nanogram quantities of U and femtogram to picogram quantities of Pu, is ideally suited for environmental swipe samples that contain a small amount of collected bulk material. As such, it may be applicable for processing swipe samples such as those collected in IAEA inspection activities as well as swipes that are loaded with unknown analytes, such as those implemented in interlaboratory round-robin or proficiency tests. Additionally, the simplified actinide separation could find use in internal laboratory monitoring ofmore » clean room conditions prior to or following more extensive chemical processing. We describe key modifications to conventional techniques that result in a relatively rapid, cost-effective, and efficient U and Pu separation process. We demonstrate the efficacy of implementing anion exchange chromatography in a single column approach. We also show that hydrobromic acid is an effective substitute in lieu of hydroiodoic acid for eluting Pu. Lastly, we show that nitric acid is an effective digestion agent in lieu of perchloric acid and/or hydrofluoric acid. A step by step procedure of this process is detailed.« less
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Partnering: An Engine for Innovation - Continuum Magazine | NREL
$10 million, five-year agreement at NREL's annual Industry Growth Forum, taking the next step in a positioned than ever before to help move big ideas to market. Industry Growth Forum Cultivates Clean Energy Entrepreneurship Industry Growth Forum Cultivates Clean Energy Entrepreneurship NREL's Industry Growth Forum brings
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Data Cleaning in Mathematics Education Research: The Overlooked Methodological Step
ERIC Educational Resources Information Center
Hubbard, Aleata
2017-01-01
The results of educational research studies are only as accurate as the data used to produce them. Drawing on experiences conducting large-scale efficacy studies of classroom-based algebra interventions for community college and middle school students, I am developing practice-based data cleaning procedures to support scholars in conducting…
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Complete Lesson 3: Breathing Easy: Keeping the Inside of Our Homes Healthy and Clean
Looks at our homes and the steps to take to keep the air healthy and avoid chemical exposure. We explore the makeup of the air that we breathe, how to keep it clean, and how to reduce asthma triggers in our homes, as well as lead.
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The purpose of this SOP is to describe the steps involved in cleaning the electronic data generated from data entry of the Questionnaire Feedback form. It applies to electronic data corresponding to the Questionnaire Feedback form that was scanned and verified by the data staff ...
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The purpose of this SOP is to define the steps involved in cleaning the electronic data generated from data entry of the Descriptive Questionnaire. It applies to electronic data corresponding to the Descriptive Questionnaire that was scanned and verified by the Data Staff during...
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The purpose of this SOP is to define the steps involved in cleaning the electronic data generated from data entry of the Baseline Questionnaire. It applies to electronic data corresponding to the Baseline Questionnaire that was scanned and verified by the Data Staff during the A...
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The purpose of this SOP is to define the steps involved in cleaning the electronic data generated from data entry of the Technician Walk-Through Questionnaire. It applies to electronic data corresponding to the Technician Walk-Through Questionnaire that was scanned and verified ...
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The purpose of this SOP is to define the steps involved in cleaning the electronic data generated from data entry of the Descriptive Questionnaire. It applies to electronic data corresponding to the Descriptive Questionnaire that was scanned and verified by the data staff during...
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Cui, Linfan; Zhang, Panpan; Xiao, Yukun; Liang, Yuan; Liang, Hanxue; Cheng, Zhihua; Qu, Liangti
2018-05-01
The use of abundant solar energy for regeneration and desalination of water is a promising strategy to address the challenge of a global shortage of clean water. Progress has been made to develop photothermal materials to improve the solar steam generation performance. However, the mass production rate of water is still low. Herein, by a rational combination of photo-electro-thermal effect on an all-graphene hybrid architecture, solar energy can not only be absorbed fully and transferred into heat, but also converted into electric power to further heat up the graphene skeleton frame for a much enhanced generation of water vapor. As a result, the unique graphene evaporator reaches a record high water production rate of 2.01-2.61 kg m -2 h -1 under solar illumination of 1 kW m -2 even without system optimization. Several square meters of the graphene evaporators will provide a daily water supply that is enough for tens of people. The combination of photo-electro-thermal effect on graphene materials offers a new strategy to build a fast and scalable solar steam generation system, which makes an important step towards a solution for the scarcity of clean water. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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Dirt detection on brown eggs by means of color computer vision.
Mertens, K; De Ketelaere, B; Kamers, B; Bamelis, F R; Kemps, B J; Verhoelst, E M; De Baerdemaeker, J G; Decuypere, E M
2005-10-01
In the last 20 yr, different methods for detecting defects in eggs were developed. Until now, no satisfying technique existed to sort and quantify dirt on eggshells. The work presented here focuses on the design of an off-line computer vision system to differentiate and quantify the presence of different dirt stains on brown eggs: dark (feces), white (uric acid), blood, and yolk stains. A system that provides uniform light exposure around the egg was designed. In this uniform light, pictures of dirty and clean eggs were taken, stored, and analyzed. The classification was based on a few standard logical operators, allowing for a quick implementation in an online set-up. In an experiment, 100 clean and 100 dirty eggs were used to validate the classification algorithm. The designed vision system showed an accuracy of 99% for the detection of dirt stains. Two percent of the clean eggs had a light-colored eggshell and were subsequently mistaken for showing large white stains. The accuracy of differentiation of the different kinds of dirt stains was 91%. Of the eggs with dark stains, 10.81% were mistaken for having bloodstains, and 33.33% of eggs with bloodstains were mistaken for having dark stains. The developed system is possibly a first step toward an on line dirt evaluation technique for brown eggs.
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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.
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Salgueiro-González, N; Turnes-Carou, I; Muniategui-Lorenzoa, S; López-Mahía, P; Prada-Rodríguez, D
2012-12-28
A novel and green analytical methodology for the determination of alkylphenols (4-tert-octylphenol, 4-n-octylphenol, 4-n-nonylphenol, nonylphenol technical mixture) and bisphenol A in bivalve mollusc samples was developed and validated. The method was based on selective pressurized liquid extraction (SPLE) with a simultaneous in cell clean up combined with liquid chromatography–electrospray ionization tandem mass spectrometry in negative mode (LC–ESI-MS/MS). Quantitation was performed by standard addition curves in order to correct matrix effects. The analytical features of the method were satisfactory: relative recoveries varied between 80 and 107% and repeatability and intermediate precision were <20% for all compounds. Uncertainty assessment of measurement was estimated on the basis of an in-house validation according to EURACHEM/CITAC guide. Quantitation limits of the method (MQL) ranged between 0.34 (4-n-octylphenol) and 3.6 ng g(−1) dry weight (nonylphenol). The main advantages of the method are sensitivity, selectivity, automaticity, low volumes of solvents required and low sample analysis time (according with the principles of Green Chemistry). The method was applied to the analysis of mussel samples of Galicia coast (NW of Spain). Nonylphenol and 4-tert-octylphenol were measured in all samples at concentrations between 9.3 and 372 ng g(−1) dw. As an approach, the human daily intake of these compounds was estimated and no risk for human health was found.
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Validation of adenosine triphosphate to audit manual cleaning of flexible endoscope channels.
Alfa, Michelle J; Fatima, Iram; Olson, Nancy
2013-03-01
Compliance with cleaning of flexible endoscope channels cannot be verified using visual inspection. Adenosine triphosphate (ATP) has been suggested as a possible rapid cleaning monitor for flexible endoscope channels. There have not been published validation studies to specify the level of ATP that indicates inadequate cleaning has been achieved. The objective of this study was to validate the Clean-Trace (3M Inc, St. Paul, MN) ATP water test method for monitoring manual cleaning of flexible endoscopes. This was a simulated use study using a duodenoscope as the test device. Artificial test soil containing 10(6) colony-forming units of Pseudomonas aeruginosa and Enterococcus faecalis was used to perfuse all channels. The flush sample method for the suction-biopsy (L1) or air-water channel (L2) using 40 and 20 mLs sterile reverse osmosis water, respectively, was validated. Residuals of ATP, protein, hemoglobin, and bioburden were quantitated from channel samples taken from uncleaned, partially cleaned, and fully cleaned duodenoscopes. The benchmarks for clean were as follows: <6.4 μg/cm(2) protein, <2.2 μg/cm(2) hemoglobin, and <4-log10 colony-forming units/cm(2) bioburden. The average ATP in clean channel samples was 27.7 RLUs and 154 RLUs for L1 and L2, respectively (<200 RLUs for all channels). The average protein, hemoglobin, and bioburden benchmarks were achieved if <200 RLUs were detected. If the channel sample was >200 RLUs, the residual organic and bioburden levels would exceed the acceptable benchmarks. Our data validated that flexible endoscopes that have complete manual cleaning will have <200 RLUs by the Clean-Trace ATP test. Copyright © 2013 Association for Professionals in Infection Control and Epidemiology, Inc. Published by Mosby, Inc. All rights reserved.
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NASA Technical Reports Server (NTRS)
Glavin, D.; Archer, D.; Brunner, A.; Buch, A.; Cabane, M.; Coll, P.; Conrad, P.; Coscia, D.; Dworkin J.; Eigenbrode, J.;
2013-01-01
The search for organic compounds on Mars, including molecules of either abiotic or biological origin is one of the key goals of the Mars Science Laboratory (MSL) mission. Previously the Viking and Phoenix Lander missions searched for organic compounds, but did not find any definitive evidence of martian organic material in the soils. The Viking pyrolysis gas chromatography mass spectrometry (GCMS) instruments did not detect any organic compounds of martian or exogenous origin above a level of a few parts-per-billion (ppb) in the near surface regolith at either landing site [1]. Viking did detect chloromethane and dichloromethane at pmol levels (up to 40 ppb) after heating the soil samples up to 500 C (Table 1), although it was originally argued that the chlorohydrocarbons were derived from cleaning solvents used on the instrument hardware, and not from the soil samples themselves [1]. More recently, it was suggested that the chlorohydrocarbons detected by Viking may have been formed by oxidation of indigenous organic matter during pyrolysis of the soil in the presence of perchlorates [2]. Although it is unknown if the Viking soils contained perchlorates, Phoenix did reveal relatively high concentrations (0.6 wt%) of perchlorate salt in the icy regolith [3], therefore, it is possible that the chlorohydrocarbons detected by Viking were produced, at least partially, during the experiments [2,4]. The Sample Analysis at Mars (SAM) instrument suite on MSL analyzed the organic composition of the soil at Rocknest in Gale Crater using a combination of pyrolysis evolved gas analysis (EGA) and GCMS. One empty cup procedural blank followed by multiple EGA-GCMS analyses of the Rocknest soil were carried out. Here we will discuss the results from these SAM measurements at Rocknest and the steps taken to determine the source of the chlorohydrocarbons.
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López-Ruiz, Rosalía; Romero-González, Roberto; Martínez Vidal, José Luis; Fernández-Pérez, Manuel; Garrido Frenich, Antonia
2017-12-31
A comprehensive degradation study of quizalofop-p, quizalofop-p-ethyl, quizalofop-p-tefuryl and propaquizafop in soil samples have been firstly performed using ultra high performance liquid chromatography coupled to Orbitrap mass spectrometry (UHPLC-Orbitrap-MS). Thus, metabolites or degradation products, such as CHHQ (dihydroxychloroquinoxalin), CHQ (6-chloroquinoxalin-2-ol), PPA ((R)-2-(4-hydroxyphenoxy)propionic acid) and 2,3-dihydroxyquinoxaline were also monitored. An extraction procedure based on QuEChERS procedure was used. Acidified water (0.1M hydrochloric acid) and acidified acetonitrile (1% acetic acid, (v/v)) were used as extraction solvents, and magnesium sulfate and sodium chloride were used as salts. Dispersive solid phase extraction with C 18 as sorbent, was needed as a clean-up step. Several commercial products (Panarex®, Master-D® and Dixon®) were used to evaluate the degradation of the target compounds into their metabolites. The concentration of the main active substances (quizalofop-p-tefuryl, quizalofop-p-ethyl and propaquizafop) decreased during the degradation studies, whereas the concentration of quizalofop-p increased. Dissipation rates of half-live of quizalofop-p were also evaluated, and it was observed that this compound is easily degraded, obtaining values lower than 1day. Taking into account that quizalofop-p is the R enantiomer of quizalofop, a chiral separation was performed by liquid chromatography coupled to tandem mass spectrometry, concluding that in samples containing quizalofop-p-tefuryl, there was a 15% contribution from the S enantiomer and a 85% contribution from the R enantiomer. Metabolites such as PPA, CHHQ and CHQ were detected in soil samples after 15days of application commercial product at concentrations between the limits of detection (LOD) and the limits of quantification (LOQ). CHQ and CHHQ were detected at concentrations higher than the LOQ in samples after 50 and 80days of application, with their concentration increasing during this time up to 500%. Copyright © 2017 Elsevier B.V. All rights reserved.
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Novel dense CO2 technique for beta-galactosidase immobilization in polystyrene microchannels.
Leclair Ellis, Jeffrey; Tomasko, David L; Dehghani, Fariba
2008-03-01
In this study we design new fabrication techniques and demonstrate the potential of using dense CO2 for facilitating crucial steps in the fabrication of polymeric lab-on-a-chip microdevices by embedding biomolecules at temperatures well below the polymer's glass transition temperature (T(g)). These new techniques are environmentally friendly and done without the use of a clean room. Carbon dioxide at 40 degrees C and between 4.48 and 6.89 MPa was used to immobilize the biologically active molecule, beta-galactosidase (beta-gal), on the surface of polystyrene microchannels. To our knowledge, this is the first time dense CO2 has been used to directly immobilize an enzyme in a microchannel. beta-gal activity was maintained and shown via a fluorescent reaction product, after enzyme immobilization and microchannel capping by the designed fabrication steps at 40 degrees C and pressures up to 6.89 MPa.
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Monitoring the clean-up operation of agricultural fields flooded with red mud in Hungary.
Uzinger, Nikolett; Rékási, Márk; Anton, Áron D; Koós, Sándor; László, Péter; Anton, Attila
2016-12-01
In the course of the clean-up operation after the red mud inundation in 2010, red mud was removed from the soil surface in places where the layer was more than 5 cm deep. Before its removal, the red mud seeped into the soil. In 2012, soil samples were taken from depths of 0 to 20 and 20 to 40 cm on some of the affected areas. The parameters investigated were pH, organic matter, salt%, and the total and mobile fractions of various elements. The values recorded in 2012 were compared with those measured immediately after the removal of the red mud in 2010 and with the background and clean-up target concentrations. The pH values remained below the designated limit, while the salt content only exhibited values in the weakly salty range on areas at the greatest distance from the dam. In the central part of the inundated area, total Na contents above the 900 mg/kg target value were observed, but the Na content in the 0-20-cm layer generally exhibited a decrease due to leaching. The pH and As concentration also showed a decline on several areas compared with the values recorded in 2010. Total As and Co contents in excess of the target values were recorded on the lowest-lying part of the flooded area, probably because the finest red mud particles were deposited the furthest from the dam, where they seeped into the soil. Nevertheless, the mobility and plant availability of both elements remained moderate. The total contents of both Co and Mo, however, exhibited a significant rise compared with both the background value and the 2010 data. The monitoring of the cleaned-up areas showed that after a 2-year period element concentrations that exceeded the target values and could be attributed to the red mud pollution were only detectable on the lowest-lying areas.
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NASA Astrophysics Data System (ADS)
Bar-Cohen, Yoseph; Badescu, Mircea; Sherrit, Stewart; Bao, Xiaoqi; Lindsey, Cameron; Kutzer, Thomas; Salazar, Eduardo
2018-03-01
The return of samples back to Earth in future missions would require protection of our planet from the risk of bringing uncontrolled biological materials back with the samples. This protection would require "breaking the chain of contact (BTC)", where any returned material reaching Earth for further analysis would have to be sealed inside a container with extremely high confidence. Therefore, the acquired samples would need to be contained while destroying any potential biological materials that may contaminate the external surface of the container. A novel process that could be used to contain returning samples has been developed and demonstrated in a quarter scale size. The process consists of brazing using non-contact induction heating that synchronously separates, seams, seals and sterilizes (S4) the container. The use of brazing involves melting at temperatures higher than 500°C and this level of heating assures sterilization of the exposed areas since all carbon bonds (namely, organic materials) are broken at this temperature. The mechanism consists of a double wall container with inner and outer shells having Earth-clean interior surfaces. The process consists of two-steps, Step-1: the double wall container halves are fabricated and brazed (equivalent to production on Earth); and Step-2 is the S4 process and it is the equivalent to the execution on-orbit around Mars. In a potential future mission, the double wall container would be split into two halves and prepared on Earth. The potential on-orbit execution would consist of inserting the orbiting sample (OS) container into one of the halves and then mated to the other half and brazed. The latest results of this effort will be described and discussed in this manuscript.
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NASA Astrophysics Data System (ADS)
Stocker, Andrea; Mosler, Hans-Joachim
2015-04-01
Recontamination of drinking water occurring between water collection at the source and the point of consumption is a current problem in developing countries. The household drinking water storage container is one source of contamination and should therefore be cleaned regularly. First, the present study investigated contextual factors that stimulate or inhibit the development of habitual cleaning of drinking water storage containers with soap and water. Second, based on the Risk, Attitudes, Norms, Abilities, and Self-regulation (RANAS) Model of behavior, the study aimed to determine which sociopsychological factors should be influenced by an intervention to promote habitual cleaning. In a cross-sectional study, 905 households in rural Benin were interviewed by structured face-to-face interviews. A forced-entry regression analysis was used to determine potential contextual factors related to habitual cleaning. Subsequently, a hierarchical regression was conducted with the only relevant contextual factor entered in the first step (R2 = 6.7%) and the sociopsychological factors added in the second step (R2 = 62.5%). Results showed that households using a clay container for drinking water storage had a significantly weaker habit of cleaning their water storage containers with soap and water than did households using other types of containers (β = -0.10). The most important sociopsychological predictors of habitual cleaning were commitment (β = 0.35), forgetting (β = -0.22), and self-efficacy (β = 0.14). The combined investigation of contextual and sociopsychological factors proved beneficial in terms of developing intervention strategies. Possible interventions based on these findings are recommended.
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Dyscirculatory encephalopathy in Chernobyl disaster clean-up workers (a 20-year study).
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.
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Automated imprint mask cleaning for step-and-flash imprint lithography
NASA Astrophysics Data System (ADS)
Singh, Sherjang; Chen, Ssuwei; Selinidis, Kosta; Fletcher, Brian; McMackin, Ian; Thompson, Ecron; Resnick, Douglas J.; Dress, Peter; Dietze, Uwe
2009-03-01
Step-and-Flash Imprint Lithography (S-FIL) is a promising lithography strategy for semiconductor manufacturing at device nodes below 32nm. The S-FIL 1:1 pattern transfer technology utilizes a field-by-field ink jet dispense of a low viscosity liquid resist to fill the relief pattern of the device layer etched into the glass mask. Compared to other sub 40nm CD lithography methods, the resulting high resolution, high throughput through clustering, 3D patterning capability, low process complexity, and low cost of ownership (CoO) of S-FIL makes it a widely accepted technology for patterned media as well as a promising mainstream option for future CMOS applications. Preservation of mask cleanliness is essential to avoid risk of repeated printing of defects. The development of mask cleaning processes capable of removing particles adhered to the mask surface without damaging the mask is critical to meet high volume manufacturing requirements. In this paper we have presented various methods of residual (cross-linked) resist removal and final imprint mask cleaning demonstrated on the HamaTech MaskTrack automated mask cleaning system. Conventional and non-conventional (acid free) methods of particle removal have been compared and the effect of mask cleaning on pattern damage and CD integrity is also studied.
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DOE Office of Scientific and Technical Information (OSTI.GOV)
SLEIMAN, Mohamad; MADDALENA, Randy L.; GUNDEL, Lara A.
Tobacco-specific nitrosamines (TSNAs) are some of the most potent carcinogens in tobacco and cigarette smoke. Accurate quantification of these chemicals is needed to help assess public health risks. We developed and validated a specific and sensitive method to measure four TSNAs in both the gas- and particle-phase of secondhand smoke (SHS) using gas chromatography and ion-trap tandem mass spectrometry,. A smoking machine in an 18-m3 room-sized chamber generated relevant concentrations of SHS that were actively sampled on Teflon coated fiber glass (TCFG) filters, and passively sampled on cellulose substrates. A simple solid-liquid extraction protocol using methanol as solvent was successfullymore » applied to both filters with high recoveries ranging from 85 to 115percent. Tandem MS parameters were optimized to obtain the best sensitivity in terms of signal to-noise ratio (S/N) for the target compounds. For each TSNA, the major fragmentation pathways as well as ion structures were elucidated and compared with previously published data. The method showed excellent performances with a linear dynamic range between 2 and 1000 ng mL-1, low detection limits (S/N> 3) of 30-300 pg.ml-1 and precision with experimental errors below 10percent for all compounds. Moreover, no interfering peaks were observed indicating a high selectivity of MS/MS without the need for a sample clean up step. The sampling and analysis method provides a sensitive and accurate tool to detect and quantify traces of TSNA in SHS polluted indoor environments.« less
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Determination of endocrine disrupting compounds and their metabolites in fish bile.
Ros, Oihana; Izaguirre, Jon Kepa; Olivares, Maitane; Bizarro, Cristina; Ortiz-Zarragoitia, Maren; Cajaraville, Miren Pilar; Etxebarria, Nestor; Prieto, Ailette; Vallejo, Asier
2015-12-01
This work describes a new methodology for the simultaneous determination of a large variety of emerging and persistent organic compounds and some of their metabolites in fish bile samples. The target compounds were musk fragrances, alkyl phenols, hormones, pesticides, phthalate esters and bisphenol-A, all of them with a known endocrine disrupting effect. To achieve the determination these three steps were optimized: i) an enzymatic hydrolysis of the metabolites to render the unconjugated compounds; ii) the solid phase extraction of the target analytes (Plexa cartridges 200-mg); and, iii) a clean-up of the extracts (Florisil cartridges 1-g). The samples were analyzed by gas-chromatography-mass spectrometry (GC-MS), though the polar fraction required a previous derivatization with O-bis (trimethylsilyl) trifluoroacetamide. Good apparent recoveries (63-122%), repeatability (<20%) and limits of detection (LODs) ranging between 0.04 and 459 ng/mL were obtained. This method was applied to the analysis of the target analytes in bile samples of thicklip grey mullets (Chelon labrosus) from five different populations of the Basque Coast (South East Bay of Biscay) during the period of May-June 2012. The target analytes were found at concentrations ranging from
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Aung, Hnin-Pwint; Pyell, Ute
2016-06-03
For the rapid simultaneous determination of monosodium glutamate (MSG), benzoic acid (BA), and sorbic acid (SA) in canned food and other processed food samples, we developed a method that combines in-capillary derivatization with separation by capillary electrophoresis. This method employs the rapid derivatization of MSG with o-phthalaldehyde (OPA) in the presence of 3-mercaptopropionic acid (3-MPA) and enables the detection of the resulting OPA-MSG derivative and of non-derivatized BA and SA at 230nm. The composition of the background electrolyte and the parameters of derivatization and separation are as follows: 25mM borax containing 5mM OPA and 6mM 3-MPA, separation voltage 25mV, injection at 30mbar for 20s, and column temperature 25°C. Because of the high reaction rate and suitably adapted effective electrophoretic mobilities, band broadening due to the derivatization reaction at the start of the separation process is kept to a minimum. The optimized method is validated with respect to LOD, LOQ, linearity, recovery, and precision. This method can be applied to real samples such as soy, fish, oyster and sweet and sour chili sauces after application of appropriate clean-up steps. Mechanisms of zone broadening and zone focusing are discussed showing the validity of the employed theoretical approach regarding the dependence of the peak shape for OPA-MSG on the concentration of MSG in the sample. Copyright © 2016 Elsevier B.V. All rights reserved.
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Zhou, Jinhui; Qi, Yitao; Hou, Yali; Zhao, Jing; Li, Yi; Xue, Xiaofeng; Wu, Liming; Zhang, Jinzhen; Chen, Fang
2011-09-01
In this paper, a method for the rapid and sensitive analysis of juvenile hormone III (JH III) and 20-hydroxyecdysone (20E) in queen larvae and drone pupae samples was presented. Ultrasound-assisted extraction provided a significant shortening of the leaching time for the extraction of JH III and 20E and satisfactory sensitivity as compared to the conventional shake extraction procedure. After extraction, determination was carried out by liquid chromatography-tandem mass spectrometry (LC-MS/MS) operating in electrospray ionization positive ion mode via multiple reaction monitoring (MRM) without any clean-up step prior to analysis. A linear gradient consisting of (A) water containing 0.1% formic acid and (B) acetonitrile containing 0.1% formic acid, and a ZORBAX SB-Aq column (100 mm × 2.1 mm, 3.5 μm) were employed to obtain the best resolution of the target analytes. The method was validated for linearity, limit of quantification, recovery, matrix effects, precision and stability. Drone pupae samples were found to contain 20E at concentrations of 18.0 ± 0.1 ng/g (mean ± SD) and JH III was detected at concentrations of 0.20 ± 0.06 ng/g (mean ± SD) in queen larvae samples. This validated method provided some practical information for the actual content of JH III and 20E in queen larvae and drone pupae samples. Copyright © 2011 Elsevier B.V. All rights reserved.
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Sanchez-Prado, Lucia; Alvarez-Rivera, Gerardo; Lamas, J Pablo; Lores, Marta; Garcia-Jares, Carmen; Llompart, Maria
2011-12-01
Matrix solid-phase extraction has been successfully applied for the determination of multi-class preservatives in a wide variety of cosmetic samples including rinse-off and leave-on products. After extraction, derivatization with acetic anhydride, and gas chromatography-mass spectrometry analysis were performed. Optimization studies were done on real non-spiked and spiked leave-on and rinse-off cosmetic samples. The selection of the most suitable extraction conditions was made using statistical tools such as ANOVA, as well as factorial experimental designs. The final optimized conditions were common for both groups of cosmetics and included the dispersion of the sample with Florisil (1:4), and the elution of the MSPD column with 5 mL of hexane/acetone (1:1). After derivatization, the extract was analyzed without any further clean-up or concentration step. Accuracy, precision, linearity and detection limits were evaluated to assess the performance of the proposed method. The recovery studies on leave-on and rinse-off cosmetics gave satisfactory values (>78% for all analytes in all the samples) with an average relative standard deviation value of 4.2%. The quantification limits were well below those set by the international cosmetic regulations, making this multi-component analytical method suitable for routine control. The analysis of a broad range of cosmetics including body milk, moisturizing creams, anti-stretch marks creams, hand creams, deodorant, shampoos, liquid soaps, makeup, sun milk, hand soaps, among others, demonstrated the high use of most of the target preservatives, especially butylated hydroxytoluene, methylparaben, propylparaben, and butylparaben.
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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.
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LT-STM/STS studies of clean armchair edge
NASA Astrophysics Data System (ADS)
Ju, Zheng; Zhang, Wenhan; Wu, Weida; Weida Wu Team
It was predicted and observed that the passivated zigzag edges of graphene host highly localized edge state. This edge state is predicted to be spin-polarized, which is appealing for spintronic applications. In contrast, no edge state was expected at passivated armchair graphene edge. Here we report low temperature scanning tunneling microscopy and spectroscopy (STM/STS) studies of electronic properties of clean monoatomic step edges on cleaved surface of HOPG. Most of step edges are armchair edges, in agreement with previous STM results. We observed only (√{ 3} ×√{ 3}) R30° superstructure near armchair edges, which has been reported in previous STM studies. On the other hand, no honeycomb superstructure was observed in our STM data. In addition, our STM results reveal an intriguing localized electronic state at clean armchair edges. Spectroscopic and spatial evolution of this edge state will be presented. This work is supported by NSF DMR-1506618.
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Gbylik-Sikorska, Malgorzata; Sniegocki, Tomasz; Posyniak, Andrzej
2015-05-15
The original analytical method for the simultaneous determination and confirmation of neonicotinoids insecticides (imidacloprid, clothianidin, acetamiprid, thiametoxam, thiacloprid, nitenpyram, dinotefuran) and some of their metabolites (imidacloprid guanidine, imidacloprid olefin, imidacloprid urea, desnitro-imidacloprid hydrochloride, thiacloprid-amid and acetamiprid-N-desmethyl) in honey bee and honey was developed. Preparation of honey bee samples involves the extraction with mixture of acetonitrile and ethyl acetate followed by cleaned up using the Sep-Pak Alumina N Plus Long cartridges. Honey samples were dissolved in 1% mixture of acetonitrile and ethyl acetate with addition of TEA, then extracts were cleaned up with Strata X-CW cartridges. The identity of analytes was confirmed using liquid chromatography tandem mass spectrometry. All compounds were separated on a Luna C18 column with gradient elution. The whole procedure was validated according to the requirements of SANCO 12571/2013. The average recoveries of the analytes ranged from 85.3% to 112.0%, repeatabilities were in the range of 2.8-11.2%, within-laboratory reproducibility was in the range of 3.3-14.6%, the limits of quantitation were in the range of 0.1-0.5μgkg(-1), depending of analyte and matrices. The validated method was successfully applied for the determination of clothianidin, imidacloprid and imidacloprid urea in real incurred honey bee samples and clothianidin in honey. Copyright © 2015 Elsevier B.V. All rights reserved.
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Sun, Xinjie; Wei, Yingqin; Hou, Baojuan; Zhou, Guowei
2017-03-01
A new nanocomposite membrane was used to clean up impurities from complex samples and the obvious synergy was obtained in this paper. The nanocomposite membrane was prepared by dispersing TiO2 nanoparticles in chloroform and filled in the pores and lumen of polyether sulfone membrane fiber. The novel microextraction method showed the ideal selective extraction effect for alkaloids in the formulae composed of Rhizoma coptidis and the excellent clean-up efficiency compared with the single membrane method. The optimum extraction conditions were as follows: chloroform as accepted phase; the number of nanocomposite membrane fiber bars, 7; extraction time, 30 min; pH of the sample solution, 10.55; desorption solvent, methanol. The limit of detection for the described alkaloids was estimated at 0.122 μg mL-1. The recovery of the four alkaloids in complex samples ranged from 93.24% to 97.94% with relative standard deviation of <4.99 (n = 5). The validated method had been successfully applied to study the transfer rate of alkaloids in the producing process of Qihuang capsule and the ideal transfer rate of alkaloids was obtained in this paper. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.
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SPARCLE: Space Plasma Alleviation of Regolith Concentrations in the Lunar Environment
NASA Astrophysics Data System (ADS)
Clark, P. E.; Keller, J. W.; Curtis, S. A.; Nuth, J. A.; Stubbs, T. J.; Farrell, W. M.
2006-05-01
The return of robotic devices and humans to the Moon will occur in the near future. Based on our previous experience, surface dust is a major problem requiring a solution: During Apollo landings, extensive locally- induced stirring of the regolith caused dust to be suspended long enough to come into contact with conducting surfaces. Dust behaved like abrasive Velcro: it adhered to everything and attempts to remove it by simply brushing did not remove fines (<10) and resulted in severe abrasion. Lunar fines, because of their electrostatic charging, were relatively difficult to collect in sample bags along with other size range particles. Within hours, seals were broken, samples contaminated, and portions of the samples, especially fines, lost. Because of this difficulty, details on lunar dust are relatively sparse. Obviously, the strategies initially implemented to deal with lunar dust failed. A major technological challenge will be developing a dust mitigation strategy. A currently proposed strategy based increased magnetic susceptibility in lunar fines may not work uniformly well for fines of non-mare, or non-lunar, composition. Based on dust behavior already observed on previous missions, we believe the successful strategy will deal with dust dynamics resulting from interaction between mechanical and electrostatic forces. We are planning test and develop an electrostatically-based device to modulate the electrical potential of conducting surfaces, hence to self clean exposed surfaces while collecting dust samples. It would scan a surface constantly to control its potential, and a plate of the opposite potential. As a first step, an experimental low mass, power, and volume device with complimentary electron and ion guns with specially designed self-cleaning nozzles are being designed for to test our concept and develop a working charging and discharging strategy in the lunar environment. Meanwhile, a laboratory simulation will act as a feasibility study for a laboratory breadboard self-cleaning device based on the use of combined electron or ion beams. The compact device would act as plasma dust sweeper.
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Darchuk, Emily M; Waite-Cusic, Joy; Meunier-Goddik, Lisbeth
2015-10-01
Consolidation of the US milk industry has led to use of tankers for up to 24 h in between thorough cleanings. As the heavy use of tankers has not been previously studied, the effect of this form of hauling on raw milk quality is unknown. This study focused on the effect of frequent tanker use during hauling on raw milk quality at a commercial facility. Standard tanker use (cleaned-in-place once per 24 h) served as our control and incremental cleaning treatments (water rinse after each load, water rinse after each load with a sanitizer treatment after 12 h, and 12 h of sanitizer treatment) were added to the study to understand if any effect could be mitigated by more frequent cleaning. Producer samples were collected from the farm before loading milk into the tanker as well as sampling the same milk directly out of the tanker truck before unloading at the manufacturer. The study was repeated at 2 different dairy manufacturing facilities, once during the summer and once during the winter. Milk quality was quantified through industry-relevant microbiological tests: individual bacteria count, thermophilic spore count, and preliminary incubation count. Within the study we defined a negative effect on milk quality as a statistically significant difference between the tanker and producer samples in any of the 3 microbial tests conducted between treatments. Results from the study showed no clear effect due to hauling in individual bacteria count, thermophilic spore count, or preliminary incubation counts. There was also no difference in milk quality between the 2 plants, suggesting that neither season nor location affected our results in the standard use variable. As we did not see a negative effect on milk quality in the standard use variable, the addition of cleaning treatments did not appear to provide any clear benefit. Tanker surface swabs and ATP swabs were also used to monitor tanker sanitation and the efficacy of cleaning treatments. Both surface and ATP swabs revealed differences between cleaning efficacy at the 2 facilities. Although the differences in efficacy did not influence tanker milk quality within our study, variability in sanitation may provide a source of contamination that could negatively affect raw milk quality in other areas. Based on this study, current hauling practices appear to be effective in mitigating any measurable effect on raw milk quality; however, further investigation is needed before making industry-wide recommendations. Copyright © 2015 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.
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NASA Astrophysics Data System (ADS)
Bozso, F.; Avouris, Ph.
1986-09-01
We report on the low-temperature reaction of ammonia with Si(100)-(2×1). The dangling bonds in the clean Si surface promote NH3 dissociation even at temperatures as low as 90 K. The N atoms thus produced occupy subsurface sites, while the H atoms bind to surface Si atoms, tie up the dangling bonds, and inactivate the surface. Thermal or electronic-excitation-induced hydrogen desorption restores the dangling bonds and the reactivity of the surface. Silicon nitride film growth is achieved at 90 K by simultaneous exposure of the Si surface to NH3 and an electron beam.
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Polycrystalline silicon on tungsten substrates
NASA Technical Reports Server (NTRS)
Bevolo, A. J.; Schmidt, F. A.; Shanks, H. R.; Campisi, G. J.
1979-01-01
Thin films of electron-beam-vaporized silicon were deposited on fine-grained tungsten substrates under a pressure of about 1 x 10 to the -10th torr. Mass spectra from a quadrupole residual-gas analyzer were used to determine the partial pressure of 13 residual gases during each processing step. During separate silicon depositions, the atomically clean substrates were maintained at various temperatures between 400 and 780 C, and deposition rates were between 20 and 630 A min. Surface contamination and interdiffusion were monitored by in situ Auger electron spectrometry before and after cleaning, deposition, and annealing. Auger depth profiling, X-ray analysis, and SEM in the topographic and channeling modes were utilized to characterize the samples with respect to silicon-metal interface, interdiffusion, silicide formation, and grain size of silicon. The onset of silicide formation was found to occur at approximately 625 C. Above this temperature tungsten silicides were formed at a rate faster than the silicon deposition. Fine-grain silicon films were obtained at lower temperatures.
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Cleaning conveyor belts in the chicken-cutting area of a poultry processing plant with 45°c water.
Soares, V M; Pereira, J G; Zanette, C M; Nero, L A; Pinto, J P A N; Barcellos, V C; Bersot, L S
2014-03-01
Conveyor belts are widely used in food handling areas, especially in poultry processing plants. Because they are in direct contact with food and it is a requirement of the Brazilian health authority, conveyor belts are required to be continuously cleaned with hot water under pressure. The use of water in this procedure has been questioned based on the hypothesis that water may further disseminate microorganisms but not effectively reduce the organic material on the surface. Moreover, reducing the use of water in processing may contribute to a reduction in costs and emission of effluents. However, no consistent evidence in support of removing water during conveyor belt cleaning has been reported. Therefore, the objective of the present study was to compare the bacterial counts on conveyor belts that were or were not continuously cleaned with hot water under pressure. Superficial samples from conveyor belts (cleaned or not cleaned) were collected at three different times during operation (T1, after the preoperational cleaning [5 a.m.]; T2, after the first work shift [4 p.m.]; and T3, after the second work shift [1:30 a.m.]) in a poultry meat processing facility, and the samples were subjected to mesophilic and enterobacterial counts. For Enterobacteriaceae, no significant differences were observed between the conveyor belts, independent of the time of sampling or the cleaning process. No significant differences were observed between the counts of mesophilic bacteria at the distinct times of sampling on the conveyor belt that had not been subjected to continuous cleaning with water at 45°C. When comparing similar periods of sampling, no significant differences were observed between the mesophilic counts obtained from the conveyor belts that were or were not subjected to continuous cleaning with water at 45°C. Continuous cleaning with water did not significantly reduce microorganism counts, suggesting the possibility of discarding this procedure in chicken processing.
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NASA Astrophysics Data System (ADS)
Kim, Jae-Hun; Mirzaei, Ali; Kim, Hyoun Woo; Kim, Sang Sub
2018-05-01
Stainless steels are among the most common engineering materials and are used extensively in humid areas. Therefore, it is important that these materials must be robust to humidity and corrosion. This paper reports the fabrication of superhydrophobic surfaces from austenitic stainless steel (type AISI 304) using a facile two-step chemical etching method. In the first step, the stainless steel plates were etched in a HF solution, followed by a fluorination process, where they showed a water contact angle (WCA) of 166° and a sliding angle of 5° under the optimal conditions. To further enhance the superhydrophobicity, in the second step, they were dipped in a 0.1 wt.% NaCl solution at 100 °C, where the WCA was increased to 168° and the sliding angle was decreased to ∼2°. The long-term durability of the fabricated superhydrophobic samples for 1 month storage in air and water was investigated. The potential applicability of the fabricated samples was demonstrated by the excellent superhydrophobicity after 1 month. In addition, the self-cleaning properties of the fabricated superhydrophobic surface were also demonstrated. This paper outlines a facile, low-cost and scalable chemical etching method that can be adopted easily for large-scale purposes.
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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.
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Assessment of Refueling Hose Visibility: Post-Cleaning Evaluation
2013-10-01
Cott, H.P., and Kinkade, R.G. (Eds.), Human Engineering Guide to Equipment Design. Washington, DC: GPO. F-35 Gen 5 HMDS spec for minimum...spectral band sensors: visible, near IR, and short-wave IR. These images will be captured for each of the samples set up for both the geometries...Contrast Ratio Near IR Black Reflectance White Reflectance Contrast Ratio Short Wave IR Black
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Sarker, Mohammad Abul Bashar; Harun-Or-Rashid, Md; Hirosawa, Tomoya; Abdul Hai, Md Shaheen Bin; Siddique, Md Ruhul Furkan; Sakamoto, Junichi; Hamajima, Nobuyuki
2014-12-09
Improper handling of medical wastes, which is common in Bangladesh, could adversely affect the hospital environment and community at large, and poses a serious threat to public health. We aimed to assess the knowledge and practices regarding medical waste management (MWM) among healthcare providers (HCPs) and to identify possible barriers related to it. A cross-sectional study was carried out during June to September, 2012 including 1 tertiary, 3 secondary, and 3 primary level hospitals in Dhaka division, Bangladesh through 2-stage cluster sampling. Data were collected from 625 HCPs, including 245 medical doctors, 220 nurses, 44 technologists, and 116 cleaning staff who were directly involved in MWM using a self-administered (researcher-administered for cleaning staff), semi-structured questionnaire. Nearly one-third of medical doctors and nurses and two-thirds of technologists and cleaning staff had inadequate knowledge, and about half of medical doctors (44.0%) and cleaning staff (56.0%) had poor practices. HCPs without prior training on MWM were more likely to have poor practices compared to those who had training. Lack of personal protective equipment, equipment for final disposal, MWM-related staff, proper policy/guideline, and lack of incinerator were identified as the top 5 barriers. Strengthening and expansion of ongoing educational programs/training is necessary to improve knowledge and practices regarding MWM. The government should take necessary steps and provide financial support to eliminate the possible barriers related to proper MWM.
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NASA Technical Reports Server (NTRS)
Goreva, Y. S.; Humanyun, M.; Burnett, D. S.; Jurewicz, A. J.; Gonzalez, C. P.
2014-01-01
ToF-SIMS images of Genesis sample surfaces contain an incredible amount of important information, but they also show that the crash-derived surface contamination has many components, presenting a challenge to cleaning. Within the variability, we have shown that there are some samples which appear to be clean to begin with, e.g. 60471, and some are more contaminated. Samples 60493 and 60500 are a part of a focused study of the effectiveness of aqua regia and/or sulfuric acid cleaning of small flight Si implanted with Li-6 using ToF-SIMS.
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Deliberate Science, Continuum Magazine: Clean Energy Innovation at NREL, Winter 2012 (Book)
DOE Office of Scientific and Technical Information (OSTI.GOV)
Not Available
2012-02-01
This quarterly magazine is dedicated to stepping beyond the technical journals to reveal NREL's vital work in a real-world context for our stakeholders. Continuum provides insights into the latest and most impactful clean energy innovations, while spotlighting those talented researchers and unique facilities that make it all happen. This edition focuses on deliberate science.
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The purpose of this SOP is to define the steps involved in cleaning the electronic data generated from data entry of the Diet Diary Questionnaire. It applies to electronic data corresponding to the Diet Diary Questionnaire that was scanned and verified by the Data Staff during t...
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NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR CLEANING: FIELD FORMS (UA-D-38.0)
The purpose of this SOP is to define the steps involved in cleaning the electronic data generated from data entry of the field forms. It applies to electronic data corresponding to the field forms that were scanned and verified by data staff during the Arizona NHEXAS project and...
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The purpose of this SOP is to define the steps involved in cleaning the electronic data generated from data entry of the Time Diary and Activity Questionnaire. It applies to electronic data corresponding to the Time Diary and Activity Questionnaire that was scanned and verified ...